WATER POLLUTION CONTROL RESEARCH SERIES
                             15080DBO 03/71
     CONVERSION OF CRANKCASE
         WASTE OIL INTO
        USEFUL PRODUCTS
ENVIRONMENTAL PROTECTION AGENCY  WATER QUALITY OFFI

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             WATER POLLUTION CONTROL RESEARCH SERIES
The Water Pollution Control Research Series describes the
results and progress in the control and abatement of pollution
in our Nation's waters.  They provide a central source of
information on the research,development, and demonstration
activities in the Water Quality Office, Environmental Protection
Agency, through Inhouse research and grants and contracts with
Federal, State, and local agencies, research institutions, and
industrial organizations *

Inquiries pertaining to Water Pollution Control Research Reports
should be directed to the Head, Project Reports System, Office
of Research and Development, Water Quality Office, Environmental
Protection Agency, Room 1108, Washington, D. C.  20242,

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   CONVERSION OF CRANKCASE WASTE  OIL INTO USEFUL PRODUCTS
                             by
           National Oil  Recovery  Corporation
              Hook Road and Commerce Street
               Bayonne, New Jersey   07002
                           for the

                   WATER  QUALITY OFFICE

              ENVIRONMENTAL PROTECTION AOENCY
                    Project #15080 DBO
                        March 1971
For sale by the Superintendent ol Documents, U.S. Government Printing Office, Washington, D.C, 20402 - price $1

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                       EPA Review Notice
This report has been reviewed by the Water Quality Office,
EPA, and approved for publication.  Approval does not signify
that the contents necessarily reflect the views and policies
of the Environmental Protection Agency, nor does mention of
trade names or commercial products constitute endorsement or
recommendation for use.
                               ii

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                           ABSTRACT
The project goal was to demonstrate a simplified technique for
reprocessing spent automotive crankcase oils into useful petroleum
products other than lube oils, without producing residues which
cause water pollution.

To achieve the foregoing objectives, National Oil Recovery Corpo-
ration modified its entire plant system with special equipment and
conducted laboratory and plant runs.

The objectives were substantially attained in that all the products
from the vacuum distillation were sold as low sulfur heating fuels
and as potential diesel fuel.  Only the water in the fuel is not
recovered.

Some technical work was done to upgrade the refinery products to
obtain a higher product realization.

This report was submitted in fulfillment of Project Number 15080
DBO, under the (partial) sponsorship of the Water Ouality Office,
Environmental Protection Agency.
                              iii

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                          CONTENTS
Section                                            Page

   I      Conclusions                               1

  II      Recommendations                           3

 III      Introduction                              5

  IV      Summary of Refinery Runs #1-11 and
            Their Significance                      9

   V      Plant Obsolescence and Depreciation      19

  VI      Review of Engineering Activities From
            1/69 - 12/31/70                        21

 VII      Summary of Plant Modifications Related
            to Product Quality Development
            1/69 - 12/31/70                        23

VIII      Review of Plant Operations With Modifi-
            cations to Improve Efficiency From
            1/69 - 12/31/70                        31

  IX      Investigation and Feasibility Report
            To Upgrade NORCO Fractions 1/69 -
            12/31/70                               37

   X      Specific Recommendations                 55

  XI      General Recommendations                  61

 XII      Appendices                               63

XIII      Acknowledgments                          69

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                           FIGURES




                                                     Page



1     Plant Flow Chart                                7




2     Flow Sheet                                     43




3     Flow Chart For Truck Routes                    48




4     Hard Rock Clinkers                             53
                            vi

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                          TABLES
1     Processing Costs and Yields                  17

2     Distillation of Crankcase Oil at 760 MM
      Hg, After Dilution 1:1 With NORCO Naptha
      and Centrifugation                           30

3     NORCO Fractions - Physical Properties        44
                           vii

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                           SECTION I

                          CONCLUSIONS
1.  The composition of waste crankcase oil has significantly
changed during recent years, thereby presenting greater problems
to the present re-refining industry.

2.  It is evident from the operational experience of existing
acid/clay treatment plants that current techniques for reprocessing
are uneconomical and the by-products of that process are environ-
mental pollutants.

3.  National Oil Recovery Corporation's experience with its modified
plant and equipment proved that its process was a simplified tech-
nique for reprocessing waste crankcase oil into useful petroleum
products without producing residues which cause water pollution.

4.  National Oil Recovery Corporation's tests indicated disastrous
results to burning equipment and to the environment if waste crank-
case oils were burned directly or in combination with virgin oil.

5.  National Oil Recovery Corporation's technical work to date has
been directed toward obtaining a higher product realization and has
shown that this goal is attainable.

6.  The collection of waste crankcase oil should be systematic and
should be monitored to assure that the collected waste oil is dis-
pensed to a non-polluting refining facility.

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                         SECTION II

                       RECOMMENDATIONS
It is recommended that National Oil Recovery Corporation demon-
strate a revised flow sheet operation that will yield the following
results:

1.  Improve the quality of side-stream products.
      a.  Modify distillation temperatures
      b.  Conduct field tests with products
      c.  Upgrade products for use as chemical feed stocks
      d.  Simplify flow sheets

2.  Modify unit processes to minimize effluent volumes.
      a.  Replace steam jets with mechanical equipment
      b.  Minimize bottoms volume
      c.  Incinerate bottoms

3.  Show optimum flow sheet conditions to be used for projected
packaged refinery units.

4.  Develop new products with greater returns.  This will encour-
age re-refiners to consider necessary process modifications.
Products should be use-tested by an accepted petroleum oriented
testing laboratory to accumulate testimonial data for market
acceptance of a "special fuel" and "special lube."

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                         SECTION III

                        INTRODUCTION
Our country is faced with the enormous problem of cleaning the
environment.  One of the most destructive pollutants is auto-
motive crankcase oil, of which one billion gallons are dumped
annually into rivers, harbors, sewers, land dumps, etc.

According to the American Petroleum Institute,(1) approximately
2.5 billion gallons each of industrial and automotive lubricating
oils are used annually in the United States.  Approximately 1.25
billion gallons are drained and replaced with new or reprocessed
oil,  A significant quantity of industrial lubricating oils are
collected and reprocessed and sold back to the original industrial
or automotive users.  However, automotive crankcase drainings must
be collected from several hundred thousand service stations through-
out the country. (2)  The drainings are collected by thousands of
relatively small independent collectors who traverse cities in a
haphazard manner, competing with each other for the waste oil and
for the cheapest way to get rid of their 'load.1  If a receiver,
such as a re-refiner or road oil user, is located within an econ-
omically geographical range, and if the re-refiner is willing to
pay the collector more for his load of waste oil than it costs
him to deliver it, the collector may deliver his load for some
subsequent reprocessing and reuse.  However, if any of these facets
of the system are not favorable, the collector may dispose of his
charge in sewers, onto empty fields, directly into rivers and
streams, or he may sell it as a substitute for #6 fuel oil to an
unsuspecting user who will pollute the air and ruin his burning
equipment.

To help remedy that condition, the Environmental Protection Agency
awarded National Oil Recovery Corporation a research and develop-
ment grant to demonstrate a simplified technique for recycling
crankcase waste oil into useful petroleum products without causing
pollution.

The grant application was submitted in March 1968, but a grant was
not received until January,1969.  The original grant request was
developed on the basis of the quality of automotive crankcase waste
oils received during 1965-67.  Crankcase waste oil is a difficult
charge stock.  It varies in that it contains different proportions
of water, solids, additives, decomposed additives, road dust, gas-
oline, gasoline additives, some spent automotive transmission oil
with additives, spent and unspent products of fuel and lube combus-
tion, etc., etc.  In the industrial New Jersey area, great care
must be exercised to avoid taking in spent cutting oils, synthetic
excessive phosphorous, etc.  Each feed tank is a challenge.

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The P&I of the previous plant, with proposed modifications to the
original process, apparatus and instrumentation, were detailed in
accordance with crankcase waste oil composition prevalent during
1965-67, and pollution controls enforced during that time.  Mean-
while, the composition of crankcase waste oil has significantly
changed.  Automobile manufacturers have greatly increased the
mileage and time intervals between recommended oil changes.  The
additive content in motor oil has been considerably increased and
markedly changed; multi-grade motor oils with much higher addi-
tive contents are in much wider usage.  Increasingly, present
motor oil is made up of relatively low viscosity neutral oils into
which are compounded ever higher percentages of additives contain-
ing more metals with dispersants, detergents and solids.  Present
waste crankcase oils delivered to National Oil Recovery Corporation
contain more and more spent and broken down additives, sludge, and
tar-forming materials from piston 'blow-by,' generating problems
in the processing equipment and the products produced under the
Process and Instrumentation Flow Diagram presented in the grant
application.  Greater pyrolytic polymerization was experienced dur-
ing processing.  All this, in addition to the special emphasis
given to pollution control requirements, caused a substantially
greater percentage of down time with the available equipment and
necessitated numerous modifications to the piping and process
equipment  as the problems appeared  plus a decrease in opera-
t ing t emp era ture s.

The project goal was to demonstrate a simplified technique for
reprocessing spent automotive crankcase oils into useful petroleum
products, without producing residues which cause water polltuion.
Products produced would be suitable either as heating fuels, or as
diesel fuels.

The foregoing objectives have been substantially attained in that
all of the products resulting from the vacuum distillation of the
waste crankcase oils are being sold as lube stocks to compounders,
as well as for a low sulphur heating fuel market.  Only the water
in the feed stock is not recovered.

Some technical work has also been done to upgrade the sidestream
and bottoms products to obtain a higher realization than the dark
lube stocks and low sulphur fuels, and there is reason to believe
this can be done.  However, additional work is required to confirm
the results obtained thus far.

In order that the general public avail themselves of the design
criteria and operating data, the flow plan attached hereto presents
the significant operating conditions, a yield balance and informa-
tion on operating controls needed by anyone wishing to operate a
similar process.  The type of equipment used is designated schema-
tically.  (See following page for flow plan)
                              6

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    A detailed operating manual presenting start-up, shut-down and
    emergency procedures has also been  prepared and is included in
    the appendices of this  publication.
     HASH
     FURT4ACE
STORAGE
TXNK I
A
n


              EAR CONO
            nf
r>> 1
\
8

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fl


*"
too PSIO
STEAM

J -~
r
FLASH
  -TOWER
                                                                 100  PSIG STEAM

                                                           BAR.CONQ.
                        50">F -96F
  CHARGE 1800 CPH
  OH. I737GPH
  H2O.C3GPH
OIL-WWER
SEPERATORS
                  rr
                                         FRACTIONATOR
                                         ZT HG-640F
                                FRACTIONATOR
                                OVERHEAD
                                WCPH
                             BOTTOMS
                             COOLER
                             396 GPH
                                  Figure 1.

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                         SECTION IV

    SUMMARY OF REFINERY RUNS #1-11 AND THEIR SIGNIFICANCE

Run #1 - January 15-20, 1970

This run, with the rather complete testing of products by E. W.
Saybolt Co., showed that the results of operations in 1966-67
could be obtained in January, 1970, with some product improvement.
The bottoms did not significantly change.  Ash content and the
color of both light and heavy sidestreams did improve slightly, in
spite of increased additive content in the used crankcase oil charge
in 1970, compared with 1966-67  (see Table I, page   ).  The run
demonstrated that operation could be maintained during very cold
weather, despite malfunction of instruments, and difficulties with
auxiliaries:  boilers, oil heater burners, pumps, and electrical
curcuits and apparatus.  We stopped the run because of a sudden
and unexplained increase in pressure at the inlet of the Fractiona-
ting Furnace.  After shutting down and dismantling the equipment,
a large amount of coke was observed in the furnace tubes.  From
the rapid rate of pressure buildup, it was deduced that a slug of
oil containing undesirable polymers that are pyrolytically re-
synthesized to high molecular polymers produced heavy deposits
inside furnace tubes, causing scaling on all heating surfaces.

An attempt at a run was made on February 28, 1970, however, hard
porcelain Raschig ring fragments fell from the top of the flash
tower and jammed the pump and control valves several times.  The
run was abandoned, but the experience later resulted in removal
of the Raschig rings and installation of a cyclone separator in
the top of the flash tower, with improved operation.

Run #2 - February 28 - March 1, 1970

NORCO placed a screen in the suction of the Fractionator feed pump
and made a run of three days.  The screen accumulated more porcelain
fragments and considerable semi-solid material from the oil which
was subsequently examined and proved to be organic metallic compounds
that precipitated or coated the screen.  We had difficulty control-
ling the Fractionator top temperature because of inadequate controls.
Excessive amounts of Fractionator overhead oil went into the Kill
van Kull.  The Army Corps of Engineers, Coast Guard and Federal Water
Quality Administration forced a shutdown until adequate oil-water
separators could be designed, fabricated and installed.

Run #3 - April 21-22, 1970

NORCO installed oil-water separators, revised instrumentation to

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control the top of the Fractionator and intermediate temperatures,
and a new pump with piping connected to bypass the Vacuum Flasher,
located at the South Feed Tank suction lines to feed unheated oil
directly to the unit.  NORCO started and operated the unit satis-
factorily for about 36 hours.  The oil-water separators, pumps,
piping and revised instrumentation for control of Fractionator Top
Temperature operated satisfactorily.  The run was stopped because
of plugging of the light product reflux cooling coil lines and con-
trol valve.  The material fouling and plugging the cooling coil line
was a dark resinous sticky and viscous material with a sharp acrid
odor.

A material of this nature had been observed at times in various
runs during the period 1965-67, in the light product section of the
Fractionator, but it had not then plugged the cooler and lines and
forced a shutdown, such as occurred during run #3.  It was observed
to separate out of the light and heavy products; and when bottled,
a discrete floe was noted that gradually settled and accumulated
as a sticky material that adhered firmly to the bottom of the
bottles.  After settlement of the floe, the oil became noticeably
lighter in color.  The floe was analyzed to be a metallic phosphate.

During this run, we pumped feed from the large cold feed tank,
directly to the Flash Furnace and then into the Fractionating Fur-
nace and directly into the Fractionator.  The pressure at the in-
let of the Fractionator Furnace was rather high, as expected, 50
psig instead of 10 psig.  However, the Vacuum Fractionator function-
ed well and produced satisfactory results.  The operation demonstra-
ted clearly the feasibility of simplifying the plant in accordance
with flow sheet #3, submitted with the original proposal.  The run
was terminated because of stoppage of flow of light reflux resulting
from an accumulation of heavy viscous material at the control and
bypass valves.  However, no trouble was experienced because of
Raschig rings or semi-solid material derived from the charge stock.
The high pressure drop did limit the feed rate and, of course, in-
creased the unit cost of processing.
Run /M - May 7-11, 1970

After accumulating and analyzing data collected during Run #3,
the Raschig rings, along with liquid distributing and collection
apparatus, and supporting structure were removed and replaced with
a cyclone arrangement positioned at the top of the Vacuum Flasher.
A large screen was installed in the bottom of the Vacuum Flasher
above the suction line to the Fractionator Feed Pump to avoid
possible trouble with gummy or leathery semi-solid material that
might foul the positive displacement gear pump, which is used to
transfer the feed from the Vacuum Flasher to the Fractionator

                              10

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Furnace and Fractionator.  We started the unit, but stopped the
run after four days of improved operation because of jamming of
the gears in the Fractionator Furnace and a boiler.  The two pumps
stopped almost simultaneously.

The fuel being pumped was largely made up of recently distilled
light product.  The material jamming the gears of the pumps was a
very tenacious, tough, thick layer of film of dark resinous materi-
al with a dark red, almost black color and a sharp acrid odor,
which characterizes the light product distilled from crankcase oil.

With Run #4, practical commercial operation is believed to have
started.  Yield data, etc. for run #4 is reported at the end of this
summary.  After run #4, certain conclusions were drawn on the basis
of observations as noted below.

During 1965-67, the overhead, light and heavy distilled products
were darker than expected from experience with similar materials
distilled in ordinary crude petroleum refineries.  This was thought
to be caused by excessive entertainment of liquid and solid parti-
cles in the vapor passing through the Fractionator.  A demister
blanket was installed, with a wash oil distributor, but the blanket
could not be kept clear.  It quickly fouled up.  Improvements in the
flash zone were made, with some improvement in color.  The improve-
ment in color was not as great as expected from prior petroleum re-
fining experience.

Under the present program, acting in agreement with the FWQA think-
ing, improved transfer line equipment, flash zone entry arrangements
and secondary cyclones with steam spray nozzle injection of wash oil
with arrangements for recycling the wash oil were installed to pro-
vide for stoppage of entrainment and improvement of color and reduc-
tion of floe in the distilled products.

The color and floe settlement from samples from runs #1 through #4
inclusive did not improve as expected.

The color of gasoline distilled over the top of the Vacuum Flasher
after installation of the cyclone arrangement was good, about what
might be expected from petroleum refinery experience.

The color of the Fractionator overhead caught in the new oil-water
separators was much darker than would be expected from petroleum
refinery experience.  Also this material darkened considerably and
quickly in the oil-water separator.

The above observations led to the conclusion that the dark color
noted in distilled products probably was not a result of entrain-
ment and carry-over of liquid or solid matter in the vapor stream.

                               11

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It was concluded that the dark color noted in the distilled pro-
ducts and the dark, resinous, sticky semi-solid material might be
derived from some material passing in the vapor phase through the
Fractionator, but polymerizing and condensing as polymer, particu-
larly in the light product section of the Vacuum Fractionator.

After conferences with the Federal Water Quality Administration
Project Officer, relative to the observations and conclusions, the
Project Officer arranged a consultation with Esso Research and
Engineering Co. scientists concerning the problems of dark color
of distilled products.  Also discussed was the problem of drop out
of dark, resinous semi-solid material from the light product as well
as the heavy product and the fouling of the light product reflux
cooler and control valves.  Furthermore, the relatively quick foul-
ing of the Fractionator Furnace tubes was discussed with the Esso
scientists.  The Esso personnel told us that the material causing
dark color, etc. probably did pass up the Vacuum Fractionator in
the vapor phase.  They suggested trial usage of an inhibitor pro-
duct which they sell.
Preparation of Run //5

We promptly began injection of the inhibitor according to their
recommendations, with hastily assembled blow cases, into the crank-
case oil charge and the two sidestreams.  Control of the injection
rate and steady application is difficult to achieve with makeshift
injectors.  Orders for positive displacement, adjustable flow in-
jectors were placed.  Results so far, in spite of primitive injec-
tion apparatus, are encouraging.  The unit operated 7 days with an
adequate flow of light product without significant indication of
light reflux cooling and coil plugging.

The deposition of dark resinous materials from the samples of
light product has been sharply reduced, and in some samples it
stopped.  In the samples were deposition is found, the material is
softer and more fluid than before additive injection.  Apparently,
fouling of furnace tubes is significantly slowed by inhibitor in-
jection.
Run #5 - May 21-28. 1970 (166 hours)

Recirculation of feed during startup and after upsets and stoppages
was reduced to a minimum during this run.  This procedure should
reduce the formation of heavy insoluble polymers from V.I. additives,
and the accompanying very rapid coking of furnace tubes and hot oil
lines as noted during run #1.  This procedure was also followed
during run /M.  During run #5 the cold feed was charged directly
from the large south feed tank.

                              12

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Several times during the run, the charge pump motor-heater "kicked
out," as if the motor was suddenly overloaded.  This may have
been caused by the passage of slugs of viscous, insoluble in oil,
polymer passing into the pump and greatly increasing, for a short
time, the power required to run the pump.  Minimum recirculation
was practiced during run M and this accounts for the high percent-
age of bottoms made during that run.  During run #5, the furnace
outlet temperatures were quickly restored after each upset and re-
circulation of feed after an upset was reduced to a minimum.  This
procedure also markedly reduced the percentage of bottoms made.

During run #5 no tendency towards plugging of the light and heavy
reflux and product coolers was noted.  Some stream samples taken
during this run produced no dark bottom settlings in the sample
bottles.  While others produced dark fluid bottom settlings with
apparent viscosity not much greater than that of the oil, no hard
sticky bottom settlings, usually observed during previous runs,
were to be found.  However, the coke deposit on the tubes in the
Fractionator Furnace was found to be rather thick, as up to 5/8"
was observed.  The variation in the above findings might be caused
by the known uneven injection of inhibitors or defective mixing of
the feed in the feed tank.

The fouling of the Fractionator Furnace tubes did seem to proceed
at an accelerated rate as the feed tank level dropped and the feed
pump motor-heater began to "kick out" more often, thus stopping the
pump.  However, suspension of flow through the furnace probably
also accelerated furnace fouling.  Installation of a recording
ammeter on the circuit was completed to provide information.

While the furnaces now in service have served to provide design and
operating data and experience, product quality and characteristics,
yield data, maintenance information and experience, it is clearly
apparent that heat distribution in the tubes in the Fractionator
heater is very uneven and leaves much to be desired.  High metal
temperatures on about eight tubes out of 84, forced reduced heater
temperatures.  Velocity through the furnace is less than optimum,
particularly for a charge stock with strong fouling tendencies.

A new spiral 3" pipe coil must soon be bought for the Vacuum
Flasher heater or a more suitable heater supplied.  The bottom
spirals of the coil are excessively burned and scaled on the out-
side.  The inside of the coil would be very difficult to clean as
the heavy deposit is not ordinary petroleum coke, readily steam-air
decoked, but is largely composed of metallic oxides and sulfides de-
rived from dispersants and detergent additives present in motor oils,

The existing heaters have provided the necessary information to set

                                 13

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up specifications for better suited, simplified standard equip-
ment for slower fouling, longer runs, and improved products to
obtain an economically viable processing scheme.
Run #6 - June 11-18, 1970

More than 200,000 gallons were processed during this run.  The
entire production was sold as high grade fuels.  The 'bottoms'
in particular, were especially attractive to our customer  who
markets this product as a low-sulphur, minus 15F, pour fuel oil
additive  with excellent heat producing characteristics when
mixed with either #4 or #6 fuel oil.  The use of improved inhibit-
ing additives resulted in improved operating equipment performance.
The replacement and rearrangement of the baffle in the boiler to
accomodate pressure surges steadied boiler performance.  In gen-
eral, the unit operated without difficulty, and with tube deposits
at a minimum.  The technique of blowing down light reflux lines
helped eliminate blockage.  Yields and product specifications were
slightly better than in previous runs.

After run #6 was completed, Esso/Enjay engineers observed on-site
conditions and recommended better inhibitor injection techniques
at certain points in the operation to achieve optimum equipment
performance.
Run #7 - July 25-31, 1970
On July 24, 1970, we started up the boilers and unit and circulated
it until shut down on Friday, July 25, which was due to holes, one
in an air line, and one in a super-heater.  After making repairs, we
once'again started up the unit and ran it until July 31, 1970.

A refinery run of five days was aborted by a fire which occurred
in the vertical primary heater (replacement of the heating coil
was anticipated).  This run pointed up the recurring problem of
coking material accumulating in the various small lines around hot
oil pumps feeding the lantern glands of the pump stuffing boxes, on
the spray decks of the light product section of the Vacuum Fractiona-
tor, at the draw-off piping seal loop which leads from the Fractiona-
tor to the light draw-off stripper, and it also accumulated at the
bottom light product stripper and light product run down tank.

The entire production was sold to our customer, who marketed the pro-
ducts as a high grade fuel blend and low sulphur, low pour fuel blend
with #6 fuel oil.  Our marketing concept was altered to accomodate

                                14

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this potential  which aided consumers unable to meet low sulphur
requirements  now being enforced throughout the nation.  Our con-
sultant engineer was assigned the task of upgrading our distillates
(4 cuts) to a specification permitting use as #2, #4 and #6 fuels.
Run //8 - August 22 - September 2, 1970

During the month of August there was a concentrated effort to
repair the damages to the vertical furnace caused by fire.  The
entire inner surface of the heater was insulated, a new burner was
installed, and the electrical and control wiring and apparatus was
replaced or repaired.

A refinery run was commenced on August 22, 1970, and terminated on
September 2, 1970.  The results of this run matched the previous
results, with a marked increase in the coking material on the tubes
of the horizontal furnace, in addition to the accumulation of gummy-
like coke in the light reflux lines.  Approximately 300,000 gallons
of feed stock were processed during this run.

All the production of this run was again sold to our customer (a
fuel oil dealer) who marketed products produced as fuel oil blends,
straight fuel without blend, and diesel fuel.
Run #9 - September 26 - October 15, 1970

This run commenced on September 26 and was characterized by running
at a higher charge rate than previous runs, in addition to which the
charge stock was of a lower viscosity.  While there was some accumula-
tion of tarry meterial in the usual critical areas mentioned in pre-
vious runs, this run was practically free of tube coking.  More than
250,000 gallons of feed stock were re-refined and sold as useful
petroleum products.

However, the demise of an acid/clay treating re-refiner in this
area, brought pleas by local  'compounders1 to do  'something' for
their critical need of a re-refined product, free of odor and tarry
material, and with a minimum of #5 color.
Run #10 - October. 16-19, 1970

To meet the product demand of  'compounders' who were now faced with
the problem of a new source for re-refined lube oils, piping and
pump changes were made to permit re-distillation of distillates #3
and #4.  Eighty thousand gallons of sidestreams were re-distilled,
with resulting good color (35) and improvement of odor.  Color was
stable.  All products were sold to 'compounders' as lube stock.

                                15

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Yield, however, was poor, as hook-up was of experimental nature
and feed stock had a narrow boiling range making it difficult to
control.  However, results were impressive enough to include re-
distillation of distillates as an added feature of the future
process unit, if economical.
Run #11 - November 21-26, 1970

The results of this run were interesting in that one combined
distillate was produced instead of the usual light and heavy
sidestreams.  While this was attributed to blockage in the light
product draw-off line, it is interesting to note the marketing
advantage of a single combined sidestream product when needed.
This phenomenon also resulted in a higher gravity 'bottoms' pro-
duct which eliminated the necessity of additional blending for
our customer.  Entire production was sold to customers at equal
or increased price
This run demonstrated ability to produce one combined sidestream
with a higher quality bottoms product, which may be desirable as
a marketing advantage, when occasion arises; such as low-sulphur
fuel shortage, and high viscosity lube and fuel distillate demands,
                               16

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                            PROCESSING COSTS AND  YIELDS
                  A Breakdown of Runs #4 and  It5  Including  Input,
                     Yields, and Costs of Products  Produced
Run #
Feed
(Gal.)
Bottoms
(Gal.)
 4      176,288  67,850
_J>	   228.324  47_,_36_0	
Total   404,612  115,210  149,000
 Hvy.
 (Gal.)
 46,700
102,300
Product
Bottoms
Heavy
Light
Barometric
Gasoline
Fuel, Loss
   (H20)
       Total Gal.
       //4 and #5
       115,210
       149,000
        84,066
        22,000
         1,776
        32,560
Lt.
(Gal.)
44
39
84
Baro.
(Gal.)
,475
.591 22.000
,066 22,000
Combined Yield
of #4 and #5

28
36
20
5
0
8
.4
.8
.8
.5
.5
.5 Fuel
Gas
(Gal.
863
913
)

1,776
% Yield
#4
38
26
25
0
9

5
5
2
5
1
Fuel
Water
Loss
16,400
16,160
32,560
%
5 Fuel


Yield %
#5
20.
44.
17.
9.
0.
7.
7
9
3
6
T 5 Fuel
                                                                4.3 Water
                                                                     2.1  Water
Total Direct Costs  (Runs #4 and #5) per gallon
    Direct Costs
    Feed Charge
Total Fixed Costs
                $16,240.77
                 404,612
                $1,226.58
                 404,612
Add Feed Charge Cost

Total Cost

Schedule of Sale of Products
Runs #4 and #5
                    ,0401/gal. processing cost)
                                               )
                  = .003/gal. processing cost  )
                                               )

                  = .03/gal.
                             .0731/gal

Items Produced
Bottoms
Heavy
Light
Barometric
Gasoline
Fuel (Plant Use)
Water (Loss)

% Yield
28.4
36.8
20.8
5.5
0.5
5.0
3.0
Total
Gal.
115,210
149,000
84,066
22,000
1,776
20,230
12,330
Selling
Price/Gal.
.05
.07
.08
.08
.10
.10
-
TOTAL
                        100.0    404,612
                                       (avg. of  .07/gal.)***
                                     Tahle 1.
*** With improved equipment, the selling price  per  gallon will double.
    (See specific recommendations - page - 55)
                                         17

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                          SECTION V

            PLANT OBSOLESCENCE AND DEPRECIATION

Any analysis of processing costs and yields should make reference
to the dramatic obsolescence and depreciation factors of the plant
and equipment.  These factors barred the way to a confirmation of
results obtained thus far, as they were not anticipated in the P&I
as presented in the grant application.

   1.  The rapidly changing composition of the waste crankcase
       oil raised havoc with plant and equipment.

   2.  Environmental codes being enforced by regulatory agencies
       required modifications to plant and equipment to solve
       problems as they appeared.

   3.  Change in the presently accepted marketing concept of
       re-refined products due to environmental restrictions
       and charge stock changes.

As delineated in the refinery runs (1-11), the present plant was
rendered obsolete and ineffective due to the numerous and
costly modifications to plant and equipment to solve problems
caused by changes in the demonstration 'ground rules' (factors 1,
2 and 3 above) in order to acquire engineering data for the optimum
design processing plant of the future.  No single piece of equip-
ment escaped the operating difficulties caused by the great per-
centage of fouling and tar formation resulting from pyrolytic
polymerization during the processing.  A plant designed for a
1965-67 feed stock was found difficult to operate and unsuitable
for present feed stock loaded with tar-forming substances and
metallic solids generated by decomposed additives.  Moreover,
environmental protection regulations practically force a small
plant to avoid use of water as a cooling medium.  Consequently,
the costly installation of our A.P.I, oil-water separators designed
to meet criteria formerly applied to refinery operations, are now
obsolete according to New Jersey water quality standards.

Accordingly, any new plant design will benefit from the subject
matter in this report, but additional work is required to demon-
strate our ability to meet effluent standards for this type of
operation, while at the same time indicating that this process,
with additional equipment, will produce economically marketable
products, i.e., total recycling of waste crankcase oils without
polluting effluents.
                               19

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                         SECTION VI

    REVIEW OF ENGINEERING ACTIVITIES FROM 1/69 - 12/31/70

The following is a summary of the engineering activities during
the grant period, including the results of laboratory and field
investigations (pursuant to P&I ground rules) with comments on
considerations for future investigation.

1.  We installed separation equipment to definitely stop entrain-
ment of bottoms into distilled products.  The equipment was
effective.

2.  We found that entrainment, when crankcase oil was distilled
under vacuum, did not account for poor color and odor.

3.  We have established that waste crankcase oil can be diluted
and centrifuged, removing substantially all solids from the waste
crankcase oil.  Centrifuging of feed effectively reduces solids
in bottoms in laboratory vacuum distillation, however, plant
operation economics has not been established.

4.  We have identified the troublesome materials in the feed which
produce tar, poor color and probably odor.  These materials act in
the same way in the plant and in laboratory vacuum distillations.
They have been generally identified by scientists working in
laboratories, and the results are available in technical literature
on the formation of sludge in lubricating oils, and deposits in
gasoline engines.  The materials are:

  a)  Oxygenated hydrocarbons generated in quite small percentages,
      mainly from fuel.  They enter engine crankcases as blowby,
      past the pistons.

  b)  The catalysts which induce formation of tar are blowby gases,
      mainly nitrogen oxide.

  c)  Additives which inhibit formation of deposits are compounded
      into motor oil.  They are almost completely broken up by
      heating crankcase oil to 700F.  The presence of inhibitors
      and their breakdown at plant operating  temperatures may ex-
      plain the relative absence of deposits  in engines, and the
      prominence of tar deposits when distilling in a crankcase
      oil plant.

  d)  The recovered tar, as expected, contains considerable ash,
      probably derived from deccomposing  additives, dust and lead.

5.  In the plant, we have demonstrated removal of tar and odorous
products, by  soaking and settling at temperatures, and by redis-
tilling, which also includes considerable soaking and settling


                              21

-------
at temperature, and by stripping.  We found that even redistilled
oil darkens and precipitates tar after soaking two hours at tem-
peratures as low as 340F.

6.  We plan to conduct laboratory investigations concerning the
use of catalysts, chemicals, separating aids, soaking and other
procedures, either singly or in combination, for economically and
completely (or almost so) reacting to, and rejecting tar, color
and odor forming materials.  Procedures such as caustic treating,
acid/clay treating, etc., produce pollutants, and are not satis-
factory economically.

7.  Laboratory work has shown that tar and color-forming material
in distilled products can be extracted with small enough quantities
of suitable solvents to be properly economic.  Plant economics has
not yet been demonstrated.

8.  We have identified problems connected with distilling and pro-
cessing crankcase oil, and have developed plant apparatus, and
procedures for dealing with some problems.

9,  As pollution problems continue to manifest and become notice-
able with time, investigation and increase of knowledge, it
becomes increasingly apparent that satisfactory complete disposal
of crankcase oil to avoid all forms of environmental pollution is
more of a problem than was at first supposed.

10.  General layout of a crankcase oil plant for avoidance of
pollution from the operation of the plant calls for very detailed
design, as in the case of an oil refinery.  Consideration of the
topography of the land helps.  The study of geology finds oil,
and the study of topography helps hold it.

11.  The major crankcase oil processing cost is labor.  Plant
processing must reckon with this fact.  The labor force in a
crankcase oil processing plant must be small.  The application
of relatively simple equipment and particularly simple instru-
mentation is an economic must.
                             22

-------
                         SECTION VII

         SUMMARY OF PLANT MODIFICATIONS RELATED TO
        PRODUCT QUALITY DEVELOPMENT - 1/69 - 12/31/70

              Conditions Prior to Grant Award

Mist Blankets

Prior to the grant award, the Fractionator had been equipped with
a mist blanket positioned between the flash zone of the Vacuum
Fractionator and the bottom bubble tray, to prevent liquid parti-
cles entrained by vapors in the transfer line from passing through
the Vacuum Fractionator flash zone into the bottom bubble tray,
and into the heavy product sidestream drawoff below the bottom tray.
The mist blanket, in spite of a wash oil stream distributed over it,
fouled rapidly and repeatedly.  The sidestream drawn off the bottom
tray ran dark; always darker than ASTM 8 color.  The upper side-
stream was also darker than ASTM 8 color.  The mist blanket was
removed and the transfer line was connected to an eductor drawing
in flash zone vapors and discharging tangentially around the
cylindrical shell of the Fractionator to induce a high circular
velocity and produce a pronounced cyclonic separating force.  The
superheated stripping steam then used was also introduced into an
eductor drawing in stripping steam and stripped vapors and dis-
charging at high velocity to set up a cyclonic separating force.

The color of the distilled heavy product drawn off the bottom
tray improved slightly, but remained darker than ASTM 8 color.
The vapor uptakes on the bottom bubble tray continued to foul,
but at a considerably slower rate.  The light product was also
usually darker than ASTM 8 color.

               Conditions After Grant Award

Cyclones

After the grant award, the 4' diameter bottom stripping section
shell of the Vacuum Fractionator was extended up into the 6"
diameter main shell of the Fractionator.  A cyclone top was placed
on top of the extended 4' diameter section.  A new larger 8"
diameter transfer line was run from the Fractionator Furnace
through the outer shell of the 6" diameter section of the Frac-
tionator, into a tangential connection with the extended stripping
section shell forming a completed cyclone with the cyclone top.
The stripping steam connections were also installed tangentially
to provide a cyclonic effect.

Above the cyclone, at the top of the stripping section, a cyclone
supporting deck was welded to the Fractionator shell.  Six "high
                              23

-------
 efficiency" cyclones,  each 17  1/2" in diameter,  with  proportions
 on which considerable  performance  data was  available,  were instal-
 led on the deck.   Each of the  6 cyclones  were  provided with a  steam
 atomizing spray nozzle which sprayed  wash oil  into  the vapor in-
 lets of each cyclone.   Several unit runs  were  made  with a  noted
 slight improvement in  bottom sidestream,  heavy and  light product
 color.   Heavy product  separators averaged about  ASTM  8 color and
 light product averaged about 7-7 1/2  ASTM color.

 To reduce the barometric  oil loss  to  cooling water, two 10'  x  22'
 x  4'  API-type oil-water separators were installed.  Operation
 showed conclusively that  a water soluble  coloring material was
 going over the top of  the Fractionator into the  barometric con-
 denser and oil-water separators.   The bottom bubble tray vapor
 uptakes accumulated very  few deposits,  however,  dark  tar deposits
 continued to accumulate,  particularly in  the pans of  the side-to-
 side spray decks of the Fractionator  and  in the  light  reflux
 accumulator.   The  barometric oil collecting on the  surface of
 the  API-type oil-water separator,  markedly  darkened on standing.

 The  wash oil spraying  was stopped, however, no definite difference
 with or without wash oil  when  considering the  variable feed  stock,
 could be noted.

 Tar  Formation and  'Blowby'

 A  dark  viscous tar  continued to  cause difficulties by  plugging the
 2" pipe coil reflux coolers in the cooling  tub.  The evidence was
 rather  conclusive  that  tar-forming material was going  over  in the
 vapor phase.   Entrained solids carryover had been reduced  to a
 practical  level, while  deposit buildup  in vapor uptakes  on  the
 bottom  tray  above  the  flash zone of the fractionator was not sig-
 nificant.  More tar was formed in  the  light sidestream product
 than  in the  heavy  sidestream product.  The  color material was
 giving  the overhead barometric condenser cooling water  a yellowish
 tint  that darkened  on  standing with an oil  layer.  The  oil  layer
 also  darkened.

A paper  by C.J. Comke, D.J. Lindley and C.N. Sechrist,  "How  to
 Study Effect  of Blowby Gases,  Hydrocarbon Processing," Vol.  45,
No.  9,  p.  303, Sept. 1966, reported various oxygenated  compounds
 in the  crankcase, derived  from blowby past  the pistons  and rings
 of the  engine.  Through Mr. Richard Keppler, the Project Officer,
representatives of  an additive and chemical concern came to  the
plant and recommended injection of a  furnace tube antifoulant,  to
be applied to  the feed at  100  ppm, and to the heavy and light pro-
ducts,  at the rate  of 50  ppm.  They also told us of a paper, "The
Mechanism of Deposit Formation and Control  in Gasoline  Engines,"


                             24

-------
by Dr. Jerome Geyer, presented before the Division of Petroleum
Chemistry,  Inc., American Chemical Society, New York City Meeting,
September 7-12, 1969, wherein it was indicated that in tests
"running a  labeled benzene fuel," the carbon in the fuel con-
tributed 95% of the total carbon found in the sludge formed in
the crankcase oil of a gasoline engine operating in the steady
state.  The crankcase oil is stated to be the presumed source of
the other 5% of the carbon in the sludge.  The oxygenated hydro-
carbons derived from gasoline, described as "including all oxys
to C-,2j" would have a boiling range which would cause them to be
found most abundantly in the light product.  This is the product
in which most tar forms.  The paper also indicates the particular
importance of blowby nitrogen oxides, and other blowby gases in
catalyzing the formation of sludge from the oxygenated hydro-
carbons, of which probably 95% are derived from gasoline.  In any
event, the total amount of active material, oxygenated hydrocarbons
and nitrogen oxides, is surprisingly small.
The injection of inhibitors seemed to hold down the formation of
coke within the furnace and the hardness of the tar in the dis-
tilled products, but the color of the products remained dark, and
tarry material could be observed settling in streaks to the bottom
of sample bottles left undisturbed.

Re-Run (Odor and Color Improvement)

Both light and heavy product were accumulated and then re-run
through.the Fractionator Furnace and Vacuum Fractionator.  The
heavy product color improved from ASTM 8, to ASTM 7 or 6 1/2.
Odor was considerably better.  Light product color improved from
ASTM 7 1/2 or 7, to ASTM 6 1/2 or 6.  Despite the fact that it
had a considerably higher boiling range than the light product
charge stock, the odor on re-run light product was noticeably
better than that of the light product charged to the re-run opera-
tion.  No fouling inhibitor was injected into the unit during
re-running.

Inhibiting Additives

The additives compounded into automotive oils are chosen for
their demonstrated ability to inhibit the formation of sludges
and tarry material in crankcase oils.  However, talks with
suppliers of additives, plant experience and some data in the
literature confirm the fact that these particular additives are
substantially destroyed when the compounded oil is heated to 700F.
When waste crankcase oil is charged to the unit, the transfer line
temperature has run between 640F and 700F, depending on the
vacuum available on the Vacuum Fractionator and the API gravity
required on the bottom product.  During the re-run operations,

                             25

-------
 the transfer line temperature ran at 680-690F.  The amount
 of inhibitor additive left in the heavy product when distilling
 crankcase oil must be low.  The inhibitor content in the re-run
 heavy product after a second heating and distillation must have
 been very slight.  Light and heavy products were re-run separately.

 Tar Settling

 The bottoms of the light and heavy product rundown tanks were
 cleaned out before the re-run operation in order to observe
 deposition of tar from re-running.  Tar settles to the bottom
 of the tanks when product is left standing in the tank.  The
 vertical shell of the tank is coated with a thin dark layer
 of tar which apparently does not increase in thickness, and no
 attempt has been made to remove this thin coating.

 After  the re-run operation,  the light and heavy product produced
 was permitted to stand for 15 days before removal and shipment.
 The accumulation of  settled  tar in the bottom of the tanks was
 observed to be approximately 1/4" in thickness.   The tar in the
 light  product tank was harder and more dense than the tar in the
 heavy  product tank,  as is also the case when waste  crankcase oil
 is charged to the unit.   The percentage of tar that  settled was
 about  three times as great as the percentage of  tar  observed to
 settle from light and heavy  products produced directly  from waste
 crankcase oil and permitted  to stand for approximately  the same
 length of time  in the rundown tanks.

 Clay Contact

 Prior  to the  grant award,  we  contacted  light  and  heavy  products
 of ASTM color 8-plus  in  both  cases,  with about 0.3 Ib./gal.  of
 activated clay,  at 550F for  30 minutes,  cooled  to 180-195F,  and
 filtered in series through a  plate and  frame  filter  press  and  a
 plate  and frame  "polish" press.   The  color on  light  product  dropped
 to 2-3 ASTM color, while on heavy product, the color dropped to
 ASTM 3-4.   Some  odor  persisted in spite  of clay treating.  The
 treated  oil lost  the  characteristic haze  of untreated light  and
 heavy  product, but color was  stable.  No  sediment fell  to  the
 bottom of undisturbed bottles  of clay treated oil.  Oxygenated
 hydrocarbons, and tar in  the oils were effectively removed by
 clay treatment.

 Labor and  other costs, as well as environmental requirements,
 render clay treating as  formerly practiced uneconomical and un-
 desirable.  The clay is  costly and constitutes a relatively large
volume of material which is costly to dispose of without genera-
 ting pollution.
                             26

-------
Soaking and Settling (Color and Odor Improvement)

The tarry material accumulated in the rundown tanks after
settling was approximately .09 - .10% of the oil volume.  This
probably represents some 60-70% of the total tar-forming con-
stituents that were originally present in the waste crankcase
oil.  Redistilling, on the very first plant attempt, did show
a very significant improvement in color and odor.  Further
improvement, if only slight, would definitely open the door to
acceptance in a higher-priced market.

However, it seems probable that the same improvement may be
obtainable without redistilling, and the accompanying tying up
of plant, with marked reduction in plant capacity, and increase in
labor and fuel cost per gallon of product.  Soaking and settling
may be more economical and provide the same result.

With the existing plant arrangement, the light and heavy products,
after distillation, are little exposed to standing or soaking at
distillation temperatures, separation, and trapping of tar in
vessels, from which tar can be removed inexpensively.

Therefore, it is planned to install a "soaker & settler" tank,
possibly containing a tilted plate separator, for soaking and
settling the light product as it comes hot off the light pro-
duct section of the Fractionator.

In essence, the soaker-settler would closely approximate the
appearance of an old-style thermal cracking plant reaction cham-
ber with inlet, outlet and some other piping.  The soaker tank
would be tilted slightly to aid peeling the tar off the bottom
of the horizontally positioned soaker tank during plant shutdown
and cleanup operations.  If soaking and settling works well with
the light product, it will be applied to the heavy product.

Elimination of Tar Traps

The top of the Vacuum Fractionator has already been altered to
provide minimum settling time for tar deposition.  We had hoped
that we could eliminate pockets and tar traps in the upper sec-
tion of the Vacuum Fractionator and keep tar moving until it
and the light product got to the product rundown tank.  However,
the tar settled particularly in cooler outlet lines where it
must be cooled to a minimum of 190F to avoid darkening by oxida-
tion in rundown tanks.  The lines now are about as short and
direct as practical.  We plan to give it a chance to form com-
pletely and settle where we can easily remove it.  We may be
able to find some catalyzing material that can be injected into
the light product as it enters the line into the soaker.  See
Flow Diagram No.

                             27

-------
Need for Laboratory Back-Up

Through organic chemistry investigations, we propose to seek
catalysts and chemicals which may accelerate tar formation and
deposition, and provide more information about the character-
istics of color removal reaction or reactions, optimum tempera-
ture, pressure reaction velocity and equilibrium factors.

In the meantime, we continue to accumulate and collate everything
in the way of data economically available that might be signifi-
cant in developing basic information for finding an economic way
to achieve better color, odor, and carbon residue on the distilled
products; and less sediment and ash in the bottoms.

Accumulation of Engineering Data for Needed Equipment

We have accumulated and will continue to accumulate and collate
experience and data relative to the equipment described in our
annual report of June 21, 1970, pages 32 and 51, namely:  Furnace;
air-cooled coolers and condensers; vacuum pump; bottoms pump; and
solids removal.  Further investigation indicates that dilution of
either the crankcase oil feed or bottoms, with low viscosity
naptha and separation, is indicated to remove the solids from the
bottoms.  In view of data recently available, relative to metals
pollution in the air, separation may become a requirement for use
of bottoms for fuel; most other usages for bottoms also require
solids removal.

Laboratory Distillation Investigation

Results of recent laboratory investigations of processing methods
are worth noting.  We diluted representative crankcase oil feed 1:1
with 46 API naptha distilled from the Vacuum Flasher and had it
centrifuged at 10,000 x gravity, removing 2-3 wt. per cent of
solids.

Then the centrifuged sample was distilled at 760 MM in the labora-
tory to remove the 46 API naptha.  Distillation was stopped when
the "head" temperature or temperature of the vapor distilled off,
reached 400F.  The temperature of the "pot" or liquid in the
flask at this time was recorded at better than 600F.  The remain-
ing sample was cooled and later distilled under 5 MM Hg absolute
pressure in a glass flask and column.  The column was equipped
with a refluxing condenser and an adjustable controlled valving
arrangement that provided a cycle of refluxing 5 seconds and pro-
duction for 5 seconds.  With crankcase oil, it tended to stick.
Cuts were made according to a schedule to produce material of the
boiling point at 760 MM ranges as stated under the heading "Vapor
Temperature of Condensing Product or Cut."  See tabulation of

                             28

-------
data from Laboratory Vacuum Distillation, attached (following page).
The distillation required about 12 hours with one day's interruption
between the first and second days of distillation.  The actual flask
or pot and head temperatures are recorded for the finish of the dis-
tillation of products No. 3 and No. A.  The peak temperature in the
flask or pot (683F) was actually about the same as the usual trans-
fer line of the Fractionator Furnace.  The cuts produced were roughly
similar to average plant products, however, the fractionation was
much closer.  The light and heavy products were quite similar in
gravity, flash and viscosity, but laboratory cuts were distinctly
different in color as they condensed and were accumulated in the
receiver.  They were much lighter in color with the exception of
the naptha cut, but all cuts quickly darkened on standing, as the
condensed liquid accumulated in the receiving vessel.  The final
colors, after prolonged standing, were still lighter than plant
products.  The dark material began settling towards the bottom.
The odor of all cuts was much more acid or sour than plant cuts,
without the acrid or burnt smell of plant products.

The vacuum distillation, as witnessed in glass, emphasezed the
advantages of lower vacuum, 5MM distillation, using motor-driven
vacuum pumps without stripping steam.

Observations of laboratory vacuum distillation of waste crank-
case oil, confirm the findings reported in technical literature
and the observations of actual plant operations.

The testing of inflowing salt-cooling water, and the outflowing
salt-cooling water also indicate the presence of acidic materials
released to the water in the barometric condensers.
                              29

-------
      H
      fu
      cr
W    |"
o    n>
p^T-nTATTriN nu r.SANVrASF. OTL AT 760 MM He. AFTER DILUTION 1 1 WITH KORCO NAPTHA AND CENTRIFUGATION
PRODUCT
KORCO
Gravity  API
Vapor Temperature
of Condensing Pro-
duct or Cut 760 KM
Viscosity SSU
at 100F
Flash
Color, ASTM
15 Days Standing
As Condensed
Color of Bottom
of. Settled Bottle
Odor of Settled
Cut
Approximate
Volume M.L.
Approximate
Percent
End of One Pot
Distillation
Temperature Hea<
NORCO Naptha
Diluent Distilled
at 760
Nunber 1, Plus
1:1 of Diluent
47.1
140-352F
	
	
Light 1
	
Very SliRht Depo-
sit of Light Tan
Sediment
Sour, Somewhat
Sharp, Slightly
Oily
1,000 Plus
	
600 Plus F
	
rn\mNn;r: IlTST ILLATION OF CRANKCASE OIL AT 5 MM AFTER DISTILLATION AT 760 KM
Remainder of
Diluent

39.1
352-400F
	
	
3 1/2
Approximately
2 1/2 I!.17V Brown
Heavy Black
Fixed Coating
Sour
130
14.3
	
	
larometrlc Oil
Number 2
33.8
400-680F
	
	
Light 5
Approximately
2 1/2 Hazv Brown
Heavy Black
Fixed Clusters
Sour and Oily
93.5
10.3
	
	
Light Product
Number 3
31.6
680-792F
130
405
4
Approximately
2 1/2 H.TZV Yellou
Soft, Dnrk Pirown
Semi Fluid
Very Slight Sour
254
27.9
622F
550F
Heavy Product
Number 4
29.8
792-900F
239
455
5
Approximately 3
Hazy Yellow
Dark Brown,
Slightly Fluid
Slight Sourish
375
41.2
683F
567F
Bottoms
Number 5
	
900F Plus
(Est.) 200 Furol
at 122F
	
Dark Brown
Dark Brown
Dark Brown, Greasy
Fine Solid Particles
Very Slight Oily
57.5
910 ML
6.3
100.0



-------
                       SECTION VIII

REVIEW OF PLANT OPERATIONS WITH MODIFICATIONS TO IMPROVE EFFICIENCY
                   FROM 1/69 - 12/31/70

The following is a summary of plant operation techniques including
feed stock control, mixing temperature controls and plant equip-
ment to achieve simplified processing with the use of antifoulants.

Uniform Feed Stock

To maintain uniform composition of feed to the process, and thereby
maintain control over product streams specifications, two 40'
diameter by 30' high feed tanks are equipped with four mixing
eductors directing the flow at an angle of 30 upward and tangen-
tially around the tank in a counter-clockwise direction.  The
eductors are fed with a rotary positive displacement pump at a
rate of about 100 gpm at 30-40 psig.  During the warmer half of
the year, the tanks are well mixed by 3-10 hours pumping.  Strain-
ers are necessary to avoid damaging pumps and plugging eductors.
The tanks are not equipped with heaters.  During the cold winter
months, mixing is difficult.  The most economic answer would pro-
bably be the installation of adequate propeller type mixers.
Keeping tanks hot all year is very costly.  High energy input
mixers, eductor or propeller types, operating a short time, are
more efficient and economic than low energy input mixers consuming
actually more KW hours of electric power.

Feeding cold, directly from tanks during the winter months has
proven practical.  Suction and discharge lines must be sized for
laminar flow and practical pressure drop.  A long suction line is
not desirable because of pressure drop and lowered pump efficien-
cy.  Considerable savings can be realized by not maintaining
feed tanks at some set temperature.  Water content of crankcase
oil as received has been low.  Some water has been drawn off the
bottoms of feed tanks.  When feeding from cold feed tanks, ade-
quate surface should be provided in the convection tube section
of the flash furnace to accomodate the high viscosity and low heat
transfer rate characteristic of cold oil.  This provision prevents
excessive skin temperatures and resultant coking of heater tubes,
especially during the winter months.  Heat exchangers might be
provided to preheat the cold feed, but would have to be proven
economic.

A motor-driven rotary positive displacement feed pump, equipped
with reduction gear drive, installed and used since early April
1970, has proven satisfactory for both summer and winter.  A
strainer is required, primarily for the relief valve on the pump.
as it showed a tendency to jam open on relatively small particles
of trash in the feed.

                              31

-------
After passing about 3,000,000 gallons of crankcase oil through
two  feed  tanks, 40' diameter by 30' high, the tanks were opened
and  inspected.  Very little water and sediment was noted and
there was no apparent corrosion.

Antifoulant Injector

We installed anitfoulant injectors, and now inject antifoulant
material  into the feed entering the Flash Furnace at the rate
of 100 ppm.  The fouling of Fractionator Furnace tubes may have
been reduced slightly, but performance is difficult to evaluate
because of feed stock variations, troubles with instrument
control,  etc.  The tube diameters in our furnaces are large,
velocities in the tubes are low, and pressure drops through
the  furnace tubes are also low.  Fouling normally is consider-
ably greater in black oil heater tubes at lower velocities.
We have increased the flow velocities in a few furnace tubes
by installing cores.  These tubes had a tendency to overheat,
but  cores increased cleaning time and cost.  A re-refining oil
heater, from our experience, should have fairly high velocities
in the tubes, coinciding with a higher pressure drop.

We also injected antifoulant into the light and heavy products
reflux to decrease the tendency to foul the Vacuum Fractionator
internals, reflux lines, pipe coil coolers and control valves.
We did notice a decrease in fouling, but color was darkened
slightly.  We have both injected and not injected, attempting
to arrive at definite conclusions.  The situation is now clouded
because we wish to remove the color forming material from the
product and are exploring re-running, soaking, polymerizing
catalyst, etc.  Antifoulants, we think, are troubleshooting
items that can be helpful.

Modifications to Equipment to Improve Operation

The  top of the flash tower was originally provided with Raschig
ring packed sections, which tended to generate Raschig ring chips
which caused trouble with the positive displacement rotary Frac-
tionator Furnace charge pump.  The Raschig ring sections were
removed.  The top of the Vacuum Flasher was converted into cyclone
structure, and the Flash Furnace transfer line was enlarged and
arranged to discharge tangentially into the cyclone top of the
Vacuum Flasher.  The results have been satisfactory.   The color of
the  overhead product dropped from ASTM 2 to 1-1 1/2.   Difficulty
with Raschig ring chips has been avoided.

There is less accumulation of loose deposits on the cylindrical
shell, and less dirt collects around the large screen, installed
at the bottom of the Vacuum Flasher to keep particles of tower

                             32

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 deposit  from getting  into  the  rotary  positive displacement pump
 feeding  the  Fractionator Furnace.  The  feed  stock  constantly
 changes,  and exact  comparison  is difficult.

 The  Fractionator Furnace is  of  classical design.   Originally,
 the  tube  surface exposed to  direct radiation of the flame was
 quite  small,  requiring excessive air  flow to avoid overheating
 of the tubes  exposed  to direct  radiation.  Before  starting up,
 after  the grant award, the furnace blower discharge was piped
 to provide flue gas recirculation into  the furnace.  This de-
 creased the  excessive radiation rate  to relatively few tubes
 and  also  reduced fuel consumption.

 Even so,  difficulty was experienced with local overheating of
 radiant tubes nearest the flame in the Fractionator Furnace.
 The  1  1/2 HP motor was replaced with  a 3 HP motor.  New sheaves
 and  vee belt were installed  on  the motor, increasing blower
 impeller  speed 26%.  This increased flue gas recirculation and
 relieved  the  tendency of radiantly heated tubes to become
 overheated.

 Wear and  Tear

 During several runs, the wear rate at the end of the 8" Frac-
 tionator  Furnace transfer line, where it discharges tangentially
 against the shell of the 41  diameter  stripping section, has been
 excessive.  We have installed a wear  plate at this location and
 will install a wear 'plate*  with a welded-on, hard-faced coating
 of a suitable super-hard metal.  We now control the outlet pres-
 sure at the furnace by adjusting the  amount of steam injected
 into the  furnace inlet, the  furnace transfer line  temperature,
 and  the dehydrated oil charge rate to the furnace.  The wear
 rate may also be a function  of  the particulate hard solid matter
which may be in the charge from time  to time.  Centrifuging feed
 stock would probably be helpful.

 Superheated Steam

We originally used a steam superheater for superheating stripping
 steam.  The superheater included controls, blower, fuel pump, ex-
 tended surface heating tube,  expansion joint, etc.  The maintenance
 and attention required, and  the upset operation of the Vacuum
Fractionator, frequently caused by the superheater, resulted in the
 decision to abandon it.  We now use throttled saturated steam for
 stripping in the bottoms stripping section,  in the Vacuum Flasher,
and in the two sidestream strippers.   The Fractionator Furnace
 transfer line is run at slightly higher temperature to offset the
 lower heat content of the stripping steam.  A furnace specifically
designed for waste crankcase  oil processing at 30-75 MM Hg would

                             33

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include a conventional superheater in the convection section.  A
plant equipped with motor vacuum pumps operating at 5-10 MM would
not require superheated steam.

Jamming and Screening

The 4" suction line for the Fractionator bottoms had no screen.
Occasionally, we experienced evidence of the jamming of the side
pot disc valves in the steam reciprocating simplex pump.  A quite
coarse screen, covering the 4" suction line, was installed at the
bottom of the Fractionator.  Now a cubic foot, or more, of solid
deposit accumulates in the bottom of the Fractionator during a
run, but the pump operates smoothly without evidence of valves
j amming.

Reduce Fouling and Contact Loss

The top light product section of the Fractionator is provided
with three spray decks and a bottom liquid catch pan.  Tar has
collected in the spray decks and catch pan.  Tar is always
heavier than oil and settles in low spots and traps, tending to
polymerize and become more viscous and of higher specific gravity
on standing.  Tar accumulations build up and distort the flow
patterns of descending light product reflux and the ascending
vapors, reducing the effectiveness of contact between vapors and
liquid.

To reduce fouling and loss of contact between liquid and vapor,
the pans of the two spray decks have been filled with sloped
concrete and provided with a low-volume flow channel at the weirs
of the spray deck.  This greatly reduces the volume available for
catching tar and for "soaking" the reflux liquid and any formed tar,

The time and labor required for cleaning the spray decks has been
very sharply reduced.  Contact between vapors and liquid, judging
from operating and product data, is good.  The third spray deck
will be modified to minimize trapping of tar and "soaking" of
light reflux liquid.  The catch pan, under the bottom of the three
spray decks, will also be modified to reduce tar trapping and
cleaning time.

Steam Blowing to Remove Tar

From observations of plant operations, examination of tar accumula-
tion, the available subject literature, etc., it was decided to in-
stall adequate steam blowing facilities for blowing all four side-
stream cooling coils.  The four coils, installed in 1966, are all
located together with the bottoms cooling coil, in a common steel
shell tub, supplied at the bottom of the tub with harbor salt water.

                             34

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The coils are made up of 2" steel pipe "U" bends, connecting
20-21' lengths of steel pipe.  The steam blowing lines are 2"
pipe, with 2" valves, 2" check valves, and 2" connections and
fittings, supplied with 100-110 psig saturated steam.  Outlet
lines for blowing coils and sections of piping and controls,
etc., are all 2" pipe.

One cooling coil or section of piping is blown at a time.  Tar,
which is quite solid at 0-95F, is plastic or fluid at tem-
peratures ranging between 212-344F, which are the saturation
temperatures at atmospheric to 110 psig pressure.  So far, the
blowing arrangements have served to clear lines and coils enough
to permit maintenance of operation.  Until now, no dismantling
of cooling coils has been necessary.  Practically no opening of
2" pipe lines has been necessary.  Suction lines to pumps have
been broken to permit pump repairs, and inspection of suction
lines, pump impellers, wearing rings, etc.

The tar is extremely adhesive and positive displacement rotary
pumps quickly jam and lock when tar gets to moving parts.  Cen-
trifugal pumps are satisfactory for moving hot oil containing
the tar, which coats impellers, but the film does not become thick.
On cooling the pump casing, the wearing rings may stick to the hub
of the impeller, but on forcing rotation of the shaft with a wrench
and breaking loose, they should run freely; once warm or hot oil
reaches the pumps.

Simplified Gland-Oil Piping on Hot Oil Pumps to Reduce
Maintenance Caused by Tar Formation

We have removed check valves, pipe fittings and other gears which
too easily plugged with tar in the 1/2" and 1/4" lines supplying
gland oil to the light and heavy product and Reflux Centrifugal
pump packing boxes.  Check valves were not replaced.  Pipe and
fittings were replaced with steel tubing and tube fittings.
Tubing was bent as required, with tube fittings permitting rapid
assembly, opening, inspection and replacement.  Flexible wire
cable provided with a cutting tip and a rotary drive arrangement,
with benzol solvent, provide practical cleaning arrangements.

We have also provided an elevated tank, for receiving cold settled
heavy product, with provisions for maintaining a level in the tank.
A line from the side of the tank provides cold heavy product under
slight pressure to all lantern glands.  This one line is provided
with a single check valve to avoid any back flow from the pumps
into the tank.  The connections from the pump dischargers to the
lantern glands have been retained, but they are normally left
closed, and used only in emergency, or in case of difficulty with
the supply of cold heavy product oil.


                             35

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                         SECTION IX

           INVESTIGATION AND FEASIBILITY REPORT
        TO UPGRADE NORCO FRACTIONS  1/69 - 12/31/70

The initial program definition focused primarily on a feasibility
study to upgrade the possible uses to which the various NORCO
fractions could be applied.

From this product engineering phase, we soon learned that not
much could be done with the distillation bottoms without prior
removal of solids.  This conclusion was reached after extensive
and time consuming investigation showed that none of the largest
potential users, namely the paint-sealant-plastics-lubrication-
and rubber industries, could tolerate metal-organic contaminants
in the oils used in compounding.  Moreover, some of these are
even sensitive as to moisture, odor and color.

For these reasons, we fell back on the old standby use as a fuel
oil which, regrettably, is advocated by the American Petroleum
Institute.  In the "Final Report of the API Task Force on Used
Oil," the Committee recommended that up to 25% of spent lubrica-
ting oil (untreated) may be blended with fuel oil, and that this
mixture may be used in existing commercial and industrial com-
bustion equipment without deleterious effects.

This recommendation is neither wholly supported by the burning
tests noted in the report, nor by the evidence from our study,
which follows:

    Re:  Progress report to Mr. Richard Keppler, Project
         Officer, Federal Water Quality Administration (FWQA),
         Project No. 15080 DBO

    Subject:  NORCO Comments on Final Report of the API Task
              Force on Used Oil Disposal

    Date:  October 16, 1970

    Dear Sir:

    We carefully studied (with subsequent laboratory and field
    work) the FINAL REPORT OF THE API TASK FORCE ON USED OIL
    DISPOSAL.  A highlight of the report was their recommenda-
    tion that up to 25% of used lubricating oil may be added
    to other grades of fuel oil, and that this blend can then
    be successfully used without deleterious effect in existing
    commercial or industrial combustion equipment.  Subsequent
    laboratory and field work led us to conclude that the API
    recommendation is erroneous and unsupportable  and may,
    if followed, result in a combination of serious health
    problems and costly maintenance problems to most oil-burning
    equipment.

                               37

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The NORCO project has placed a high priority on the clean-
ing up and purification of the feed stock and/or distilla-
tion bottoms without resorting to conventional acid/clay
treatment.  (This is in order to avoid a large buildup of
process residue which would have to be disposed of, and
which would constitute an ecological violation.)  Our
tests and investigations have shown that the major road-
blocks in most applications to which the reclaimed oil
may be put are the additives, high molecular organic metal
compounds which are not readily released from solution.
Unfortunately, they will decompose and constitute a serious
hazard even in low-grade applications such as when used in
industrial combustion equipment.  This is substantiated by
samples taken from the combustion passages and flues of
several boilers.  In these instances, reclaimed crankcase
oil and deposits ranging from fly ash to hard rock clinkers
resulted.  Spectro-analysis of these clearly shows the
presence of lead, magnesium, copper, aluminum, vanadium,
silicone, iron, barium and various compounds with calcium
and phosphorous which are deposited as phosphates, carbonates,
and silicates; and as such are intolerable in boilers.  We
append a number of documents which will support this
contention.

Exhibit A reports the particulate matter contained in the
distillation bottoms from the NORCO refinery.  It consists
largely of carbon ranging into the colloidal state.  The
metallic constituents derive from automotive additives and
to a smaller extent from engine wear.  This analysis does
not reflect on the metal-organic compounds still in solution.

Exhibit B deals with the above subject matter far more
exhaustively.

 Specimen #8U is a bottoms sample similar to the one analyzed
in Exhibit A.  All major, minor and intermediate metallic
contaminants are present in the amount of approximately 5.6%
of the total bottoms.  The balance to be found in colloidal
and particulate carbon, asphaltines, olephines, and of course,
aromatic, naphthenic and paraphenic hydrocarbons.

Specimen #9U is a boiler tube deposit.  This analysis clearly
shows the presence of all inorganic compounds found in #8U.
These deposits are formed from the organic state during the
short transit of the fuel droplet through the burner flame.
A Commentary (page 5) is appended and discusses some of the
findings, conclusions and recommendations of this effort.

                           38

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Exhibit C is a further analysis of boiler tube deposits
and was conducted by the Research and Development Depart-
ment of Texaco.  As may be seen, these findings are very
much in agreement with Exhibit B in that the spectro-graphic
analysis shows lead and iron to be present in major amounts
and barium, phosphorous, magnesium, aluminum, silicone and
vanadium are minors.  Further, an x-ray analysis evidences
the presence of rust, sand, lead sulphate and magnesium
phosphate.

Exhibit D is an analysis of the #6 (low sulfur) fuel oil
which was burned in the boilers from which the deposits
in Exhibit A and Exhibit B (Specimen #9U) were collected.

This analysis confirms the absence of any contaminants in
the other fuel used.  The presence of vanadium in a concen-
tration of 46 parts per million is insignificant.

Exhibit E shows a graphic presentation of a Cleaver-Brooks
fire-tube boiler which is similar to the equipment used.

In addition, samples were also collected from residential
boilers in apartment buildings.  In these, the deposits
were not hard rocks, but rather dense, one-quarter to one
inch thick layers of fly ash which substantially covered
all cast iron heat exchanger surfaces, thus very really
preventing any heat transfer to the building.

It appears that, given the proper flame temperature and
transit time of the atomized fuel/additive droplets, there
results a coating which is very much akin to that achieved
by flame spraying of metal parts with inorganic metal oxides,
a process often resorted to to prevent heat transfer, thus
causing exactly the opposite of the results desired in com-
bustion equipment.

Further reference is made to the Final Progress Report on
Water Pollution Control Demonstration by Villanova University
(Project Grant WPD 174-01-67).  On page 3, (6) recites as
follows:  "The vacuum bottoms contain solid metallic compounds
(probably as organo metallics) that render it unsuitable as a
residual fuel."

The comments of Exhibit B attempt to go a step further, show-
ing that the high metal concentrations found in used lubrica-
ting oils is not only a hindrance in its use for most com-
mercial purposes, but also constitutes a valuable by-product
which may easily be recovered and thus yields additional
revenue for the re-refiner.

                           39

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   To restate in more dramatic form what is said in the
   foregoing:

   The combustion (or decomposition) of one gallon of distil-
   lation bottoms causes the formation of 7 grams of heavy
   metals (based on 2 grams per liter).  This is equal to a
   quantity of 5 gallons of collected oil, since the bottoms
   account for approximately 20% of the feed stock.  However,
   7 grams of metal in turn yield roughly 21 grams of deposits
   in the oxide form.

   According to API recommendations, a boiler operating on
   60,000 gallons of fuel per day would consume 25% of this
   amount in waste oil, resulting in 120 pounds of rock clinkers
   similar to those analyzed in #9U and the samples furnished
   herewith.

   That this quantity is not supported by actual boiler opera-
   tion, is entirely due to the fact that some of these sub-
   stances are lost as volatiles and fly ash in the form of
   oxides, carbonates, sulphides, sulphates, phosphides and
   silicates, and as such, constitute an intolerable air
   pollution hazard.

   In view of the above supporting evidence, the recommenda-
   tion in the API report appears irresponsible since it has
   led to the disabling of a number of boilers which had to
   be cleaned and repaired.  Moreover, the presence of motor
   fuel additives in fuel oil constitutes a very real health
   hazard to the entire community.

                           Very truly yours,
                                  '*/
                           Solfred Maizus, Project Director
                           NATIONAL OIL RECOVERY CORPORATION

From these studies, we conclude that burning with untreated crank-
case oils can cause serious maintenance problems with many burners
and can potentially produce serious health problems associated with
the discharge of heavy metals in exhaust gases.  The spectro and
particulate analyses also clearly indicate that the ensuing metallic
oxide and carbonate clinkers, as well as any fly ash, are direct
derivatives of the metal phosphates in the oil.  Consequently, an
extensive development program was initiated to develop techniques
to remove these suspended solids and dissolved organo-metallics to
not only make all the streams useful as products, but to also
maximize the duration of plant runs.

                              40

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Methods of Separation

Our efforts to find suitable separation methods included the
following:

A)  Centrifugation

Up to 50,000 g's and 1/2 hour residence time in a SORVAL machine
proved commercially impractical.

Further work in a PFAUDLER centrifuge by varying temperatures and
flow rates proved unsatisfactory.  Similar results were obtained
with a SHARPLES machine.

The introduction of another variable - namely dilution ratios -
finally proved successful in causing significant separations and
precipitations of additives as a dirty white to gray sediment.
We noted approximately 3% of detention.

These preliminary results initiated a more intensive program, using
solvents for pretreatment.  These experiments were carried out by
Centrico using WESTPHALIA equipment.  Practical feedrates (resulting
in approximately 20 seconds residence time) were obtained for the
following minimum dilutions:

        0.5 parts Naptha  : 1 part waste oil, and
        0.3 parts Naptha  : 1 part distillation bottoms

B)  Considerations relating to centrifuge cost and maintenance,
plus a limit of roughly 1.5 on the specific gravity of the solid
particles which can be safely processed, led to an investigation
of Cyclone separators (DEMCO, - DORR OLIVER).  It was not possible
to properly evaluate this equipment due to budget restrictions, but
indications are very promising, and this approach is definitely to
be pursued further.

C)  Settling Tanks

From our studies with centrifugation, it is also possible to use
settling tanks in place of, or preceding centrifuges.  Budget
restrictions prevented a parametric study of this concept.  How-
ever, it is safe to say that dilutions must be at least doubled
in order to achieve fair results, and for cold temperature opera-
tion these ratios may have to be substantially increased.

D)  Filtration

Organic and inorganic filter cartridges made of metal, ceramics,
hair, fiber, felt, paper and plastic were investigated.  Also

                              41

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studied were the various filter shapes; namely round, flat and
accordian zig-zag.  Filters which were both throw-away and clean-
able (wash or burn-off) were also investigated (CUNO, FRAM, PALL,
CARBORUNDUM, etc.).  Of these, edge-type filtration (VOKES) proved
promising by providing relatively long filter runs.  Further
extensive efforts in this area should be beneficial.  Also, the
use of filter aids in combination with the above method is recom-
mended for further study.  (The use of clay and filter aids was
not permitted to be included in this study by the Water Quality
Office.)

E)  Tests with Ultrasonic treatment in order to achieve coagulation,
separation and emulsification are inconclusive.  The response from
FIBRSONICS and BRANSON SONIC PRIORY CO., as to performance, experi-
ence and available electro acoustic equipment, ranged from doubtful
to negative.  However, HOMO-REX, a mechanical ultrasonic emulsifying
machine, yielded very stable suspensions. This should be pursued
further.

F)  Ion Exchange Resins

All literature investigations reveal this method as effective,
but too costly for our plant-scale operation.  D) and F) may be
used without diluents, while E), on the other hand, should be
combined with solvent pretesting in order to reduce the required
force field power levels.
                              42

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                                                             TO DISTILLATION
                                                            (FRACTIONATION)
                                            CENTRIFUGE
                                            (OPTIONAL)
   WATER


OEEMULSIFIERS
 COAGULANTS
                  ULTRASONIC
                 HOMOOENIZER
ADDITIVE SEDIMENT
   AND WATER
                            Figure 2.
Pretreating System
From the above studies, it is obvious that  the  existing  or  pre-
viously proposed flow sheets should be revised.  NORCO proposes
a process (see flow sheet above) which pretreats the  incoming
lube stock with organic solvents or aqueous diluents, including
coagulants and de-eraulsifiers to neutralize surfactant action.
Centrifugation or settling tanks are used to  eliminate particulate
contaminants as well as precipitated metal-organic  additives.
Aqueous diluents are removed by decanting,  separation and evapora-
tion.  Organic solvents are returned for use  with fresh  lube stock
via a solvent recovery system.  In this cycle,  the  solvent  function
is entirely mechanical and not chemical in  nature.

A precise laboratory vacuum distillation of representative  NORCO
feed stock, pretreated as indicated above,  provided the  tabulated
information that follows:  (Note: Some overlap  in boiling ranges
of NORCO plant products, with less precise  fractionation, would
be expected.)
                               43

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NORCO Fractions - Physical Properties
Frac-
tion   Name

 1    Naptha

 2    Baro-
      metric

 3    Light
      Side-
      stream

 4    Heavy
      Side-
      stream

 5    Bottoms
Residue Water
        Loss
                   Viscosity
Amount %           Saybolt      Boiling     Specific Flash Pt.
   of              Seconds      Range of    Gravity     of
Feed Stock  Color  Univ. (SSU)  Init./Final (g/cm3)  Open Cup,
                                             .7972
  1 1/2                         145 - 446    46 API
  9

  36



  28



  22
 41/2  33-34@ 100F 400 - 680

 8      100 @ 100F  680 - 792
        39.1 @ 210F
        222 @ 100F  792 - 900
        47.6 @ 210F
Dark
284 Sayb.
Furol
< 122F
900 - up
  3.5
                          .8602
                          33 API

                          .8735
                          30.5 API  350
                          .8789
                          29.5 API  430
.9937
10.9 API
                                  1.0
                                  10 API
               Total
               100%
                            Table  3.
                                             Av.  S.G.
                                             Feed Stock
                                             .9035
                                             25.1 API
The naptha and barometric fractions may be used as solvents, thinners
or in the blending of fuel oil and diesel fuel.  The light and heavy
sidestreams can be considered to be for various products such as
lubricants, diesel fuel, rubber extenders or as vehicles in paints,
coatings and sealants, and as plasticizers in the plastics industry.
The goal is to provide extensive pretreatment so the bottoms will
contain negligible residues of additives as well as colloidal matter
(mostly carbon).   In this way, it can be used as a fuel oil without
deleterious effect or need for mixing or monitoring.  Alternately,
the bottoms may be further cleaned for use as lubricants or any of
the above-mentioned compounding applications.  Their higher viscosity
and flash point make them well suited as heavy blending components.
                              44

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Analysis of the first four fractions shows the complete absence
of particulate matter and metal ions.  However, residual odor and
color are present.  These properties appear generic to olephines
and asphaltines.  These contaminants are presently removed by an
adsorption process known as "clay treating."  However, in order to
avoid the ensuing clay waste, we propose to explore the use of
solvent extractions and column chromatography.

The ecological error in clay treating is best illustrated by the
fact that upward of 1/8 Ib. (approx. 50 grams) of clay are used
per gallon of oil in order to remove less than 1 gram of odor and
color-carrying organic material, which could be easily incinerated
were it not for the inorganic adsorbent.

Further investigation relating to odor and color in the distilla-
tion fractions led to the development of solvent extraction as a
non-polluting, non-residue producing method in place of clay treat-
ment.   It was found that selective  solvents for olephines and
asphaltines, are capable of pulling  these contaminants, as well as
water,  out of the oil.  The dirty solvent is  then separated by
decanting and recovered by distillation  (solvent recovery).

Hydrogenation presents an alternate approach  to the above-mentioned
methods, and its ability to change  the offending organics  into
aromatics  is not  seriously questiond.  However, the economic
viability  of hydrofining vs.  extraction  is open to question.  Also,
the equipment needed  to carry out this process is of  necessity
expensive, complex and not generally available in small refineries.

A Discussion of Results and Recommendations

Producing  several  petroleum  fractions having  discrete boiling
point  and  viscosity  ranges may prove to  be  quite  unnecessary
 for a  successful  product  development program.

 In this connection,  one may  question the need for  distillation,
 except as  an established  economical fractionating means.   Since
 it appears quite feasible to remove the additives,  particulate
 matter, as well as color  and odor carriers by emulsification,
 filtration,  solvent extraction, electrophoresis,  membrane dialysis,
 coagulation and centrifugation or settling,  the case for  distilla-
 tion is not clearly established.  In fact,  there is a tempting
 notion that it should be possible to tailormake a process for the
 disposal of a variety of industrial waste oils by combining
 several of the.above methods.

 A further process alternative is suggested for consideration.  The
 distillation of incoming lube stock, without pretreatment, results
 in an accumulation of additive and particulate matter in the bottoms

-------
These could be ignored altogether, as a potential source of revenue,
and incinerated.  Such a notion becomes even more attractive if the
quantity of this fraction is reduced from 22% to 10% by suitable
changes in the distillation temperature ranges.

Proposals solicited from THE ENGINEER CO. and THERMAL RESEARCH AND
ENGINEERING CORPORATION evidence the availability of commercial
equipment at reasonable cost where an incineration method is
indicated.

If products can be found that do not need to be deodorized or
decolorized after distillation, there emerges an extremely simple
reclamation scheme requiring no pretreating.  For the conversion
to carbon black, oils need not be odor or color-free, but the
admission of metallics from additives seems out of the question.

In order to make reclamation possible, all carbon and hydrocarbon
matter must be separated from organic as well as inorganic con-
taminating particulate and additive material.  This could be
difficult.  It may prove economical and perhaps even very profitable
to produce industrial grades of carbon black from tank bottom resi-
dues.  (See Product Creation below)

Finally, the exploitation of additives promises a source of revenue
to be investigated.  Our research has shown approximately 2-3% by
weight of "dry mud" can be collected from the incoming waste oil.
This is equal to roughly 9 Ibs. per barrel (approximately 42 gal.
or 360 Ibs.).  This material represents metals primarily in car-
bonate and phosphate form which can be extracted.

We have no knowledge about the economics of such a process.  How-
ever, at worst, incineration can yield a clean landfill, abrasives
and anti-skid coatings.  From the organic state, fertilizers and
salts for ice and snow removal may be precipitated.

From the foregoing, it is clear that regardless of this last
reclamation phase, it is necessary to complete the clean-up and
separation of the incoming waste oil into compounds which may
logically lead to further exploitation.  We hope to be able to
show that this can be accomplished profitably and without violence
to our environment.  At any rate, incineration is generally an exo-
thermic process from which heat can be realized for the refinery
operation.

In summary, the NORCO process is sufficiently effective and flexible
that with new and added equipment, it should be able to recover
over 90% of the collected waste oil, without residual waste and
at a lower cost than existing methods allow.  Moreover, it utilizes
existing process equipment and is, therefore, not dependent on
technological breakthroughs.

                              46

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Product Creation

If this project is continued, it is probable that the NORCO
refinery products will be upgraded to a market potential to be
sold competitively as petrochemicals to the paint-sealant,
plastics and rubber industries.  As explained elsewhere in this
report, extensive investigation of the foregoing possibilities
reveals that these potential markets have never been tapped by
the re-refining industry.  The added advantage of the use of
re-refined products in these potential market areas is that the
re-refined lubes will not return to haunt the environment as a
waste lube oil, as it will be totally consumed in these petro-
chemical uses.  The present re-refined lubes which are primarily
for automotive uses do come back to pollute the environment as
waste lube oils.

The rubber, paint-sealant-coatings, plastics, carbon black and
special fuel industries can absorb more than the entire annual
crankcase waste oil accumulation in the United States and, if
the know-how to produce petro-chemicals from waste crankcase
oils can be demonstrated, these industries would be the most
logical market for the re-refiner  to consider.

Operational Analysis  of the Projected Refinery

The proposed process  may  be carried out in a typical re-refining
facility capable  of processing  1,000 barrels/day  (42,000  gallons)

   Collection  Costs                                3c/gallon
     This  is a maximum  figure  and  does not  include
     allowances  for BS&W (10-15%  of  the collected waste).

   Wages                                           l<:/gallon
     Based on  3  shifts,  3 men  per shift @ $50/day,
      including workman's  compensation,  social  security
     and  fringe  benefits.

   Utilities, Maintenance and Repairs                lO/gallon

   Overhead,  Management. Insurance & Sales Costs    lc/gallon

   Depreciation,  Contingencies, etc.                 lC/gallon

   Total Operating Costs  (not including pre-
   treating or special extraction steps             7(?/gallon

 Oil Collection Data

 The independent collector, probably the main supplier of most

                                47

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  re-refiners, can gather about 3,000 gal/day.  He is paid 2-3<:/gal.
  by the service stations for removal, plus 3c/gal. at the refinery.
  His daily receipts, therefore, amount to approximately $180.

  The proprietary truck fleet operator can expect to collect about
  3,000 gal/day/truck at a cost of approximately $100-125/day/vehicle.

  Availability and geographic limitations indicate a practical
  collection radius of 50 miles (7,500 square mile area) for direct
  truck pickup and delivery to the refinery (*Af below), over 100
  miles (37,500 sq. mi.) if trailers are used to pick up the oil
  from collection storage depots ('B1 below).

  Under 'C' below, we attempt to show how a truck can successfully
  cover a collection route of up to 150 miles (60,000 sq. mi.) radius
  over several consecutive days of operation, or involving the use of
  a fleet of several trucks concurrently.
           (A)
(B)
(C)
                                  TRUCK-ROUTES
AREA COVERAGE:
       7.50O SQ. Ml.
                               37.5OO SQ. Ml.
                                                      60.000 SQ Ml.
                              Figure 3.
                                 48

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                            LABORATORY

                                OF

                        ARTHUR M. SIEGELMAN

  Telephone                                            62 Dosoris Way
516 - OR 6-9248                                     Glen Cove, N.Y. 11542

                                          October 16, 1970


  INTERIM REPORT - ANALYSIS OF SAMPLES #8U and #9U:

  The following report is a partial one, pertaining only to the
  principal metallic constituents of these two samples.

  #8U - marked "Bottom no additive" is one of a NORCO distillation
  series.
          Analysis:
  A)  1) microscopic - by polarizing interference microscopy
      2) michrochemical
      3) microphysical (magnetic, hardness, density, etc.)

  The following are participates in approximately decreasing order
  (as to estimated total particulate volume).

  a) Abundant (accounting for over 99.9 percent of the particles and
     about 96 percent of the particulate volume - other than carbon)
     Ca  (1) as various phosphates
         (2) as carbonates, rarely sulfates
     Ba  (1) as carbonates
         (2) much less as phosphates, etc.
     Pb  (1) as the oxide
         (2) much less as the sulfide, etc.
     Fe  (1) as hematite
         (2) as magnetite; OH, CO^, etc.
     Zn  (1) as the oxide
         (2) much less as sulfide, carbonate, etc.
  b) Intermediate
     Mg  (1) oxide, phosphate, carbonate, rarely sulfate
     Al  (1) oxide, silicate
     Na  (1) silicate, oxide
     Cr  (1) oxide, inchromate
     Sn  (1) oxide
     Cu  (1) oxide, sulfide, carbonate
  c) Rare (less than 0.5 percent)
     Nl  (1) oxide, phosphide, sulfide
     Mo  (1) present both as a metal and in the Molybdate radical

  Note:  occasional particles of free metal - also present

                              49

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B)  Emission Spectrographic Analysis, etc.

Ion           mg percent       Calculated wt/wt percent  (to total ash)

Ba               892                        16.0
Ca               852                        15.2
Pb               380                         6.8
Zn               140                         2.5
Fe               140                         2.5
Mg                64                         1.2
Al                52                           .9
Na                42                           .8
Cr                21                           .4
Sn                16                           .3
Cu                13                           .2
Ni                 9                           .06
Cd                 3                           .05
B                  2                           .04
Mn                 2                           .04
Sb                 1                           .02
Cu                 1                           .02
K                  1                           .02
In                 0.2                         .004
Ag                 0.1                         .002
               2,631.3    equals 2.6%         approx. 46%
P                279   (as the oxide and               5
                        in phosphates)
Si                12   (as oxide and in silicates)       .2
Mo                 8   (as methal and in molybdate)      .15
S                793   (as S, H2S, oxide and in
              	sulfides and sulfates)        14.0
               3,723.3    equals 3.7%                  approx. 65%
Total ash (carbon free) equals 5.6 percent.

NOTE:  1)  0, H and C in inorganic radicals equals about 1.9 percent.

       2)  Approximate ratio of metal to nonmetal probably about
           2.8: 2.4 indicates phosphates and carbonates predominate
           over oxides.

       3)  It is likely that almost all  (certainly over 90%) of the
           above metals are particulate.  This should be investigated.

       4)  Dissolved metals are probably Na, Ca, and Ba.
                             50

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#9U - This sample consists of hard, dense, coarse, irregular
masses of a mineral-like conglomerate; predominately gray with
reddish and brownish streaks; the surface powders readily with
hardness appearing to range from about 2-4 (MOHS) ; the core and
some streaks leave sizeable particles (up to about 2-3 mm) rang-
ing from about 4-8 (MOHS).

This sample is the residue from the burning of a  sample similar
to #8U in an industrial boiler.

Reference A) -Microscopic, etc. (as for #8U above) - examination
ground particles - reveals an extensive array of  inorganic mineral
compounds, and suggests formation in layers at highly variable
temperatures and oxygen availability (outer layers, for example,
show C20; inner layers, Ca(X>3; CaC03 converts at  900C.

Free carbon is negligible, consisting of less than .01 percent
of the particulate volume; no free S is detected.

Oxides are considerably higher than in #8U; sulfides are much
lower than in #8U.
Principal constituents:  Ca - phosphate  (various); CaC03,
Ba - PO^  (various) PbO, PbOo (indicating low temperature areas).
PbS, Pb in complexes, e.g. (spinels); 6263 (hematite); Tfe^Q^,
FeO; ZnO, ZnS.

Others:  P, ?205'> Mg> MSO^; Al  (as oxides, silicates, spinels
and conjugates) (^203; SnO; CuO;  Cus: various Na salts; Si - 0.

Rare:  Sb, Ni, Mn, Cd, Co. - various

At least 65 different compounds have been identified.

Note that a given mineral array will depend not only on the
initial sample, but also on the temperature and available oxygen.
                              51

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Reference B) Emission Spectrography

                     Percent wt/wt
Ba
Ca
Pb
Zn
Fe
Mg
Al
Na
Cr
Sn
Cu
Ni
Cd
B
Mn
Sb
Co
K
In
Ag

P
Si
Mo
               13.8
               26.3
                6.8
                3.9
                5.7
                1.6
                1.4
                 .7
                 .5
                 .6
                 .3
                 .9
                 .2
                 .03
                 .13
                 .03
                 .08
                 .17
                 .02
                 .02
Approximately  63 percent
                9
                 .6
	.05
Approximately  73 percent
C, 0, H and S are approximately 27 percent, indicating that oxides
are higher by comparison with #8U, i.e.  (mean molecular wt. of non-
metals has dropped).

COMMENTS:

A)  Apparent discrepancies between the percentages calculated for
the two samples may be due to the following:
    1)  The samples are not from identical sources.
    2)  "Bottom" samples will vary with  time of sampling,
        i.e. (temperature, oxygen, etc.) and sampling techniques
        i.e. (mixing).  For example, particles of greater weight
        and/or density settle out faster, while total ash determina-
        tion accounts for particulates and solutes both.
    3)  "Residue" samples will similarly vary with location of
        sample with respect to temperature, oxygen, updraft
        gradients,  etc.
    4)  Total ash (for either sample) varies with technique,
        i.e. (temperature, oxygen, etc.).
                             52

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     5)  For #9U, some substances may be lost as volatiles and
         fly-ash particles.
     6)  Higher percentages, in general, are expected for #9U
         because conditions allow for greater initial oxidation.

B)  It is likely that high oxygen, high temperature incineration
would yield a higher percentage of metals, but oxides would
predominate.

C)  It is recommended that dilution-centrifugation and/or
dilution-filtration techniques be investigated and, as the
initial data seems to indicate, if recovery of metal particu-
lates exceeds 90 percent of that found by ashing, such techniques
should be used in preference to recovery from burning of "bottoms"
because:
     1)  High metal concentration in the feedstock boiled for
         distillation will act catalytically in a number of
         indefinite and uncontrolled reactions.
     2)  High metal concentration would tend to poison, perhaps
         irreversibly, most of the adsorbants that could be
         used at any step in recovery, i.e. (removal of odor
         or color by various "clays").
     3)  Metals obtained by dilution-centrifugation and washing
         would be in a form that would probably be more easily
         recoverable from their compounds, i.e. (C03, OH, S
         504, etc.) than from the highly oxidized forms.
                     Hard Rock Clinkers
                          Figure 4.

                              53

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                          SECTION X

                  SPECIFIC RECOMMENDATIONS

The following are detailed and specific recommendations based on
information gained during NORCO plant operations in refinery runs
1-11, on conferences held with vendors and their engineers, and on
a survey of the available subject literature.

Furnace

A new furnace design is required which will be more efficient and
require less maintenance.  Furthermore, the pipe still heater for
waste crankcase oil processing should be designed to charge cold
oil directly from a mixed feed tank to a large convection section
at relatively low velocities, which can be increased with increases
in temperature.  Tubes should be equipped with headers for cleaning.
Variation in charge feed and unknown future possibilities rule
against closed furnace coils and steam-air decoking without consid-
erable plant experimentation and development, both of which are
costly.

Preheat, by heat exchange with product streams, at this stage of
waste oil plant development, should stand on its own economic feet,
and not be thrown into process development.  If recovery of heat
from products is thought to be economic, it might first be applied
to generation of steam, usually required for treating sludges,
emulsions, BS&W, and for firing furnaces, burners and incinerating
wastes.  Steam is often produced from waste heat in petroleum re-
fineries where there are fewer unknowns.

The main furnace for vacuum distillation should provide for fairly
high mass velocities in furnace tubes, and the reduction of mass
velocity just ahead of the transfer line, to provide for consider-
able vaporization in tubes.  Tubes equipped with headers and
removable plugs are again advisable.

The radiant heat transfer rates should be kept quite low to avoid
quick fouling of tubes, say at 5,500 BTU per sq. ft/hr on outside
areas.  Whether or not separate heaters should be provided for each
heating and incinerating duty, depends on what is available.  There
are advantages and disadvantages in separate units.  Separate fur-
naces are more flexible, more available, and many even cost less
since they are not necessarily custom jobs, whereas, a combination
two or three coil unit with incinerating burners, etc. will almost
certainly be specially designed.  Delivery time would probably be
longer.  In any event, handling, labor and attention required on
the part of operators must be cut to a minimum, but not by attempt-
ing heavily instrumented automation; that is, for major refineries.

Special attention must be paid to collecting, transporting and
firing the difficult waste materials which are incinerated.  Also,
                             55

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attention must be paid to removal of particulate metallic dust
and solid matter from flue gasses, and transporting of incinerator
dust and solid matter to avoid nasty, dirty, depressing surround-
ings, characteristic in the past of re-refining.  Shoveling,
scraping, moving with a wheel barrow, clearing of plugged lines,
sweeping, thawing out lines and wiping, all have one common denom-
inatorthey all cost too much.  They are to be avoided by instal-
ling sloped bottom and cone bottom tanks, proper drainage systems
for tankage, vessels, pumping, slopping, shutdown and startup
draining, and all the little nasty, time-consuming details required
to handle the difficult end of re-refining procedures.  In the past
this housekeeping end of re-refining has been shoved into the future
by piling up clay, dumping into lagoons, or letting acid and oil
seep into the ground, but the future has a way of pushing the stuff
right back into the present.  Apparently, the future has its own
plans.  The best time to work with the future, as regards house-
keeping details, is when the experience of plant operations is
being detailed into drawings.

Incinerator

An incinerator for the NORCO processing plant would have to accept
the following products:

     1.  Tar, which is a special material because of stickiness
         and tensile strength.
     2.  Tank bottoms containing solids or semi solids.
     3.  Emulsions from tanks; liquid or semi-liquid.
     A.  Acid water from crankcase dehydration, or neutral water
         containing oxygenated hydrocarbons.

It would have to have special burner, transportation and exposure
arrangements for solids, and it would probably be similar to a
cement kiln for handling solids and semi-solids, and be provided
with special burners for emulsions and tars, plus be provided with
spray-in devices for phenolic and acid water.

Conveying arrangements for getting solids into the incinerator and
removing them from the incinerator would be required.

Satisfactory particulate matter removal equipment would be re-
quired for flue gases with suitable solids handling conveyors, and
a bin or bins, plus associated equipment, required for transporting
the solids into a tank truck.

Considerable shopping around and after-purchase debugging, or
development, would probably be required to produce a satisfactory
incinerator calling for an economic amount of attendance.

                              56

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Air-Cooled Coolers and Condensers

Air-cooled coolers and condensers should certainly be tried out
as the cooling required permits relatively high outlet cooler
temperatures, which air coolers economically provide.  The great-
er part of the cooling load would not require cooling below 140F,
while 160F might be acceptable.  Dehydration and removal of naptha,
if diluted feed or bottoms are centrifuged, can readily be per-
formed at 800 MM Hg down to 200 MM Hg at condenser coutlet tem-
peratures of 120-130F.  If economic, a small refrigerated cooler
might be installed before the suction of the motor-driven vacuum
pump - if dehydration and naptha evaporation is not performed at
800 MM.

In the case of the Vacuum Fractionator, if operated at 5-10 MM,
a small refrigerated cooler, installed before the inlet of the
motor-driven vacuum pump, would be desirable.  Minimum economic
temperature in an air-cooled condenser outlet would be 105F in
hot weather.

A small refrigerated condenser would be practical for reducing the
temperature further - to about 40F.  The heat quantity involved is
small.  The control specifications, as furnished by a large air-
cooled cooler manufacturer, show clearly that the manufacturer is
well aware of the need for simple rugged instrumentation for air
coolers in duties where instrument maintenance service is not
economically available.

This manufacturer has also produced skid mounted, modular pre-
fabricated cyrogenic processing plants for natural gas processing,
with one man in operating attendance in the gas fields.

Available in chemical and petroleum processing technical magazines,
are reports on the economy of operation of air-cooled coolers, in-
cluding variations in very hot areas with ambient temperatures of
100-110F, where air is economically cooled by evaporation of a
minimum amount of water to provide product outlet temperatures
at 1000F.

Vacuum Pump

Steam actuated vacuum jet pumps are not desirable for a waste
crankcase oil plant.  A three-stage installation, with two inter-
condensers and a final after-condenser, would be required for a
5-10 MM vacuum.  High pressure, 90-100 psig steam would be needed.
Water treatment, licensed boiler attendance, blow-down disposal
to avoid pollution, feed water testing, etc., would also be required.

Motor-driven vacuum pumps which will operate at 5 MM Hg are avail-
able.  We recommend installation of such a pump to replace steam
jet vacuum pumps.

                              57

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Fractionation

As it is planned to provide some head-end treatment to remove the
suspendid solids prior to processing, it is extremely difficutl to
know exactly how to proceed with fractionation arrangements.  Until
the apparatus and process for dealing with the tar problem are more
fully developed, the fractionation unit process will have to be
somewhat flexible.  At best, this unit process will require rela-
tively extensive development and modifications.  For example, at
the moment, the best arrangement would be to go ahead with the
transfer line from the Fractionator Furnace discharging into an
efficient cyclone, at about 5-20 MM Hg.  Vapor coming out of the
cyclone goes to a series of air cooled partial condensers with
horizontal tubes.  If we find cases of severe trouble with fouling,
the tubes might be pitched down or placed vertically.  In case of
no fouling, tubes could be pitched up or vertically, providing
liquid refluxing and probably the equivalent of a fractionating
tray.  At low absolute pressure, and high differences in relative
volatilities of compounds, the fractionating effect of a fraction-
ating tray or partial condensation is greater than at higher
pressures.

It should be noted that the existing Vacuum Fractionator heavy pro-
duct section is provided with two trays located above the cyclone
separators, both six feet in diameter:  the bottom bubble cap tray,
provided with a liquid drawoff pan; and a glitsch ballast top tray.
Circulating reflux is fed to the top tray and reflux and products
are drawn off the bottom tray.  The total fractionating effect is
probably about like that of a partial condenser.

The Vacuum Fractionator light product section is provided with
three spray decks, each four feet in diameter, over which circula-
ting reflux passes.  Circulating reflux is fed to the top spray
deck and circulating reflux, plus light product, are drawn off a
catch pan below the bottom spray deck.  The fractionating effect
is obviously limited, probably not greater than that of a partial
condenser.

Waste crankcase oil contains substantial amounts of solids.  Addi-
tive suppliers say the additive materials break down to yield
solids in the range between 400-700F.  At 7009F, breakdown is
rapid and substantially completed within a few minutes.  The effect
of presence of NaOH with exposure to temperature is not fully known,
It is known, however, that crankcase oil which has been diluted and
centrifuged, and vacuum distilled at temperatures between 600-700F
does not yield a fair amount of additional solids.  Some investiga-
tion indicates this is largely carbon.  Further work would be re-
quired to predict whether future air quality standards require
removal of this material to meet heavy fuel oil specifications.

                                58

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Rotary positive displacement pumps of several types are recom-
mended for use with cold and warm waste crankcase oil, and also
with the bottoms stream.  Very stiff bottoms requires short
suction lines.

Rotary pumps stick and jam on even small quantities of the tar
produced in the Vacuum Fractionator or strippers.

Centrifugal pumps, with suction lines under the vacuum are recom-
mended for use on hot light and heavy products, and also on reflux
containing tarry material.  The lantern gland in the hot oil stuf-
fing box should be provided with a supply of cold oil under a
slight positive pressure to avoid air leakage into the pump suction.
Adequate piping for venting and discharging back to the suction
vessel should be provided to get and maintain flow, particularly
when starting up the operation.

Centrifugal pumps also do well on light and heavy products being
pulled from storage tanks.

The present NORCO Fractionator bottoms pump is an all steel, side
pot valve simplex steam reciprocating pump.  There is very little
suction head available.  While the pump runs reasonably well, a
variable speed motor-driven reciprocating hot oil pump, to save
on steam, would be preferable.

Other Specific Recommendations

The results of the completed studies indicate that the quality
of the products and bottoms can be increased if the suspended
colloidal and dissolved organics and metallic compounds can be
removed prior to processing.  Accordingly, treatment and/or
physical removal equipment is required at the charge stock end
of the process system.

Present lube distillates are dark and emit a slight odor.
Double distillate runs indicate that the recommended head-end
handling will increase the quality of the product streams and
the color and odor specifications of the products.  Diesel
runs should be included to unify the quality of the light pro-
duct and its effect on diesel engines.

Removal of the polymers and metallics at the head-end should
produce a bottoms product with an acceptable solids level and
with minimal sulphur to make it compatible with burning equip-
ment.  Controlled burning tests should be conducted to determine
if any limitations on the use of the bottoms exist.

                           59

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Centrifugation, solvent extraction, chemical treatment equipment
or a combination of these concepts should be installed in the
head-end of the plant.

The head-end treatment will permit greater furnace temperatures.
This design will also mitigate coking, permit greater extractions
of product and longer, more reliable runs.

Provide a furnace with optimum flow velocities through the tubes,
thus avoiding coking and erosion and resulting in an increase in
percentage of product stream recovery as well as increase 'on
stream1 time and reduce 'down time.'

Provide a plant waste converter to condition solids, emulsions
and all plant wastes into materials meeting pollution standards.

Install a motor-driven mechanical high-vacuum pump to reliably
maintain the vacuum required which will increase the quality of
the sidestream products and improve the length of runs.  This
would also eliminate the high pressure boiler apparatus and a
costly licensed engineer.

Replace existing water-cooled condensers and coolers (to eliminate
water cooling from plant operations, as present water quality
standards are difficult to meet) with new air-cooled condensers
and coolers or circulating water cooling systems.  Some would meet
national refinery concept criteriaas inland refineries need not
rely on hard to obtain water sources.

Conduct runs necessary to determine optimum flow sheet conditions.

Subject products produced to use testing so as to accumulate
testimonial data for market acceptance of "special fuel" and
"special lube" products.  In this regard, a close affiliation with
an accepted petroleum oriented testing laboratory is recommended.
                             60

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                         SECTION XI

                  GENERAL RECOMMENDATIONS

Crankcase disposal plants have, in the past, been catch-as-catch-
can, makeshift, haphazard affairs.  In the design of future plants,
attention should be paid to details, such as:

1.  Topography and geology of the selected site, to avoid under-
    ground movement of liquids.

2.  Grading for drainage, prevention of fire hazards, losses by
    leakage from tank or personnel failure.

3.  Surface water drainage, collection, separation, treatment and
    final disposal.  Loading and receiving arrangements for good
    housekeeping and low fire hazards.

4.  Design of vessels and tanks for economic settlement and trans-
    portation of B.S.W. sediment and all other waste materials.

5.  Collection and disposal of vapors, fumes, flue gases, etc.

6.  Placement of drainage sewer lines to avoid freezing, permit
    economical cleaning, etc.

7.  Fire protection criteria for this scale refinery should be
    developed for operation by one or two men, with provisions for
    access by fire department equipment.  A guide list should also
    be developed such as used in petroleum refinery or chemical
    plant design which would serve as a practical designer's re-
    minder list.  API publications and Chemical Industry publica-
    tions would also be helpful.
                              61

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                              SECTION XII

                              APPENDICES

                                                       Page No,

A.  Preliminaries to Startup	    64

B.  Startup Instructions 	    66

C.  Instructions on Controlling Product
    Specifications 	    69

D.  Shutdown Instruction 	    72

E.  Cleanup Instructions 	    74

F.  Emergency Procedures 	    82

G.  General Fire and Safety Instructions	    85
                               63

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                                                                  Who
A.  Preliminary to Startup                          Done  When  Initial
Mix feed tank 	
Complete all lubrication items  ....
Complete all instrument air items . .  .
Clear all level glasses and connections
Clear all stripping steam distributors
Clear all suction lines 	
Clear gland oil connections to pumps
Fill gland oil tank 	
Clean all burner fuel screens 	
Clear all pump casing vents 	
Steam blow & clear light & heavy reflux coolers,
  lines, and control valves.  Repair, fix leaks . .
Steam blow & clear light & heavy reflux coolers,
  lines, and control valves.  Repair, fix leaks . .
With top fractionator manway open, circulate light
  reflux.  Make repairs or clean as needed to pass
  inspection  	
With both fractionator heavy cut section manways
  open, circulate heavy reflux  	
Make repairs or clean as needed to pass inspection.
Clean all strainers on list 	
Pressure test Flash Furnace at 30 psig with steam  .
Pressure test Fractionator Furnace at 50 psig
  with steam  	
Drain all items on drain list 	
Check vacuum pumps as required  	
Close unit  	
Put boilers on H.P. steam  	
Close cooling water system  	
Fill gland oil tank on cooling water pump 	
Start cooling water pump   	
                           64

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                                                                  Who
Preliminary to Startup  (continued)                 Done  When  Initial

Put steam test on unit & repair leaks as required .

Drain all items on unit drain list  	
Test Flash and Fractionator Vacuum pumps against
  shut suctions.  Repair as required.  Get 29.2"
  vacuum  	

Open stripping steam line; hold 12 psig steam
  pressure against stripping steam distributor
  valves; crack steam drains at bottom of Frac-
  tionator on 3" line, and at end of 3" line at
  heavy cut stripper  	
Put vacuum test on Flash Tower and Fractionator;
  repair as required.  Get 28.9" Hg vacuum  .  .
                            65

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                                                                  Who
B-  Startup  Jnstruetions                           Done  When  Initial

Establish flow from Feed Tank through Flash
  Furnace and Tower  	
Establish flow from Flash Tower through
  Fractionator 	
Establish flow from Fractionator Bottom to pump,
  cooler and feed tank 	
Check over system, note leaks and other items

Stop feed flow as required, repair leaks and
  other items  	
Re-establish feed flow through Flash Tower and
  Fractionator as required 	
Fill light & heavy reflux tanks & light settler  ,

Establish flow through light & heavy make coolers
  and note repair items	
Repair light and heavy reflux flow as needed .

Check over light & heavy reflux systems and
  note items 	
Stop light & heavy reflux flow; make repairs as
  needed 	 ,

Re-establish light & heavy reflux flows and leave
  flowing	,

Start cooling water flow to pipe coils in box
  coolers  	 .

Adjust Flash and Fractionator Furnace dampers;
  leave stack dampers wide open	,
With feed flowing through unit, start Flash
  Furnace burner 	
With feed flowing through unit, start Fractionator
  Furnace burner.  After fire is established,
  start blower discharging up stack.  Gradually
  get flue gas recirculating, and stop discharging
  to stack 	

                           66

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                                                                  Who
Startup  Instructions (continued)                   Done  When  Initial

When Flash & Fractionator Furnace transfer lines
  are up to 180F, start stripping steam into
  bottom of Flash Tower, bottom of Fractionator,
  and into expansion joint in Fractionator Furnace
  transfer line.  Keep raising both transfer line
  temperatures  	

Adjust flow of feed to unit at rate specified in
  log book instructions  	
Bring up Flash & Fractionator transfer line
  temperatures as fast as possible, maintaining
  light & heavy reflux flows to hold specified
  Fractionator top temperature 	 ,
Increase stripping steam flows as transfer line
  temperatures go up, unitl the specified strip-
  ping steam is flowing into Fractionator bottoms
  and Flash Tower  	 ,
When levels in Light & heavy cut strippers begin
  to build up, line up flow and discharge to slop
  tank	

When Fractionator bottoms reach specified API
  gravity, pump bottoms to bottoms tank  	
Put stripping steam flow specified in log book
  into light & heavy cut strippers 	
Keep close watch on Flash and Fractionator
  bottoms levels 	
When Fractionator light & heavy cuts from strip-
  pers reach specified gravities and colors, pump
  to light & heavy cut make tanks  	
Now hold operating temperatures, flows, pressure
  vacuum, etc. steady; vary only to maintain pro-
  duct streams as specified in log book  	

Keep barometric oil accumulating in oil-water
  separator skimmed off and pumped into baro-
  metric oil tank  	
Keep water drained off barometric oil tank . . . .
                           67

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                                                                  Who
Startup  jCnstrucjj^ns (continued)                   Done  When  Initial

Every two hours, look into furnace fire boxes for
  hot spots (black spots) on furnace tubes or
  coil.  If found, adjust burner, dampers, feed
  flow, steam into feed going through furnace
  tubes to maintain furnace inlet pressure, and
  reduce black area on tube; avoid operating con-
  ditions that result in large black areas on
  furnace tubes.  Note situation in log book.  Do
  not operate with large sections of tubes black
  and overheated 	
Hold 200-210F temperature at the bottom of the
  Flash Tower at 19.0-21.0" Hg vacuum  	
                             68

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C,  Instructions on Controlling Product Specifications

Regulate Naptha, API gravity, end point and yield by adjusting
the Flash Furnace transfer line and the Flash Tower stripping
steam flow and vacuum.  Usually, the Vacuum jet pump will be
left with the steam flow to the pump set, and not changed except
under unusual circumstances.

Regulate API gravities, viscosities, flash points and yields of
bottoms, heavy cut, light cut and barometric oil by adjusting the
Fractionator Furnace transfer line, the Fractionator vapor tem-
peratures with light and heavy section vapor temperature control-
lers controlling flow of heavy reflux, light reflux and steam to
light and heavy strippers.

Note:  Hold stripping steam flow to light and heavy strippers
steady by putting pressure controller on stripping steam in
operation.
Flash Tower

Change

Raise flash furnace
transfer line temperature.
Increase stripping steam flow
(the stripping steam flow is
adjusted mainly to control the
flash point of the barometric
oil).

Increase vacuum on flash tower,
Fractionator

Raise Fractionator  transfer
line temperature.
        Results, Assuming One
          Change at a Time

API gravity of Naptha decreases.
End point of Naptha increases.
Flash point of barometric oil
increases.  Viscosity of Naptha
increases.  API gravity of baro-
metric oil tends decrease.  Vis-
cosity of barometric oil tends to
increase if fractionator conditions
are steady.  Initial boiling point
of barometric oil increases.  Flash
point of barometric oil increases.
Flash and initial boiling points
of barometric oil will increase.
All other specifications will change
as above, but only slightly, unless
change in steam flow is large.

Same as for raising Flash Furnace
transfer line temperature.
API gravity on all products:  Bottoms,
heavy cut, light cut, barometric oil,
goes down.  Viscosity on all above
products goes up.  Flash point on all
above products goes up.  End point on
all products goes up.  Initial boil-
point on all products goes up.  The
yield of bottoms decreases.
                             69

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Increase vacuum on
Fractionator.
Increase stripping steam
flow to bottom of Fractiona-
tor, mainly to reduce the
yield of bottoms, but also
to raise the flash point and
incidentally lower the API
gravity of the bottoms and
raise the viscosity.
Raise vapor temperature
above top heavy reflux
bubble tray (hvy. reflux
flow is reduced).
Raise vapor temperature
above top light reflux
bubble tray (It. reflux
flow is reduced).
Increases stripping steam
flow to heavy cut stripper,
Same as above.  However, vacuum
pumps are usually operated to pro-
duce maximum possible vacuum.

The bottoms specifications will be
most affected.  Gravity goes down.
Yield goes down.  Viscosity and
flash point of bottoms go up.
Heavy cut, yield, viscosity & flash
point go up; API gravity goes down.
Light cut yield goes up some; API
gravity goes down; viscosity and
flash go up. Barometric oil yield
goes up some; gravity goes down.
Viscosity and flash point go up
slightly.

Bottoms API gravity goes down some-
what.  Bottoms yield goes down some-
what, while bottoms viscosity and
flash point tend to go up.  Heavy
cut yield and API gravity go down.
Viscosity and flash point go up.
Light cut yield, viscosity and flash
point go up and API gravity goes down.
Barometric oil yield, viscosity,
flash point and API gravity remain
unchanged.

Bottoms are unaffected.  Heavy cut
yield and API gravity go down very
slightly, while viscosity and flash
point tend up.  Light cut yield and
API gravity go down; viscosity and
flash point go up.  Barometric oil
yield, viscosity, flash point, in-
itial boiling point and end point go
up, while API gravity goes down.

Bottoms are unaffected.  Heavy cut
flash point goes up.  Heavy cut vis-
cosity goes up very slightly, but
heavy cut gravity and yield go down
very slightly.  Light cut flash
point and viscosity tend to go up
slightly, but light cut gravity and
yield change very little.  API gravi-
ty goes down very slightly.  Baro-
metric oil end point goes up slight-
ly, while API gravity goes down very
slightly.
                             70

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Increase stripping steam         Bottoms and heavy cut are not affect-
flow to light cut stripper.      ed.   Light cut flash point goes up.
                                 Light cut viscosity goes up very
                                 slightly, while light cut API gravity
                                 and  yield go down very slightly.
                                 Barometric oil yield goes up very
                                 slightly.

Limitations

The flow of stripping steam that can be used is limited by the
pressure drop of the vapors going through the Fractionator, and
the tendency of excess steam to blow oil out of the stripper or
out of the light cut section, over the top of the Fractionator.
Steam cost is also a consideration.

The flash and Fractionator Furnaces transfer line temperatures are
limited by the tendency of furnace tubes to overheat.  It is very
difficult to insure even tube metal temperatures where an oil burner
flame radiates heat to tubes in a poorly designed furnace.  The
quantity of heat which can be absorbed by oil going through the
tubes is limited by the coke depositing tendency of the oil going
through the tubes.  A build-up of coke inside the furnace tubes
causes the tube metal to overheat.  The ash dust, normally present
on the outside of the tube, melts, causing the side of the tube
which is exposed to the radiation from the burner flame to become
black as the tube overheats.  When black spots and areas show up
on tubes, the transfer line temperature and/or the feed flow rate
must be reduced to avoid having the tube split, permitting oil to
leak into the fire box.  Turbulence in the oil passing through
furnace tubes is maintained when the oil flow is reduced by opening
the steam valve to pass more steam into the tubes.  Normally, as
the oil flow is reduced, open the steam valve into the oil feed
line, into the inlet pipe  to the furnace tubes, just enough to main-
tain the same furnace inlet pressure as before reduction of the oil
flow into the furnace tubes.

To repeat, black spots appear on tubes in the furnace.  Reduce oil
feed to the furnace 5-10%, and furnace inlet pressure will drop.
Increase steam flow into the oil feed to bring the inlet pressure
back up to where it was before reduction in the feed flow.  If black
spots do not fade, reduce  feed rate another 10%.  Add steam to oil
feed to maintain furnace inlet pressure.  If black spots do not  fade,
reduce furnace transfer line temperature by 10-15F.  Notify super-
visors, upon completion of above reduction of transfer line tempera-
ture.  In case of a sudden onset of evidences of overheating, with
reductions in flow and transfer line temperatures not effective,
shut down furnace burners  and proceed to  shut down the entire unit.

                                71

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                                                                   Who
D.   Shutdown  Instructions                            Done  When  Initial
Stop flash and vacuum furnace burners  	  ,

Open wide, all furnace, stack and burner dampers

Slop bottoms to feed tank  	

Shut off heavy and light reflux 	
Pump out heavy and light strippers and soaker
to product tanks  	
When cyclone deck temperature in Fractionator drops
to 425F, shutdown cold charge pump and flash tower
bottoms pump  	

Shut off all stripping steam valves to steam
distributors at flash tower, heavy and light
strippers, and bottom of Fractionator 	
Close stripping steam block valves at 100 psig main .

Open all stripping steam piping drains  	

Pump out bottom of flash tower to slop tank 	

Close all flash and vacuum furnace dampers  	

Open wide 100 psig steam valve to vacuum furnace oil
inlet.  Steam through tubes for 30 minutes  	
Open wide 100 psig steam valve to flash furnace oil
inlet.  Steam through furnace coil for 15 minutes . .

With vacuum furnace tubes wide open, steam blow
again for 30 minutes  	
With flash furnace coil wide open, steam blow
again for 15 minutes  	
With tubes and coil of vacuum and flash furnaces wide
open, continue steam blowing alternately for 30 and
15 minutes respectively, until you have blown through
both furnaces four times  	

Close off block valves on steam lines for blowing
furnace tubes and coil at 100 psig.  Steam main and
open drains on blowing steamlines 	
Open wide all air and flue gas dampers on both
furnaces  	 ,

Leave wide open to allow furnace interiors to cool

Remove brick from manways into interior of both
vacuum and flash furnaces 	 ,
                              72

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                                                                   Who
Shutdown Insturctions (continued)                    Done  When  Initial

Reduce steam pressure to vacuum jet pumps on flash
tower to 50 psig and allow steam to backflow and
bring both flash tower and Fractionator back up to
atmospheric pressure.  Then close off steam to
vacuum jet pumps 	
Shut 100 psig steam block valves on lines to vacuum
pumps.  Open steam drains on these lines 	
Pump Fractionator bottoms, heavy and light cut
stripper and soaker as low as possible, through
the pump and out the lines to the feed tanks ....

Put steam boilers on low pressure operation  ....

Pump flash tower as low as possible to slop tank,
through 1" direct line, pump slop tank to feed tank.

Shut down instrument air compressor  	

Open drains at instrument air tank, salt dryer, etc.

Pump naptha from flash tower barometric oil-water
separator tank to naptha tank  	
Shut down salt cooling water pump, drain pump

Drain salt-cooling water strainers and piping

Leave drains open	,

Drain water from cooling coil box  	
Close block valve at main on steam line to bottoms
pump and open drains on steam line 	
Open steam cylinder drains on bottoms pump, rod
through and leave clean and wide open  . . . . ,
                               73

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                                                                   Who
E.  Cleanup Instructions                             Done  When  Initial,

Open 3" caps on flash furnace coil and inspect.
Clean as indicated by inspection 	
Open 2 headers located on east side of vacuum
furnace, in bottom row of tubes.  When inspection
of above indicates, open last two tubes before the
transfer line and inspect.  If these two tubes
need cleaning, clean and proceed to open tubes
from back of transfer line towards furnace inlet
until tubes in upper section do not require
cleaning 	

In the lower tube section of the vacuum furnace,
in all of the six rows, open the two tubes closest
to the burner, inspect and clean as necessary  . .

Open the last two tubes in each row, as the con-
dition of the above two tubes closest to the
burner indicates and clean as necessary  	
Inspect vacuum furnace transfer line and clean
as inspection dictates 	
Open bottom manway of flash tower.  Clean suction
screen and bottom of flash tower  	
Rod through flash tower level glass and float level
instrument connections and blow them out 	
Inspect stripping steam distributor, cleaning as
required 	

Inspect 4" suction line to vacuum furnace feed
pump and clean if necessary  	
Clean strainer before relief valve on vacuum furnace
feed pump  	
Plate-up bottom of flash tower
Open all Fractionator manways, top to bottom, and
clean as each are opened using dirty wiping cloths .

Clean Fractionator shell, light reflux piping inside
of Fractionator, light cut trays and light cut draw
off pan and entry to A" draw off line into soaker
if necessary 	

Inspect top 6' diameter tray, clean as needed as
all valve discs must be clear and free moving  . . .

Inspect top 6' tray liquid downcomer, clean out the
bottom of liquid downcomer and liquid entry onto
next tray  	

                              74

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                                                                  Who
Cleanup Instructions (continued)                     Done  When Initial

Inspect under side of bottom 6' tray, clean vapor
uptakes under bubble caps as inspection indicates.
Also go down through top 6' tray and clean bubble
caps as inspection requires 	
Clean cyclone deck, clear cyclone deck drain pipe
as necessary  	

Remove 6 cyclone caps, clean cyclones inside as
required  	

Clean 6 cyclone drain pipes, remove as necessary
to clean below drain pipes  	
 Ranove coke from outside of 6 cyclones and Frac-
tionator shell as needed  	
Clean out tower shell below drain pipes
Clear 3" drain pipe from cyclone section of Frac-
tionator down into bottoms stripping section  . .

Remove dirt around strainer at bottom of
Fractionator  	

Remove suction strainer at bottom of Fractionator
and clean below strainer  	
Remove cyclones section 3" drainpipe, and
clean as necessary   	
Inspect inlet of 4" section to bottoms pump.  Note
condition of 4" suction line.  Put plug in 4" inlet
end of 4" bottoms pump suction after cleaning, to
avoid dropping dirt inside  . 	

Clean inside of bottom shell of Fractionator  .  .  .

Clean stripping steam distributors   	

Clean top of cyclone  	
Inspect cyclone entry wear plate, report condition
of same and repair as needed   	
Clean bottoms level instrument connections   .  .

Rod through bottoms stripping vacuum connection
to manometer  	
Rod  through bottoms level glass connections,
including loop inside the vessel   	
                              75

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                                                                  Who
Cleanup Instructions (continued)                     Done  When Initial.

Position stripping steam distributors in bottom
of Fractionator  	
Replace 3" drain pipe from cyclone section of
Fractionator  	
Remove 2" pipe plug in 4" bottoms pump suction
line, and inspect.  If inspection of 4" inlet into
4" suction line and appearance at 2" pipe plug, and
operation of bottoms pump all indicate need for
cleaning 4" suction line, unflange line, remove
center section and clean the whole line from the
pump suction flange to the bottom of the Frac-
tionator.  Replace 2" plug and flanged section
of pipe  	

When light cut soaker, light cut stripper, and
heavy cut stripper are cooled down, pumped out,
and drained as low as possible, remove the follow-
ing:
      a)  8" cover plate at bottom of light cut
          soaker
      b)  8" cover plate at bottom of light cut
          stripper
      c)  8" cover plate at top of light cut
          stripper
      d)  3" pipe cap on oil inlet line.  Light
          cut stripper
      e)  3" reducer at bottom of 3" drain pipe
          on seal loop on 4" oil line into top of
          heavy cut stripper

Remove tar and clean out bottom of light cut
soaker   	

Remove tar and clean out bottom of light cut
stripper  	

Inspect, also clean top of light cut stripper as
needed   	

Inspect 3" oil inlet line to top of light cut
stripper and clean as needed  	
Blow with air hose through above item and check for
volume of air coming out at 8" cover plates opening
at bottom of light cut soaker.  If low, repeat the
cleaning out process  	

                            76

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                                                                  Who
Cleanup  Instructions  (continued)                     Done  When Initial

Also, blow with air hose through 3" pressure equali-
zer line, back into light cut soaker and check for
volume of air coming  out at 8" cover plate opening
at bottom of light cut soaker.  Clean 3" equalizer
line as  necessary  	

Blow with air hose through 6" vapor outlet line at
the top  of the light  cut stripper and check volume
of air coming out of  top manway of Fractionator  .  .

Rod through level instrument and level glass con-
nections on light cut stripper 	
Rod through level glass connections on light cut
soaker  	

Open 2-3" suction pipe plugs, also 4" cover on pot
in 3" suction line to light reflux pump.  Clean out
suction pipe as required . . 	
Air blow the heavy cut pump 4" suction line back
from pump discharge into heavy cut stripper.  Check
flow at 4" vapor outlet line in Fractionator at
manway at the top 6' tray, cleaning as necessary . ,

Air blow into 4" heavy cut stripper vapor outlet
line, inside Fractionator, at top 6? Fractionator
tray, and observe volume of air coming out of
the bottom 6' bubble tray vapor uptakes under the
bubble caps.  Clean as needed  	
Remove 3" reducing coupling at end of 3" drain
nipple on 4" heavy cut seal loop, in the 4" heavy
cut draw line and clean out the 3" drain nipple
as necessary	

Air blow into the 4" heavy cut stripper vapor outlet
line and out of the 3" drain nipple on the bottom of
the seal loop.   Observe volume of air, clean again
if necessary 	

Rod through Light cut stripper level glass and
level control instrument connections 	
Rod through heavy cut stripper (2) level glasses
connections and the level control instrument
connections  .  	
                            77

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                                                                  Who
Cleanup Instructions  (continued)                     Done  When Initial

As is necessary, fill level glasses with "Red
Devil" paint remover, and clean out level glasses
on the flash tower, Fractionator drain oil section,
Fractionator bottom section, light cut soaker,
light cut stripper and the two heavy cut strippers .

Steam blow, following coolers with 2" steam blow
lines, the heavy cut to the 2" outlet at the line
to the rundown tank, the heavy reflux to the 2" out-
let at the base of the Fractionator, the light cut
to the 2" outlet at the line to the rundown tank,
and the light reflux to the 2" outlet at the base
of the Fractionator   	
After steam blowing the cooling coils, blow out
the cooling coils with an air hose through the heavy
cut to the outlet at the line to the rundown tank,
the heavy reflux to the outlet at the base of the
Fractionator, the light cut to the outlet at the
line to the rundown tank, and the light reflux to
the outlet at the base of the Fractionator 	

When time allows, do the following to thoroughly
clean out the cooling coils and maintain the re-
quired cooling effectiveness:

  a)  Freezing weather:  First steam blow the
      cooling coils with 2" steam blow lines wide
      open to clear the cooling coils.  Then leave
      the 2" valve on the steam blowing lines
      cracked open, to avoid freezing the cooling
      coil, and permit water to dissolve tarry
      material.

  b)  Above freezing weather:  Repeat procedure as
      in a) above, but shut off steam completely
      and let cooling coil sit full of water.

In both cases, a) and b), before startup, blow out
coolers with 2" steam blow valve wide open, and
finish up by air blowing all coolers to remove
water and dirt as completely as possible 	
The above instructions apply to the following coolers:  Heavy
cut, heavy reflux, and light cut and light reflux.

The above blowing procedure is based upon blowing experience and
the following observations:  The material which forms and pre-
cipitates out of the distilled oil liquid and vapor, in flow lines,
cooling coils, bubble trays, vessels, etc., is a material of a
density of approximately 1.2 to 1.3 specific gravity at 60F.


                            78

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Cleanup Instructions  (continued)

It is dark brown or black in color, and settles out quite slowly
in the rundown tanks, but more quickly in hot oil.  It forms
mainly in the liquid or semi-liquid state at the usual atmospheric
temperatures, but also is found as a solid, occurring in solid
particles bound together by a viscous, extremely sticky, tarry
binder.  Both the solid particles and the tar binder phases
apparently enter the liquid phase and are fluid at 338F, the
saturation temperature of 100 psig.  The tar is brittle at low
temperatures, showing a glossy surface upon fracture.

The tar or conglomerate of tar and solid material are both some-
what soluble in hot or cold water and the tar and solid particles
slowly crumble into fine particles, readily entrained in a flow-
ing stream of water.  Both materials are soluble in other polar
solvents, but relatively insoluble in various hydrocarbons.  The
tar or tar and conglomerated solids both form a brownish solution
in water.  The odor of the solution and dissolving material tends
to change on standing, from a burnt, pungent acrid odor to a
much more flat, earthy smell.

Cooling coils and piping tend to plug, but upon prolonged exposure
to 100 psig steam, have gradually opened up.  Once even a small
flow is established, it tends to increase fairly rapidly.
                                                                   Who
                                                     Done  When  Initial

With the air hose, back-blow the discharge of light
cut pump into the light cut soaker; check air vol-
ume coming out of the 8" bottom opening.  Clean the
light reflux pump suction if needed 	
With the air hose, back-blow from the discharge of
light reflux pump into the light stripper; check air
volume coming out of the 8" bottom opening.  Clean
the light reflux pump suction if needed 	 ,
Air blow gland oil lines to the light reflux, light
cut and heavy cut pumps, cleaning as necessary  .  .

Clear cooling water lines to stuffing boxes of
bottoms pump and heavy cut pump as needed 	
Brush and blow dust off the flash furnace coil
inside the firebox  	
Brush and blow dust off the Fractionator Furnace
tubes and header surfaces inside the five boxes.
Brush and blow scale and dirt from all cooling coils
in the cooling coil box; including, bottoms, heavy
cut, heavy reflux, light cut and light reflux .  .  .  .
                            79

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                                                                   Who
Cleanup Instructions  (continued)                     Done  When  Initial

Remove the 4" cap on  instrument air dryer, check salt
level in the dryer and refill as necessary. Brush
thread compound into  4" pipe cap threads and
replace 	

Plate-up manways and  8" openings; including, bottom
of Fractionator, drain oil section of Fractionator,
bottom of light cut soaker, and bottom of light cut
stripper  	
Go over lines, pumps, etc., and close them, ready
for pumping bottoms, light cut, light reflux, heavy
cut and heavy reflux  	
From the heavy cut make tank, fill to normal opera-
ting level, the heavy cut stripper, light cut soaker
and light cut stripper  	
Circulate light cut from soaker over the top of the
Fractionator.  Check flow over the light cut trays.
Check the reflux control valve.  Clean and repair
as needed to get satisfactory flow and make the
lines and cooler tight and the control valve opera-
tive  	

Circulate heavy reflux from the heavy stripper over
the 6' trays in the Fractionator.  Check the flow
over the 6' trays and the bottom tray for leakage,
as well as make a check of the reflux control valve.
Repair as needed to get satisfactory flow, bottom
6' tray tight, control valve operating, and lines
and cooler tight, and with no leaks 	
Warning;  The bottoms cooler is a special case.  Care must be taken
to avoid getting any water into the bottoms in the three bottoms
tanks.  Water does not settle readily out of the bottoms because
of the low API gravity and high viscosity.  Customers complain of
poor burner operation when even a very small amount of water gets
into the bottoms tanks and product.  It does not settle well.

The bottoms cooler does not foul quickly.  It seldom needs to be
blown with steam and air and does not require soaking with water
to dissolve tarry material.

Avoid steam blowing the bottoms cooler during cold weather until
shortly before startup.  This prevents freezing-up and wasteage
of steam.  Careful!  Never, under any circumstances, let any water
get into any of the 3 bottoms tanks.
                            80

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                                                                    Who
 Cleanup Instructions (continued)                     Done  When  Initial

 Bottoms, Cooler, Steam, Air Blowing

 Blow bottoms cooler with steam valve wide open
 and cooler discharging to slopping tank line, until
 cooler is empty and oil and solid matter stop com-
 ing out	
 Blow with air wide open,  until all water stops
 coming out  	

 During startup or before, as required  by other cir-
 cumstances,  establish feed flow through the plant
 into the bottom of the Fractionator, through the
 bottoms pump,  cooler, and back to  the  feed  tank.
 Hold feed at a maximum flow with bottoms pump keeping
 up,  for 10 minutes to thoroughly flush water out  of
 the  system.   The bottoms  cooler is now ready for
 startup 	

 During startup,  turn  bottoms into  bottoms tank when
 API  gravity  is down and cooler outlet  temperatures
 are  both within the range specified in the  log book .

 Pump light cut from the light  cut  stripper,  through
 the  control  valve,  into the  slopping tank.   Clean
 as needed to get satisfactory  flow, lines tight and
 control  valve  operating 	
Pump heavy cut from the heavy cut stripper, through
the control valve, and into the slopping tank.  Clean
as necessary to get satisfactory flow, lines tight,
and control valve operating 	

Start at top of Fractionator and plate-up three
upper manways 	

Plate-up the top of the light cut stripper and re-
place the 3" pipe cap on the oil inlet line 	

Install a 3" blank in the suction to the Fractionator
steam jet vacuum pumps  	

Check over the whole unit and close up anything found
open which should be closed 	
                            81

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F.  Emergency Procedures

Drastic and Immediate action which must be taken when there is
little or no time for investigation or troubleshooting follows:
                                                                   Who
Electric Power Failure                               Done  When  Initial

Open wide all furnace stack and burner dampers . . .

Shut off power to both furnace burners 	

Shut off both stripping steam valves at the main . .

Open furnace doors into fire boxes, and push in
the brick to let cold air inside 	
Shut off steam flow to vacuum pumps  	

Swing Fractionator bottoms product into feed tank

Pump Fractionator bottoms level low, with steam
left in the boilers	 .  .
Pump Fractionator bottoms slowly.  There is no flow
of cooling water 	
Blow down vacuum furnace tubes into Fractionator
with steam left in the boilers 	
Shut off the valves from the feed and the light
and heavy cut tanks	,
Go over electrical systems; including, circuit
breakers, fuses, etc., and check for trouble.  Shut
off all starters until ready to start up again . . .

Start up plant when ready, following the usual
procedures 	

Cooling Water Failure

Stop both furnace burners  	

Open wide all furnace stack and burner dampers , . .

Shut off both stripping steam valves at steam main .

Open furnace doors into fireboxes and push in brick
to let cold air inside 	
Shut off steam to vacuum pumps


                            82

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                                                                    Who
 Cooling Water Failure  (continued)                    pone  When  Initial
 Pump out bottom of Fractionator into feed tank . . .
 Reduce feed to flash furnace 	
 Keep feed going through furnaces until the vacuum
 furnace outlet temperature is 4509F  	
 Shut down cold feed and vacuum furnace feed pumps
 When cooling water supply is normal, start up
 following the usual procedure  .... 	
 Steam Failure
 Stop both furnace burners  	
 Open wide all furnace stack and burner dampers ....
 Shut steam to vacuum jet pumps 	
 Shut both stripping steam valves at steam main ....
 Open both furnace doors into fireboxes and push
 brick in to allow cooling  	
 Shut  down cold  feed  and  vacuum furnace feed  pumps
 Shut  down heavy and  light  cut  pumps  and light  reflux
 pump	
Leave vacuum pumps  running  ,
Leave cooling water running
When vacuum furnace  transfer line is down  to 450F,
shut down cold feed  and vacuum furnace feed pumps   .  .
Bad Fire in Furnace
Stop cold feed and vacuum furnace feed pumps 	
Stop both furnace burners  	
Shut off PROPANE to  furnace burners  	
Shut air dampers at  furnace burners when not too hot  .
Spray water into firebox with fog nozzle 	
Pump out bottom of Fractionator to feed tank 	
Pump light and heavy cut strippers and light cut
soaker to product tanks or slop,  according to gravity.
                            83

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                                                                   Who
General Fire; Outside of Furnaces                    Done  When  Initial

If possible, shut off material which is burning,
i.e., oil, vapor or gas 	
If that cannot be done safely, or the source cannot
be identified, go back to tank valves and shut off
all valves at all tanks, i.e., PROPANE supply, fuel
oil to burners, naptha, Fractionator overhead,
light cut, heavy cut and bottoms  	

Shut down burners on both furnaces as well as the
boilers, if practical 	
Open all furnace stack and burner dampers, if the
burners are stopped and it is possible to do so
with safety 	

Do not use water on areas traversed by electrical
power lines 	

Shut off main electric power switch as necessary

Shut down all pumps at individual starters, or at
main electric power switch as necessary 	
City water may be used as required for fire
fighting  	
The salt water pump is electric motor driven  .  .  .

When the fire is out or under control, do not
attempt to start up again until careful inspection
proves the repair or cause of the fire is com-
pletely adjusted, and there is no hazard in start-
ing up again  	

The foregoing instructions are action directed for maintanance of
safety.  They are, "Do it now, and we will talk about it later,"
directives.  The objectives are given below in approximate order
of importance:

     1)  Avoid injury to others and yourself.

     2)  Save the plant, or parts of the plant that  can be saved.

     3)  Do not waste time on details.  First get  things under
         control and talk about it later, etc.

                            84

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  Small Fire in a  Furnace

  In case of smoking  at  one  or  several  of  the  stacks, and  the
  furnace outlet temperature goes up while burner flames go down,
  inspect the inside  of  the  furnace carefully  for leakage  in a
  tube  or header.   If the flame  leak is small  and stays small,
  reduce  feed flow through the furnace and shut down gradually
  as  in a regular  shutdown.   Proceed according to what happens.
  Do  not  try to  start  up  again if the fire goes out while  shut-
  ting down.   Shut  down completely and examine the evidence.
  Make necessary repairs,  evaluate the situation and then  think
  about starting up again.

  G.  General Fire and Safety Instructions

 Three things are necessary for a fire:  fuel, air and ignition
 temperature.  When a fire is going,  shut off the fuel if  at all
 possible, close all valves that might possibly be passing flam-
 mable material to the flame.  Next,  shut off the air supply to
 the flame by using dry powder and/or  foam.   Extinguishers should
 also direct cooling fluid into the flame area and cool  the fuel
 supply to the flame.  Water-borne  foam,  and water fog are partic-
 ularly effective  in reducing the temperature within  the fuel
 vaporizing and flame space.  If the  temperatures  can be dropped
 low enough, the fuel stops  vaporizing,  the  flame  temperature
 drops  and the combustion reaction  stops    hence,  the fire goes out.

 Use red  or blue dry  powder  extinguishers  on oil, gas and  electrical
 fires.   The blue  dry powder extinguishers are also effective on
 fires  fueled by wood, paper,  textiles  and the usual  solid combus-
 tibles.   Do not use  foam or water on electrical fires until elec-
 tricity  is shut off.

 In  case  of a general  fire,  before the fire  department or  anyone else
 applies  water,  be sure  to shut  off all electric power in  the plant
 by  opening the  main  switch.

 Use  foam and water on fires  inside of tanks, oil-water separators
 or any place else where  the oil is confined and will not  overflow
 and  spread.  Water spray  nozzles are effective on crankcase oil,
 heavy and  light cuts, barometric oil and bottoms.   It is not
 effective  on gasoline or  naptha fires.

 In general, apply the stream from an extinguisher at the base of a
 fire.  Approach a  fire from upwind  and upslope if possible, but
avoid going above  fires where a release of gas liquid or a puff
of air may cause an upsurge of flame that might  surround you.
                            85

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In case of a large general fire around the Fractionator and strip-
pers, with a situation where the fuel feeding the fire cannot be
shut off, call the fire department.  Shut off the main electric
power switch and request the fire department to blanket the Frac-
tionator and stripper area with a fine water fog to keep the
structure cooled down.
                            86

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                      SECTION XIII

                    ACKNOWLEDGMENTS

We are grateful for the dedicated cooperation and assistance
given by Mr. Richard Keppler, the Project Officer, and other
representatives of the Water Quality Office of the Environ-
mental Protection Agency.

We also acknowledge the untiring and consistent efforts of
the National Oil Recovery Corporation's personnel, the vendors
and oil collectors, and our consultants who contributed above
and beyond the normal requirements of their respective activi-
ties, without which, this project could not have been completed,
                         87

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            Number
                             Subject Fie/d& Group
                                05D
                                 SELECTED WATER RESOURCES ABSTRACTS
                                        INPUT TRANSACTION  FORM
     organization  Natlonai oil Recovery Corporation  (NORCO)
               Hook  Road and Commerce Street
               Bayonne, New Jersey  07002
     Title
               CONVERSION OF CRANKCASE WASTE OIL  INTO USEFUL PRODUCTS
 10
     Authorfs)
            Solfred Maizus
            Kenneth Urquhart
                      16
                                     21
                          Project Designation
                           EPA. WQR;   Project No. 15080 DBO
                                         Note
 22
     Citation
 23
     Descriptors (Starred First)
               *0il, *0il Wastes
 25
     Identifiers (Starred First)
               *Crankcase  Oil,  *Reprocessing, *Vacuum Distillation
 27
     Abstract
Abstractor
The project  goal was to demonstrate a  simplified technique for
reprocessing spent automotive crankcase  oils  into useful petroleum
products  other than lube oils, without producing residues which
cause water  pollution.

To achieve the foregoing objectives, National Oil Recovery Corpora-
tion modified its entire plant system with  special equipment and
conducted laboratory and plant runs.

The objectives were substantially attained  in that all the products
from the  vacuum distillation were sold as low sulfur heating fuels
and as potential diesel fuel.  Only the  water in the fuel is not
recovered.

Some technical work was done to upgrade  the refinery products to
obtain a  higher product realization.

This report  was submitted in fullfillment of  Project Number 15080
DBO, under the (partial) sponsorship of  the Water Quality Office,
Environmental Protection Agency.
                               Institution
           Solfred Maizus
                        National D-f 1 Reenvpry
 WR:I02 (REV JULY 1969)
 WRSI C
                                SENCTTO:  WATER RESOURCES SC I EN Tl F 1C INFORMATION CENTER
                                        U.S. DEPARTMENT OF THE INTERIOR
                                        WASHINGTON. D. C. 20240
                                                                                * 5PO: 1999-399-339

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