United States
 Environmental Protection
 Agency
Industrial Environmental Researc'
Laboratory
Cincinnati OH 45268
 Research and Development
EPA-600/S2-81-147  Sept. 1981
Project  Summary
 Removal  of  Heavy  Metals and
 Suspended Solids  from
 Battery  Waste waters:
 Application of HYDROPERM™
 Cross-Flow Microfiltration

 Norman I. Shapiro, Han-Lien Liu, John Baranski, and David Kurzweg
  Laboratory  and  full-scale  field
demonstrations were  conducted to
demonstrate the applicability of the
HYDROPERM™ cross-flow microfil-
tration system for the removal of
suspended solids, and for the removal
of suspended toxic heavy metals from
lead-acid battery production waste-
waters.

  The  results  of the  program  con-
ducted at Hydronautics, Inc., Laural,
Maryland and General Battery Corpor-
ation,  Hamburg, Pennsylvania show
that the system achieves virtually
complete removal of suspended solids
(the filtrate water has a suspended
solids concentration of < 5 ppm) regard-
less of the feed concentration. Lead is
typically reduced to 0.1  ppm.
  The waste from the  battery manu-
facturing facility is   a mixture of
sulfuric acid from occasional dumping
of open-tank formation of the anode
and cathode  battery plates, rinse
water from the plate washing facilities,
and various floor drains from through-
out the plant.  The combined total of
daily waste production is ~ 75,000 liters
per day (20,000 gallons per day). The
waste acid and rinse water mixture is
neutralized with high calcium lime to
convert the soluble metals to a sus-
pended metal hydroxide form.
  The microf iltration system is a treat-
ment  process  which  employs  a
physical principle of treatment for
suspended solids (SS) removal after
chemical precipitation. The principal
element of. the system is  a thermo-
plastic tubular filter (6 mm ID) con-
structed with a controlled porosity in
the micron-size range. Relatively low
feed pressures (1.05 kg/cm2, — 15 psi)
is employed, which is of significance to
energy conservation.
  The first phase of the study was to
determine  the proper porosity, con-
struction material and diameter of the
tubes.  In  addition, studies were
conducted to optimize operating con-
ditions (pressure and velocity). The
second phase of the study involved the
design, fabrication, installation and
demonstration of a full-scale system.
  Both from a flux and a filtrate quality
standpoint, the test and demonstration
programs indicated that microfiltra-
tion is effective for treating  battery
manufacturing wastewaters for dis-
charge. Reuse of the permeate  is
recommended for study.
  Microfiltration technology wiH have
wide application  in the removal  of
heavy metals from such industries  as
battery manufacture, metal finishing.
metal refining, and other  industries
producing similar wastes.

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  This Project Summary was develop-
ed by EPA 's Industrial Environmental
Research Laboratory, Cincinnati, OH,
to  announce  key  findings  of the
research project that is  fully docu-
mented in a separate  report of the
same title (see Project Report ordering
information at back).


Introduction
  Two types of filtration processes have
been  widely used for removal  of sus-
pended solids: (1) the through-flow (e.g.,
multimedia) filter;  and  (2) cross-flow
filtration (e.g., ultrafiltration and reverse
osmosis).  Although they can  remove
some of the suspended solids, conven-
tional through-flow filters have the dis-
advantage of  requiring frequent  back-
washing,  since  the  filtered particles
continuously accumulate on, oractually
enter, the  filtration  barrier. Through-
flow filtration is, by  its  very nature, a
batch process, with the flux declining'
relatively  rapidly  when  the  driving
pressure differential  across the  filtra-
tion barrier is held constant.
  On the other hand, in cross-flow fil-
tration,  Figure  1, the direction of the
Feed flow is parallel to thefilter surface,
so that accumulation of  the  filtered
solids on the  filter medium  can be
minimized by the shearing action of the
flow. Thus, cross-flow filtration affords
the possibility of a quasi-steady state
operation with  a nearly-constant flux
when driving  pressure  differential  is
held constant.

               Filtrate
                          Tube Wall
      ttftttttmttttttmttmt'fa
       ummmuuuuiuuuu
               Filtrate

Figure 1.     Cross-flow filtration sche-
             matic.

  Cross-flow filtration is intended pri-
marily for  the  removal of suspended
solids and is significantly different from
membrance ultrafiltration (UF) or hyper-
filtration   (RO)  which  removes
substances on  the molecular  level  in
addition to  suspended solids.
  HYDROPERM™  is  a  thick-walled,
porous plastic tube. Thesetubes, whose
wall thickness,  inside diameter, poros-
ity,  and pore-size distribution can all be
closely controlled, can be selected for a
particular wastewater so  as to obtain
optimum performance.  The filtration
characteristics of the tubes combine
both the "in-depth" filtration aspects of
multimedia filters and the "surface"
filtration  aspects of membrane filters.
For  example,  while the  removal  of
micron- and  submicron-size particles
is  often  difficult  or impossible  with
conventional  gravity  settling  or
through-flow   filters,  the  cross-flow
microfiltration tubes  are  capable  of
virtually  complete  removal of  such
particles.
  This report gives  a summary of the
results  of  a   two-phase  program  to
demonstrate  the  applicability  of the
microfiltration system for the'removal of
toxic  heavy  metals  from  lead-acid
battery   manufacturing   wastewaters
after the metals have been chemically
precipitated.  This program was  con-
ducted under the sponsorship of the
United States Environmental Protection
Agency's   Industrial   Environmental
Research   Laboratory  in   Cincinnati,
Ohio, under a cooperative agreement to
General Battery Corporation, Reading,
Pennsylvania. The  program  was
initiated in August 1978 and terminated
in  June 1980. The  results reported  in
the  report  include  both the  Phase I
laboratory test program and the Phase II
on-site demonstration  of  a full-scale
microfiltration system at the General
Battery Corporation  plant at Hamburg,
Pennsylvania.
  The two-phase program is outlined as
follows:
  The objectives of the Phase I labora-
tory program were to test, evaluate, and
optimize  HYDROPERM™ tubes for the
effective treatment of battery manufac-
ture  wastewaters.  Since a  unique
feature of the tubes is that they can be
selected for optimum performance with
specific wastewaters by  varying the
tube material and pore structure as well
as the system operating conditions, a
principal objective  of  the proposed
program was  to conduct such optimiza-
tion studies.
  The objectives of the Phase II program
were to design, construct, install, and
demonstrate a full-scale microfiltration
system at the General Battery Corpora-
tion plant in Hamburg, Pennsylvania.
Phase I
  The wastewater used for the Phase I
laboratory program was obtained from
the General Battery Corporation plant at
Hamburg,  Pennsylvania.  The   raw
wastewaters  typically  contained
-1500-1900  mg/l  of  lead.  When
received at the Hydronautics laboratory,
the wastewater had a pH of 1.0. Toxic
heavy  metals were precipitated at a
range of pH's by adding hydrated lime.
The best results in terms of lead precipi-
tation were obtained at a pH of 8.5-9.5.
After  lime addition,  total solids (TS)
values increased to 45,000 mg/l in the
feed, most of which were in the form of
suspended solids (SS) (40,000 mg/l).
  Thirteen single-tube tests of up to 160
hours in duration were performed with
the lime-precipitated waste  described
above. In  all but one of the tests the
filtrate was  remixed  with  the  feed,
which  resulted in a "constant concen-
tration" mode of operation.  One test
was performed  with  increasing sus-
pended solids concentration in the feed,
with periodic removal of the filtrate from
the feed until an 85% reduction in the
total volume  of  the  feed had  been
reached. The purpose of these tests was
to provide information on filtrate flux
and quality as a function of the type of
tube and the operating conditions used.
  The  results  of the  test  program
exceeded  all original  expectations  in
terms  of  flux and  permeate quality.
Forty-hour plateau flux  levels well  in
excess of 8150 Imd  (200 gal/ft2-day)
were  demonstrated  in  the  Phase  I
laboratory  program.  These  represent
integrated 40-hour flux values probably
in the  range of over 12,000 Imd (300
gfd). With  periodic cleaning of the tubes,
fluxes  in the range of 7700-9800 Imd
(190-240  gfd) were  obtained after a
range of 114-164 hours of operation. In
addition, when operating at optimum pH
(—8.5-9.5) the quality of the permeate
was excellent in terms of heavy metals
removal. For example, Pb, was typically
reduced from > 10 ppm in the feed to as
low as < 0.01 ppm in the permeate with
median values in the  range of 0.6-.09
ppm. Similar results were achieved for
other  metals, with typical  permeate
values of: 0.05 for Cu; 0.05 for Ni; < 0.1
for Zn; < 0.002 for As; and — 0.3 for Sb.
Suspended  solids   were   typically
reduced from > 30,000 ppm in the feed
(after lime treatment) to less than 10 in
the permeate.

Phase II
   Figure  2 shows a  schematic of the
system designed for  General Battery,
based on the results of Phase I. After the
microfiltration  system  had   been  in-
stalled and interfaced with the systerr

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Wastewater Feed
                                Recirculating an<$
                               Sludge Settling Tank
                                                        Pressure
                                                         Gauge
                                                      Level Sensor
                                                                                » —
                                                                       H
                                                                                                           Cleaning
                                                                                                             Tank
                                       H
                                                                                         Main
                                                                                      Feed Pump
                                                                                          Pressure Gauge
                                                                                         HYDROPERM™
                                                                                            Modules
                                                                                       Permeate Line
                                                                                              Permeate
                                                                                           Collecting Tank
                                                Permeate
                                                 Holding
                                                  Tank
                                                                     Transfer Pump
 Figure 2.    HYDROPERM™ system schematic diagram.
components  provided  by   General
Battery Corporation, a two-week period
of system  checkout, debugging,  and
operator  training was initiated.  The
system checkout included not only the
operation of the units but also: (1) defini-
tion of the  procedure which  had to be
followed  with  respect to  the plant
wastewater neutralization process and
(2)  preparation  of  the   operational
manual  based on both the laboratory
experience  and upon field operation of
the unit. Thus, the manual was updated
to reflect:  field  operating  conditions;
sampling procedures,  techniques  and
frequencies; and the logistics of trans-
porting  collected   waste  feed  and
permeate samples to and from the inde-
pendent  analytical  laboratory.  Quick
turn-around of laboratory results were
critical in  terms of  the control  of the
operational procedures to optimize the
performance of each individual module.

System  Performance in the
Field

Permeate Flux and Quality
  Initial daily flux values were typically
in the  range of 32,600  Imd (800  gfd)
leveling off to 16,300-20,400 Imd (400-
500 gfd) after several hours of operation.
The flux was readily -restored to the
initial value by cleaning the modules for
several minutes daily with  permeate.
Cleaning  with  dilute HCI  (2%)  was
practiced  generally only on a  weekly
basis.
  At these high flux levels, production
of permeate by only one unit is in the
range  of  13,200 to 18,900  liter/hr
(3500 to 5000 gal/hr) during a filtration
run of several hours duration. Typically,
a load of 94,600 liters (25,000 gallons)
of wastewater is filtered in 4-1/2 to 5

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hours  by only one unit,  producing
75,700 liters (20,000 gallons) of clear
permeate  and  18,900  liters (5000
gallons) of sludge. The solids content of
the sludge was in the range of 20-35%
SS by weight.
  Figure  3 shows  the  frequency  of
occurrence for  lead and  suspended
solids contents analyzed during the field
investigation.   It  indicates that the
majority of the lead concentration in the
permeate is below 0.5 ppm.  For properly
controlled pH adjustment  in  the neutral-
ization process, lead concentration can
be easily  reduced to less  than 0.2 ppm.
This is because most of the toxic metals
are amphoteric. They can subsequently
precipitate out in  the  permeate if pH
varies  which can  also  contribute  to
higher suspended  solids  concentration
in the permeate. The suspended  solid
concentration plot  shows  that more
than two-thirds of permeate  samples
analyzed have a concentration less than
3 ppm.

Sludge  Generation
  Waste sludge production is  typically
about 17,000 liters (4500  gallons) for
every two days of operation,  with SS
concentrations of 20-35%  by weight.
The wastewater generated  at the plant
during a typical two-day period is about
94,600 liters (25,000 gallons). From
these wastes, approximately 75,700
liters (20,000 gallons) of clear permeate
were produced. One tank truck load of
sludge is transported to the  land-fill site
in  Reading  every  other day  greatly
reduced from the trips which the tank
truck had to make in the past (previously,
two to three trips were required daily).
The  clean  permeate  is  discharged
directly to a local stream. The reuse of
this  high  quality  permeate water for
plant use is now under evaluation.

Conclusions and
Recommendations
au
1 7°~
1 60-
 10
pH< 8

pH 8 -10







m
wOua
M B r-n il •
      0<0.04    0.04-  0.07-  0.1-   0.2-   0.3    0.4     0.5-   >1.0
                 0.069  0.099   0.199  0.299  -0.399 -0.499 1.0
                              Lead Concentration, ppm
S 70-
N
SL
2 60-
c
1 5°"
"I 40-

•Q
S 70-
1







































i —
n „ n
 Figure 3.
    1-3   3-10  10-15  15-20

      Suspended Solids, ppm


Pb and SS concentration in HYDROPERM™ permeate from lead-act
battery wastewater.
in  the feed in the range of several
hundred ppm was typically reduced to
0.02-0.1  ppm  in the permeate.  Other
toxic heavy metals, such as Cu, Ni, Zn,
As,  and  Sb   were  removed   with
comparable effectiveness. Although the
filtrate is discharged directly to a local
stream, the quality of the filtrate in
terms of  SS and toxic heavy metals is
such that reuse is also a viable option.
                          Recommendations
                            Cross-flow   microfiltration   should
                          have broad application for the removal
                          of SS and suspended toxic heavy metals
                          in a wide range of industries, including
                          battery manufacture, metal  finishing,
                          smelting   and  refining,  and  other
                          industries with similar  wastewaters.
                          Economics for the concept remain to be
                          developed.
General
  Cross-flow microfiltration is an effec-
;ive technology for the treatment of SS
in wastewaters from the production of
lead-acid batteries.
Permeate Quality
  Suspended solids in the feed which
exceeded 150,000 ppm were typically
reduced to 3 ppm in the permeate. Lead
Flux
  One HYDROPERM™ unit with 16.7
m*  (180  ft2)  of filter  surface  area
achieved a plateau flux value of 16,000
Imd (400 gfd), lime-treated, lead-acid
battery wastewater.

Sludge
  Sludges in the range of 20-35 percent
SS by weight were regularly produced
by the HYDROPERM™ system.

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   Norman I. Shapiro and Han-Lien Liu are with Hydronautics. Inc., Laurel, MD
     20810; John Baranski and David Kurzweg are with General Battery Corpora-
     tion, Reading, PA 19603.
   Charles Darvin is the EPA Project Officer (see below).
   The complete report, entitled "Removal of Heavy Metals and Suspended Solids
     from Battery Wastewaters: Application of HYDROPETiM™ Cross-Flow Micro-
     filtration," (Order No. PB 81-234 833; Cost $9.50. subject to change) will be
     available only from:
           National Technical Information Service
           5285 Port Royal Road
           Springfield, VA 22161
           Telephone: 703-487-4650
   The EPA Project Officer can be contacted at:
           Industrial Environmental Research Laboratory
           U.S.  Environmental Protection Agency
           Cincinnati, OH 45268
•h US GOVERNMENT PRINTING OFFICE, 1981 —757-012/7320

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