United States
Environmental Protection
Agency
Industrial Environmental Research
Laboratory
Research Triangle Park NC 27711
EPA 600 2 80 055
March 1980
Research and Development
Closed-cycle Textile
Dyeing: Full-scale
Hyperfiltration
Demonstration (Design)
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RESEARCH REPORTING SERIES
Research reports of the Office of Research and Development, U.S. Environmental
Protection Agency, have been grouped into nine series. These nine broad cate-
gories were established to facilitate further development and application of en-
vironmental technology. Elimination of traditional grouping was consciously
planned to foster technology transfer and a maximum interface in related fields.
The nine series are:
1. Environmental Health Effects Research
2. Environmental Protection Technology
3. Ecological Research
4. Environmental Monitoring
5. Socioeconomic Environmental Studies
6. Scientific and Technical Assessment Reports (STAR)
7. Interagency Energy-Environment Research and Development
8. "Special" Reports
9. Miscellaneous Reports
This report has been assigned to the ENVIRONMENTAL PROTECTION TECH-
NOLOGY series. This series describes research performed to develop and dem-
onstrate instrumentation, equipment, and methodology to repair or prevent en-
vironmental degradation from point and non-point sources of pollution. This work
provides the new or improved technology required for the control and treatment
of pollution sources to meet environmental quality standards.
EPA REVIEW NOTICE
This report has been reviewed by the U.S. Environmental Protection Agency, and
approved for publication. Approval does not signify that the contents necessarily
reflect the views and policy of the Agency, nor does mention of trade names or
commercial products constitute endorsement or recommendation for use.
This document is available to the public through the National Technical Informa-
tion Service, Springfield, Virginia 22161.
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EPA-600/2-80-055
March 1980
Closed-cycle Textile Dyeing
Full-scale Hyperfiltration
Demonstration (Design)
by
Craig A. Brandon (Carre, Inc.)
LaFrance Industries
LaFrance, South Carolina 29656
Grant No. S805182
Program Element No. 1BB610
EPA Project Officer: Max Samfield
Industrial Environmental Research Laboratory
Office of Environmental Engineering and Technology
Research Triangle Park, NC 27711
Prepared for
U.S. ENVIRONMENTAL PROTECTION AGENCY
Office of Research and Development
Washington, DC 20460
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ABSTRACT
The report describes the first (design) phase of a full-scale demonstra-
tion of hyperfiltration for closed-cycle operations of a LaFrance Industries
dye house. (The remaining three phases are installation, operation, and
maintenance.) The decision to demonstrate the process was based on earlier
projects that showed hyperfiltration to be potentially economical for recycle/
reuse of energy, water, and chemicals in textile preparation dyeing, and wet
finishing. On-site pilot tests of three hyperfiltration modules led to the
selection of the Mott-Brandon ZOPA module. Representative wash waters from
LaFrance dyeing operations were characterized as a basis for demonstration
equipment design. The dye range is to be converted to counterflow with a water
flow rate of 50 gpm at 82 C, with 96% of the wash water recovered as permeate
for direct recycle. Reuse and/or disposal of the concentrate and dye pad
residuals will require further study. Payback period, without credit for
chemicals recovery, is estimated to be 5.2 years.
ii
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SUMMARY
Hyperfiltration is a pressure driven membrane separation process that
has been shown to be potentially economical for recycle of energy, water,
and chemicals within textile preparation, dyeing and wet finishing operations.
This demonstration project follows three prior research and development pro-
jects which (1) showed reusability of membrane permeate (purified water) and
the residual concentrate from hyperfiltration of a dye house wastewater,
(2) general reusability of permeates for wastewater from eight selected
textile plants, and (3) the potential for conservation of about 50 percent
of energy used in wet processing by direct recycle of permeate at full
process temperature. The three projects led to the recommendation for this
full scale demonstration of hyperfiltration for closed cycle operation of a
representative textile unit process - a dye range.
La France Industries was the site of the first project mentioned above
and has been involved in all the subsequent projects. This dye house
incorporates both batch dyeing (dye becks) and continuous dyeing (a dye
range). The La France site is centrally located for the textile industry in
the Southeast. The textile industry is heavily concentrated in the Southeast.
The demonstration project consists of four phases:
Phase I - Design Phase
Phase II - Equipment Installation Phase
Phase III - Demonstration Operation Phase
Phase IV - Evaluation and Reporting Phase
This report presents the results of Phase I. The textile process, a dye
range, is described and the wash water is characterized (chemically) for each
of several fabrics/dye classes processed. The data from on-site pilot tests
are presented for three types of hyperfiltration modules. The design of the
recovery system is described. The economics of the recovery system are
estimated based on the quoted price for installation and projected operating
costs and savings for the dynamic membrane system selected for the demonstra-
tion.
The dye range will be converted to counterflow with an expected water
flow rate of 190 £/min (50 gallons per minute). The principal fabrics dyed
are cotton, acrylic, nylon, rayon and polyester. The dye classes used are:
direct, dispersed, acid, premetalized, basic and fiber reactive. The dyes
and auxiliary chemicals will result in a wash water composition of: COD
(mg/£) = 1200, color (ADMI) = 1750, pH of 5 to 10.5, total solids (mg/£) =
1400, suspended solids (mg/£) = 45, and hardness (mg/Jl) = 30. The wash
water temperature is expected to be 82 C.
iii
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The three high temperature hyperfiltration membrane module types that
were pilot tested included two that utilized dynamically formed zirconium
oxidepolyacrylate membranes; one with these membranes deposited on the out-
side of carbon tubes and one with the membranes deposited on the internal
surface of sintered stainless steel tubes. The third module was a spiral-
wound poly(ether)amid membrane. All these modules provided a permeate
satisfactory for recycle. The degree of pretreatment, i.e., prefiltration
and temperature control can be designed based on the pilot test results.
The recovery system is designed with 23m3 (6000 gallon) tanks for the
wash water and permeate so that the membrane unit can operate continuously
while the dye range undergoes periodic shutdowns between production lots.
All effluent from the range, except steam condensate, is collected into the
recovery system. Ninety-six percent of the wash water is recovered as
permeate for direct recycle as wash water. The unused dye pad liquor goes
directly to the concentrate tank and is not processed by the membranes. The
control and monitoring instrumentation provide for automatic operation and
complete documentation of water and energy savings achieved by recycle. The
reuse and/or disposal of concentrate and dye pad residuals will be studied
throughout the later phases of this project.
The economics of recovery are based on the installed cost (quoted prices)
of approximately $400,000 and the operating costs estimated for the Single
Pass membrane system utilizing dynamic membranes on sintered stainless steel
tubing. The payback period, calculated by the Riegel Textile Corporation's
standard procedure, is 3.8 years with chemical recovery and 5.2 years without
chemical recovery. The annual energy savings are about 2 x 1010 Btu per year.
The operating costs are estimated based on February 1979 prices for energy
and materials.
The equipment selection and decision to proceed with the demonstration
were made on April 6, 1979.
iv
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CONTENTS
Summary -ii
Figures v
Tables , vi
Englishc-Metric Conversion Table vii
Acknowledgment viii
1. Introduction 1
2. Conclusions 9
3. Recommendations 10
4. Textile Process Description 11
Standard Washing Procedure 11
Modified Washing Procedure ... 13
5. Recovery System 19
6. Membrane Performance Tests 23
General Membrane Performance 23
Test Equipment 26
Procedures 30
Membranes Tested 30
Test Results and Discussion 32
7. Recovery Economics 54
References 57
Appendices
A. Dye Range Effluent Chemical Analyses 58
B. Modified Washing Procedure Tests 70
C. Reuse Evaluations 74
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FIGURES
Number Page
1 Molecular Range Versus Flux for Filtration Processes 4
2 Continuous Dye Range Arrangement 12
3 Continuous Dye Range Modified Arrangement 18
4 Conceptual Diagram of the Recovery System 20
5 Estimated Drug Room and Net Make-up Flowrates 22
6 Schematic Diagram of the High Pressure Test Unit . 27
7 Schematic Diagram of the Low Pressure Test Unit 29
8 Product Flow and Conductivity and Color Rejection Versus
Operation Time for U.O.P. Module No. 90 33
9 Product Flow and Conductivity and Color Rejection Versus
Operation Time for U.O.P. Module 380 34
10 Flux Versus Pressure for U.O.P. Module No. 380 35
11 Flux Versus Temperature for U.O.P. Module No. 380 36
12 Flux Versus Circulation Flow for U.O.P. Module No. 380 37
13 Product Flow and Conductivity and Color Rejection Versus
Operation Time for Mott-Brandon Module No. 452 41
14 Flux Versus Pressure for Mott-Brandon Module No. 452 42
15 Flux Versus Temperature for Mott-Brandon Module No. 452 43
16 Flux Versus Flow Velocity for Mott-Brandon Module No. 452 .... 44
17 Product Flow and Conductivity and Color Rejection Versus
Operation Time for Kusters Module No. 480. . . . 48
18 Flux Versus Pressure for Kusters Module No. 480 49
19 Flux Versus Temperature for Kusters Module No. 480 50
vi
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TABLES
Number Page
1 Conservation and Resource Recovery Potential for the
U.S. Textile Industry 2
2 Textile Industry Evaluation of Hyperf iltration 5
3 Phase I Milestones 7
4 Continuous Dye Range Discharge Rates and Temperatures 14
5 Present and Expected Chemical Characteristics of the
Total Dye Range Effluent i5
6 Characteristics of Fix Bath Effluent 16
7 Summary Comparison of Modules Tested. ... 24
8 Characteristics of Hyperfiltration Membranes Tested . 31
9 The Capacity of the Carborundum Filter Elements 39
10 Chemical Analysis of Concentrate and Permeate Samples
for U.O.P. Module No.'s 90 and 380 '. . 40
11 Chemical Analysis of Concentrate and Permeate Samples
for Mott-Brandon Module No. 452 45
12 Chemical Analysis of Concentrate and Permeate Samples
for Kusters Module No. 480
13 Estimated Annual Savings Due to Recycle ............ ^6
14 Estimated Membrane System Operating Costs ........... 56
vii
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ENGLISH METRIC CONVERSION TABLE*
To Convert From
To
Multiply by
Inch
Feet
Square inch
Square feet
Cubic feet
Gallon
Pound
Pound per sq. inch (psi)
Horsepower (Hp)
Gallon per day
Gallon per minute (GPM)
Gallon per sq. ft-day (GFD)
Gallon per minute per sq. ft.
Meter
Meter
Square meter
Square meter
Cubic meter
Cubic meter
Kilogram
Atmosphere
Watt
Cubic meter per day
Cubic meter per day
Cubic meter per sq. meter-day
Cubic meter per sq. meter-day
2.54 x 10-2
3.05 x ID"1
6.45 x 10-1*
9.29 x 10~2
2.83 x 10~2
3.79 x 10~3
4.54 x 10-1
6.80 x lO-2
7.46 x 102
3.79 x 10~3
5.45
4.10 x 10~2
5.87 x 101
*The units most familiar to the projected readership of this report have been
maintained.
viii
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ACKNOWLEDGMENTS
This study was conducted by a team and major contributions were made by
a number of people. The cooperation and assistance of the La France staff .
members is particularly acknowledged; Mike Drummon, Perry Lockridge, Charles
Smith, and many machine operators and laboratory technicians. Dr. Jim Bostic,
Jr., Mr. Ted Meyer and Mr. Ernie Freeman of Riegel Corporate staff provided
valuable advise.
This demonstration is an interagency program and thus benefited from the
guidance of Dr. Max Samfield, U.S. Environmental Protection Agency, as
Principal Project Officer; John Rossmeissel, Department of Energy, and Frank
Coley, Department of the Interior, as Project Officers, and Mr. Robert
Mournigham, U.S. Environmental Protection Agency, as Technical Advisor.
Dr. J. S. Johnson, Jr., of the Oak Ridge National Laboratory has served as
membrane technology consultant on this and all the previous related R and D
projects. A special acknowledgment is given to Dr. K. C. Channabasappa of the
Department of Interior whose knowledge of the membrane technolgy was
instrumental in initiating the project. His untimely death was a major loss
to the entire project team.
CARRE, Inc. provided overall program management and developed the
conceptual design of the recovery system. The contributions of staff members
at CARRE, Inc. are acknowledged. Staff members making major contributions are
Drs. J. L. Gaddis and H. G. Spencer; Donald K. Todd, James Schubert and Kris
Turschmid, engineers, and Roger Hunt and Don King, technicians. Dr. J. J.
Porter and Mr. Grant Goodman of Texidyne, Inc. make significant contributions
in providing chemical analyses and consultation. Dr. E. Harrison served as a
consultant on control and instrumentation.
The detailed design and bid specifications were provided by J. E. Sirrine
Company. The membrane equipment vendors made significant contributions in
technical comments and advice.
Don Hill Craig A. Brandon
Project Director Project Coordinator
ix
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SECTION 1
INTRODUCTION
The technical feasibility of renovating textile wastewaters for recycle
has been shown in a series of government sponsored research grants with the
textile industry that began in 1972. The current project to demonstrate
closed-cycle operation of a production dye range at La France Industries will
determine the practicality of the previous feasibility research. This report
summarizes the results of Phase I of the demonstration program. The wide
application of hot process effluent recycle has a large potential impact on
energy conservation and pollution abatement.
IMPACT OF RECYCLE
High temperature hyperfiltration applied to hot industrial process
effluents will result in significant reduction in the fresh water demand and
waste treatment requirements as well as achieving energy and material
conservation.
The hot process water (vLOO°C) is discharged at a rate of about 2 x 1012
gallons per year* (7.6 x 109 m3/year). In the temperature regime to 100 C
(where high temperature hyperfiltration has already been evaluated) direct
recycle can achieve energy conservation of 2.4 x 1015 Btu/year. For example,
the estimated potential in energy and material resource conservation by
recycle in the U.S. textile industry in 1978 is shown in Table 1 (1). The
energy conservation for the textile industry is vL5 x 106 barrels of oil
(equivalent) per year. Other industries represent much larger potential
energy savings through hot water recycle.
The reduction of the demand for fuel, industrial chemicals and treated
process water has a favorable environmental impact all along the manufacturing
chain from extraction through distribution of finished goods. The direct
environmental impact where closed-cycle operation eliminates contamination
discharges is obvious. The specific potential for reduced pollution is nearly
identical with the list of potential resource savings.
BACKGROUND
Recycle is an obvious and perhaps necessary, method of conserving the
available water supplies, whether from natural sources or from desalination
* The units most familiar to the projected readership of this report have been
maintained. A table of conversions is included in this report.
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TABLE 1. CONSERVATION AND RESOURCE RECOVERY POTENTIAL FOR THE U.S. TEXTILE INDUSTRY (1)
Study Total3
Industry Total
Recycle Potential
Estimated Annual Savings ($102)
Water
Discharge
(103 kgal/d)
31.4
706
635
79
Dyes
(103 Ib/d)
59.80
2191
129
95
Auxiliary
(103 Ib/d)
27.50b
594
489
24
Salt
(103 Ib/d)
26.9
581
481
2.6
Process Thermal
Energy
(103 Btu/d)
37.90d
352e
264
°EPA Grant No. S802973.
Exclusive of 176,000 pounds of NaOH used daily at these plants.
,1972 census of manufacturers, assuming 250 days/year on stream.
Industry estimate of 50 x 10° barrels/year; 70% In wet finishing.
^15 x 106 barrels/year.
Unit costs: water @ $0.5 kgal; dye @ $3/#; auxiliary chemicals @ $0.2/#;
salt @ $44/ton; process steam @ $4/106 Btu.
-------
facilities. The engineering problem associated with the application of mem-
brane technology to industrial effluents is different from the problems
associated with desalination (2). Major differences include:
Feed water characteristics that vary from strongly basic to strongly
acid,
Pretreatment that must not destroy the chemicals for recycle,
High volumetric recovery to achieve direct reuse at process conditions,
Operation at high temperature for direct recycle at process conditions,
and
' Relatively low permeate quality requirements (in some cases) for direct
recycle as industrial process water.
Because some of the separation results achieved with complex industrial
effluents by even "reverse osmosis" membranes is really very fine filtration,
the terms "hyper" filtration and "ultra" filtration are used to more accurately
describe the membrane technology being demonstrated. Figure 1 gives a simpli-
fied view of the range of filtration from conventional to "hyper."
This demonstration program is the culmination of a series of cooperative
research projects conducted by the present participants for the U.S.
Environmental Protection Agency and the textile industry. From 1972 through
1977 (Table 2) many configurations of commercially available ultrafiltration
and hyperfiltration equipment have been evaluated with both total plant
composite wastewater and unit manufacturing process effluents. The research
has involved both field and laboratory tests.
PURPOSE AND SCOPE
The purpose of the demonstration proejct is to design, install, and
operate a full scale commercially available membrane system to evaluate the
practicality of the use of high temperature hyperfiltration in the textile
industry.
Because of the background of research, the textile industry was chosen
for the demonstration. Both a dye range and atmospheric beck, two types of
equipment representative of the two broad categories of dyeing and wet
processes of textiles, were considered. The scope of project includes the
following activities divided among four phases (the phases are identified
in parantheses):
A system design based on on-site test results and including all
engineering details and commercial quotations for installed cost
(Phase II)
Installation and start-up of a full scale hyperfiltration unit (Phase
II)
Evaluation of any long term effects on the manufacturing quality
control and productivity of the dye range and determination of operating
costs (Phase III)
Evaluation of project results for economics of hyperfiltration (Phase
IV)
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HUMAN HAIR
RED BLOOD CELLS
TALCUM POWDER
LIGHT MICROSCOPE
SMALL BACTERIA
INFLUENZA
VIRUS
TOBACCO
UJ
O
I
U
MOSAIC VIRUS «J
STARCH
MOLECULE
EM ALBUMIN
ELECTRON
MICROSCOPE
OLUCOSE
MOLECULE
CHLORIDE ION
HYDRO0EN
MOLECULE
2
T
CONVENTIONAL
PARTICLE
FILTERS
MICROPOROUS //
FILTERS /
ULTRAFILTRATION
MEMBRANES
HYPERFILTRATION
MEMBRANES
10' '
1.0
10
10*
10
FLUX, go|/ft2/doy/Ap»i
Figure 1. Molecular Range vs. Flux for Filtration Processes
100
10
(O
o
DC
U
10 ..
M
Ui
,6'I
5
10
10
10" 10"
CARRE DWG. 65
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TABLE 2. TEXTILE INDUSTRY EVALUATION OF HYPERFILTRATION
DATE: 1972-75 USEPA Grant No. S800929 (3)
OBJECTIVE: Complete reuse of plant wastewater at La France
GRANTEE: La France Industries, Division of Riegel Textile Corporation
PRINCIPAL INVESTIGATOR: C. A. Brandon and J. J. Porter
CONCLUSION: Both purified product and concentrate residue reused in
eighteen production dyeings.
DATE: 1974-77 USEPA Grant No. S802973 (4)
OBJECTIVE: Assess application to composite wastewater at eight plant sites.
GRANTEE: South Carolina Textile Manufacturers Association
PRINCIPAL INVESTIGATOR: C. A. Brandon and J. J. Porter
CONCLUSION: Purified water was recycled in every process; chemical recovery
in some cases.
DATE: 1975-78 USEPA Grant No. R803875 (5)
OBJECTIVE: Assess recycle with high temperature membranes for five selected
wet finishing unit manufacturing processes.
GRANTEE: Clemson University
PRINCIPAL INVESTIGATOR: C. A. Brandon, J. L. Gaddis, and J. J. Porter
CONCLUSION: Cost effectiveness for closed-cycle operation of selected wet
finishing unit processes estimated.
DATE: 1977-81 USEPA Grant No. S805182 (6)
OBJECTIVE: Demonstration of closed-cycle operation of full scale textile
processes.
GRANTEE: La France Industries, Division of Riegel Textile Corporation
PRINCIPAL INVESTIGATOR: C. A. Brandon
DATE: 1978- USEPA Grant No. R805777 (7)
OBJECTIVE: Determine feasibility of hyperfiltration membranes for toxic
emission control.
GRANTEE: Clemson University
PRINCIPAL INVESTIGATOR: J. L. Gaddis and H. G. Spencer
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The scope of Phase I, the design phase, included:
characterization of the textile process,
study of production procedure modification,
design of the recovery system,
on-site qualification testing of membranes, and
estimation of the economics of recovery.
METHOD OF STUDY
This demonstration project is conducted at La France Industries,
Division of Riegel Textile Corporation, with the assistance of five major
subcontractors. The Oak Ridge National Laboratory loaned a hyperfiltration
test trailer and provided consultation on membrane technology by Dr. J. S.
Johnson, Jr. Clemson University conducted some specialty chemical analyses
under the direction of Dr. H. G. Spencer. The other subcontractors and their
contributions are described below.
This demonstration project was conceived of as the logical culmination
of the USEPA research itemized in Table 2. Dr. C. A. Brandon developed, in
cooperation with La France Industries, the grant request proposal and work
plan for this demonstration. He with his associates in CARRE, Inc. provide
the overall program management. They planned, conducted, and evaluated the
pilot testing, developed the conceptual design of the recovery system and
prepared recommendations on program continuation in Phase I.
Texidyne, Inc. performed chemical analyses and provided consultation.
They assisted in the evaluation of process modifications and laboratory tests
of recycle. They also performed the chemical analyses to characterize the
process effluents and membrane performance during Phase I.
J. E. Sirrine Company detailed the recovery system including
preparation of the equipment and installation specifications and the request
for bids for equipment and installation. They also received and reviewed the
quotations.
The manufacturers of the membrane equipment participated in the planning
of the on-site qualification testing and in preparation of formal designs and
commercial quotations of the membrane component of the recovery system,
including estimates of operating and maintenance costs.
The method of study is illustrated in the list of milestones, Table 3.
The duration of Phase I was September 23, 1977 to September 22, 1978.
OVERALL RESULTS - PHASE I
Two major results of the study and design activities during Phase I were:
1) The selection of the dye range, instead of the becks, for the full
scale demonstration.
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TABLE 3. PHASE I MILESTONES
1. Detailed Work Plan Completed
2. Quality Assurance Plan Completed
3. Review of Membrane Process Compatability Data
4. A & E Chosen
5. Process Selected
6. Preliminary Design Drawings & Cost Estimated Completed
7. Submit Project Continuation Application
8. Recovery System Design Completed
9. Equipment & Installation Bids Received
10. Project Continuation Authorized
11 November 1977
30 November 1977
15 February 1978
28 February 1978
31 May 1978
31 May 1978
30 June 1978
31 July 1978
31 August 1978
6 April 1979
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2) The economic estimates indicated a 3.8 year payback, after taxes,
for the installed recovery system.
The dye range was selected because it is the more modern dyeing equipment
technology and is representative of the trend in the industry due to lower
production costs. At La France, the dye range has largely replaced the becks
as the standard production equipment.
The payback period was calculated based on estimated recycle savings, at
current (1979) energy and chemical prices, and the quoted membrane price
installed.
The decision to continue with Phase II, the equipment purchase and instal-
lation was made based on these results.
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SECTION 2
CONCLUSIONS
The conclusions of Phase I, the design phase of this demonstration pro-
ject, relate both to the technical feasibility and to the economic feasibility.
TECHNICAL FEASIBILITY
Technical feasibility of using hyperfiltration for closed cycle operation
of a dye range involves the performance of the membrane equipment and the reuse
(recycle) of the membrane permeate (the purified 95% of wash water volume) and
the concentrated chemicals (in the remaining 5% of the wash water volume).
Three hyperfiltration membranes were evaluated under test conditions
compatible with the membrane manufacturer recommendations and the anticipated
operating conditions at La France. The test results all indicated technical
feasibility for the application to dye wash water. The membrane permeates
were found to be adequate for recycle as process water. The reuse and/or
disposal of the concentrated chemical residue will be studied in subsequent
phases of this program.
ECONOMIC FEASIBILITY
The economic feasibility of hyperfiltration is estimated based on
three factors: the installed cost of the membrane system and the estimated
operating costs and the savings.
The quotations accepted for the membrane recovery system and the instal-
lation of the auxiliary tanks, piping and controls totaled $485,000. It is
estimated that about $85,000 is for extra features useful in a demonstration
but not necessarily required for standard commercial installations. The
estimated operating costs and savings yielded a 3.8 year payback period, after
taxes.
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SECTION 3
RECOMMENDATIONS
It is recommended, based on the above conclusions from Phase I results,
that Phase II be implemented. It is recommended that the Mott-Brandon
Corporation stainless steel membrane system be used in the full-scale
demonstration. This system employs high temperature ZOPA dynamic membranes on
the internal surface of porous sintered stainless steel tubing. Stable fluxes
were achieved at all test conditions with no indication of plugging by
suspended solids in wash water.
The full-scale evaluations scheduled for the latter phases of this
program will determine the practical feasibility of hyperfiltration. The
development of optimal membrane operation procedures, including development
of cleaning and/or flux maintenance procedures may enhance the economics of
applying membranes for recycle.
The development of techniques and procedures for reuse of major portions
of the concentrated chemicals could contribute significantly to the economic
benefit of membranes. However, the study of the disposal of the concentrate
by means other than reuse is necessary to complete the final evaluation of
closed cycle operation.
10
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SECTION 4
TEXTILE PROCESS DESCRIPTION
Most of the production is done on the dye range. The range consists of
a dye pad, spiral atmospheric steamer, jet washer, dip box, and four wash
boxes (see Figure 2). After the dip box and each of the four wash boxes,
nip rolls remove excess water. The range is fully automated to control cloth
speed and process temperatures. The continuous range is designed to run in
the range from 9 to 36 meters per minute depending on the fabric and process
details. Cotton, acrylic, nylon, rayon, and polyester fabrics as well as their
blends are processed on the range. Dyeing is done as a steady state process
with both the natural and synthetic fabrics.
Several classes of dyes are used: direct, dispersed, acid, pre-metalized,
basic, and fiber reactive. The dye formuli include, in addition to the dyes,
auxiliary chemicals. The dye formuli are mixed in the drug room and pumped to
the dye pad on the range. The flow to the pad is controlled by a level
control valve in the dye pad.
As the fabric leaves the pad it goes through a set of nip rollers to
remove the excess dye. The fabric then goes into an atmospheric steamer.
The steamer contains about 150 meters of fabric. The fabric speed is
determined by the residence time required in the steamer for the fabric and
dye system.
After the fabric leaves the steamer it is rinsed sequentially in a
washer employing a large recirculating flow, a small'dip box, and three
washers. The rinse water used is plant process water. Steam injection into
the washer is used to bring the rinse water to the appropriate process
temperature (Table 4).
STANDARD WASHING PROCEDURE
The rinse water from the 2nd washer counterflows by gravity to the 1st
washer which discharges to the drain. The rinse water from the 3rd washer is
pumped to the jet washer which discharges to the drain. The rinse water
from the dip box directly discharges to drain. A set of nip rollers, after
the dip box and each of the wash boxes, removes the excess water in the fabric.
The 4th washer is used as a fixing pad bath approximately 90% of the time.
When the 4th washer is not used as a fixing bath, the water counterflows to the
3rd washer. There is a set of nip rollers after the 4th washer also. When
used as a fixing pad, the 4th washer is discharged to the drain at the end of
the dye run.
11
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Dye Formula
Steam
Cloth
In
Dye
Pad
(501)
Continuous
KUster
Range
Steamer
Sump
Overflow
Jet
Washer
(3701)
Di
1st Washer U
(6301)
2nd Washer
(6301)
3rd Washer
(6301)
Floor
Drain
Figure 2. Continuous Dye Range Arrangement.
12
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The physical characteristics of the wash water are indicated in Table 4.
Noting from above that only the water from the jet washer, the dip box, and
the 1st washer discharge to drain, the total water discharge rate is 400 £/min.
The 1.0 5,/min overflow from the steamer pump is quite pure condensate. The
chemical characteristic of the individual discharges and their composite
mixed effluent are tabulated in Table 5. (The expected characteristic for
the modified washing procedure, described below, are also included in Table 5).
The chemical characterization of the dye range effluent involved
analytical parameters selected with regard to the chemicals used in the
dyeing process and to data relevent to the membrane recovery process.
Analytical procedures are summarized in Appendix A. Initially each
discharge point was evaluated, however, preliminary analysis indicated that
the steamer effluent was essentially condensate quality, and sampling at
the steamer was discontinued. The 2nd and 3rd washers were eliminated as
sampling points since the effluents from these washers are counterflowed.
The process effluents were characterized during February to May 1978.
A total of eleven production runs were sampled, direct dye formulations
applied to three automotive fabric runs, direct dye formulations applied
to three cellulosic fabric runs, fiber reactive dye formulations applied to
two cellulosic runs. These process types accounted for ^95% of the La France
dyehouse production during the sampling period.
Average effluent characteristics are tabulated in Table 5 for each
process effluent. The composition of the effluent streams is highly variable
because of the differences in dye pad bath formulations for the wide range
of shades produced with several fabrics.
The evaluation of effluent composition with time during selected runs
showed that the jet washer, dip box, and wash box effluents all reached a
steady concentration after 20 to 30 minutes from the start of the process run.
Subsequently grab samples, after 20 to 30 minutes of run-time, were used. The
fix bath samples were collected as composite samples because of the variations
of the bath composition during the entire process run.
Also of potential interest for recovery is the fix bath effluent
discharged at the end of each production run. The fixing chemicals are
generally cationic organic polymers, some of which contain an inorganic salt
such as magnesium chloride. The characteristics of the fixing bath discharge
is presented in Table 6. (The complete study of fixing chemical recovery has
been postponed.)
MODIFIED WASHING PROCEDURES
Studies have suggested that complete counterflow will improve the
washing efficiency. Also elevated water temperature should improve the
effectiveness of the washers. A series of full scale tests were conducted
at 50% reduced wash water flow rate and at elevated temperatures. The
fabric quality (hand and crock) improved with water temperature. However,
at 82 C (180 F), the highest test temperature, dye addition was required
to maintain shade. It was estimated that dye additions would range from
13
-------
TABLE 4. CONTINUOUS DYE RANGE DISCHARGE RATES AND TEMPERATURES
Unit Process
Dye Pad
Steamer Sump
Jet Washer
Dip Box
1st Washer
2nd Washer
3rd Washer
4th Washer
(Fixing Bath)
Temperature
I
20
98
20
20
40
40
40
20
( 0
- 25
- 100
- 30
- 60
- 60
-.60
- 60
- 40
Overflow
Rate (£/min)
0.5
1.0
160
140
100
35
100
0.0
Holding Volume
<*>
50
2500
370
50
650
630
630
630
-------
TABl.Ii 5. I'KKSIiNT AND EXI'lif.TEO UIFHICAl. UIAKACTLUJ STICS OF THE OYK RANUli EFFLUENT.
Average Concentrations or Flow
ASSAY
Flow, Jt/mln.
HOI), lug/*
COD, rng/t
Conductivity, mg/*
Alkalinity, mg/*
Color, ADMi
Hardness, mg/^
I'll
IMieuols, mg/*
TOC, nig/*
T'otal Solids, mg/*
Suspended Solids, mg/£
Dissolved Solids, mg/l
Cliroinium, mg/£
Co p per, mtj/J.
Iron, iug/«.
Manganese, mg/fc
Nickel, nit-/*
2.ilic, mts/*
Magnesium, rng/S
Calcium, mg/*
i)ye I'ad
.1
5 ,400
23,900
1580-28,000
4,150
98,800
2
3.6-10.9
0.84
6,250
20 , 900
1 , 7 30
19,200
5.3
19.2
2.8
0.2
0.1
2.7
10.4
7.4
.let Wash
170
88
620
110-1550
160
990
20
4.8-1.0.
0.09
180
630
17
610
0.03
0.13
0.49
0.08
0.007
0.19
6.0
2.3
er IHp 11 OK
76
130
620
190-950
70
370
32
8 4.9-10.7
_3
250
700
26
680
0.32
0.1.7
0.10
0.08
0 . 005
0.19
7.2
3.1
Wash llox //
133
122
740
130-810
40
1260
4
5.3-10.4
_3
150
600
.15
570
-'J
0.145
0 . 34
0.05
--0.001
0 . 06
1.5
1.1
1 Compos i te
Effluent
1.380
108
660
140-UOO'1
100
960
17
5. 0-10. 51'
-3
180
630
25
610
0.12
0.13
0.3C
0.07
0.004
0.14
4.6
2.0
Expected Compos i te
lit f 1 uent
v.210
200
1,200
200-2,000''
180
1,750
30b
5.0-:i0.5M
_3
325
1,140
45
1,100
0.2
0.2
0.65
0.1
0.007
0.25
8.5 =
3.5s
Dye pad drops depend on cloth pickup characteristics
concentrate and this concentration will have no influ
Sample cujor Interferes
with analytical
Too feu data were taken for a meaningful
procedure .
average .
.inn.
and volume of dye pad
eiice on HF system feed
prepared. Dye
qua! i ty .
pad drop will he
mixed with HF
d;iLa w! ] 1 probab Ly be much lower as the rue i I'nulatecJ product wil ] he soft wa
-------
TABLE 6. CHARACTERISTICS OF FIX BATH EFFLUENT
Parameters
BOD , mg/2.
COD, mg/2.
Conductivity, umho/cm
Alkalinity, mg/£-
Color, ADMI
Hardness, mg/£
PH
Phenols, mg/£
TOC, mg/£
Total Solids, mg/X.
Suspended Solids, mg/Jl
Dissolved Solids, mg/£
Chromium, mg/S,
Copper, mg/£
Iron, mg/&
Manganese, mg/&
Nickel, mg/£
Zinc, mg/H
Magnesium, mg/£
Calcium, mg/J-
Minimum
110
95
89
19
44
63
4.6
-
50
130
2
120
0.001
0.007
0.04
0.06
0.001
0.05.
1.0
1.93
Fix Bath
Maximum
110
3310
3200
32
470
460
7.2
00
780
6980
87
6890
0.05
0.09
1.15
0.46
0.10
210
1900
16.0
Average
*a
770
1140
*a
160
250
-
230
1840
34
1810
0.01
0.05
0.21
0.20
0.02
23.0
350
7.6
*a
Too few data were taken for a meaningful average.
16
-------
0-20% depending on the dye formulation. Test results are presented in
Appendix A.
The flow rates and counterflow arrangement selected for consideration in
the closed cycle operation are indicated in Figure 3. The temperature for
all the wash water will be 82 C. The largest portion, 76 £/min of the total
wash water flow, is introduced into wash box No. 1 and counterflowed. Water
is also introduced, primarily as nip roller sprays, into the other wash
boxes; 38 &/min in wash box No. 2, and 19 £/min into wash box No. 3. A
significant flow, 38 &/min is introduced into the dip box to prevent build-up
of contaminants in the dip box. Each wash box is connected to a drain so
that the water can be collected during equipment wash downs between shade
changes.
Both the low flow rate and the high temperature reduce the required
membrane area. With recycle, use of high temperature wash water does not
result in a high energy loss. The vapor losses, of course, are larger at
high temperature. However, the improved washing effectiveness with
temperature elevation permits a flow reduction such that energy conservation
is achieved with hot water washing, particularly if recycle is implemented.
The chemical characteristics of the wash water from the modified
washer arrangement were not measured. The composition of the 190 £/min
completely counterflowed wash water was calculated, Table 5, assuming the
same removal from the cloth as is achieved in the standard washing procedure.
As indicated by the improved hand and crock quality of the fabric washed
with hot water, actually more removal may be expected. The recycle system
was designed for 210 £/min flow (SECTION V). The calculated composition
therefore may be somewhat conservative.
17
-------
RINSE MAKEUP TANK (22,700 LITERS)
38£/min.
\ DIP
W
/i
m/min.
\ r
i \
38X,/min.
76£/min.
J
WASH BOX
NO. 3
f _.
I
f
WASH BOX
NO. 2
1
*
'^
l( , .
WASH BOX
NO. 1
190£/min.
H.F. UNIT
FEED ACCUMULATOR TANK
(22,700 LITERS)
CONCENTRATE
174£/min
CARRE DWG. NO. 55H
1-30-79
Figure 3. Continuous Dye Range Modified Arrangement.
-------
SECTION 5
RECOVERY SYSTEM
All the water used on the dye range, water used to wash the fabric, water
used to rinse the equipment between production runs, and the residual, full
strength liquor in the dye pad will be collected. The wash water and rinse
water flow to a 23 m3 accumulator tank and to be processed by the high
temperature hyperfiltration unit. Approximately 95% (by volume) of the
wash and rinse water will be recovered as membrane permeate. The permeate
flow to 20 m3 tank from which it will be used as needed as wash and rinse
water. The remaining 5% containing the concentrated chemical residue, will be
collected in a 3 m tank where it will be combined with the residual full
strength dye liquor. This concentrate will be used as the initial formulation
for a subsequent dye shade or will be treated for ultimate disposal.
The design of the membrane recovery system for the dye range is presented
in this section. Details of the actual installed system will be presented in
subsequent phases of this program. The system consists of accumulator tanks,
valves, pumps, meters and controls.
ACCUMULATOR TANK SIZE
Figure 4 shows conceptually the water flows involved in the recovery
sys,tem. The design wash water flow rate is 210 £/min during operation and
approximately 2700 liters following each run for wash down of the equipment.
The range is inoperative for 20 minutes or longer between consecutive
production runs. The longest production run is probably 3.67 hours (80
pieces of cloth) based on current practice. Two consecutive shifts each with
two 80 piece runs, separated by 20 minute clean-up periods is considered to be
the heaviest probable loading on the recovery system.
The accumulator tank size was selected considering its impact on the
membrane system size and capacity to permit temporary recovery unit stoppage
without overflow. An accumulator tank of 23 m3 has a holding capacity for ^2
hours of wash water flow at 210 £/min, thus providing two hours of spillfree
operation. The tankage also allows the membrane system to be sized at 170
A/min, for the two-worst-shift hypothetical case described above. The size
of the membrane unit may be reduced even more if the load profile involves
shorter production runs and/or longer periods between production runs.
The rinse accumulator tank is sized equal to the feed accumulator tank
to prevent overflow. Normal operation has the rinse tank nearly full of clean
hot water and the feed accumulator tank nearly empty.
19
-------
RINSE
MAKE UP
TANK
WASHERS
ON
DYE RANGE
LINT
FILTER
CAKE
T
FEED
ACCUMULATOR
TANK
CONG.
PERMEATE
Figure 4 Conceptual Diagram of the Recovery Syste
m.
20
-------
CONCENTRATE REUSE
The recovery system is configured to allow reuse of the permeate and
also reuse of the concentrate. Reuse of the concentrate requires a balance
of concentrate and water to the drug room. The average maximum usable.flow
rate of concentrate is approximately 9 £/min, and the maximum usable drug
room average flow is approximately 23 £/min. The recovery system will require
make-up to replace water drag-out by the cloth. The make-up requirement
closely parallels the drug room flow, Figure 5. The result shown in Figure 5
is for one selected condition of cloth speed and water content that is
reasonably typical, i.e., 20 meters/min and 1 kg per meter of cloth.
WASTE DISPOSAL
Waste from the system will include the lint cake from the 100 mesh
prefilter and any non-usable concentrate. The steamer condensate overflow
will be used as hot make-up water. The ultimate disposal of waste material
is the subject of study in Phase II and III of this demonstration project.
PERFORMANCE REQUIREMENTS
The hyperfiltration unit is designed to treat approximately 170 £/min
influent at the process temperature of 82 C (or the maximum temperature for
the membrane). The required color removal, to permit recycle of wash water
(see Reuse Tests, Appendix C) is 97% (based on a comparison of the influent
and the mixed average permeate). The concentrate flow rate from the
hyperfiltration unit should be in the range of 9 to 13.5 ft/min to permit
volume flow matching the preparation of dye formulations in the drug room.
21
-------
20
w
H
OS
W
en
PC:
w
H
o
£
15
10
Basis:
20 raeter/min.
1 kg/meter
Net Make-up Flow
10
20
30
PIECE SIZE OF RUN
Figure 5. Estimated Drug Room and Net Make-up Flowrates
22
-------
SECTION 6
MEMBRANE PERFORMANCE TESTS
A series of tests were conducted to evaluate the candidate membrane
modules, Table?, with a continuous fresh supply of wash water for an
extended time. The test conditions were altered to systematically increase
the fractional recovery of wash water as purified hot process water. At each
of three recovery levels (selected to be typical of inlet, middle, and exit
of a full-scale membrane system), the effects of velocity, pressure, and
temperature were measured. The objective of this test program was to obtain
field data covering the range of expected operating conditions so that vendors
could design a membrane unit with pretreatment for the recovery system.
f
Flux decline of a membrane due to wastewater constituents and/or due to
particulate fouling cannot be predicted exactly. Experience suggests a test
period sufficiently long for a treatment of about 20 m3 per square meter
(500 gallons per square foot) of membrane surface. Because of the membrane
flux and the availability of prototype modules, the three candidate membranes
processed widely differing volumes of rinse water. The tests are summarized
in Table 7.
While the volume of wastewater processed was low the PA-300 membrane
(spiral wound module), apparently stable flux levels were achieved within
about 5 days at each set of operating conditions. The necessity of at least
1-micron prefiltration was demonstrated by the plugging of one module.
The flux reached nearly stable levels for the Kusters membrane (formed
on the external surface by carbon tubes). A small continuing flux decline
may have been the result of plugging of the flow passage that culminated in
an excessive pressure drop after about 4 weeks. Mechanical cleaning, carried
out by the vendor, was reported to have restored the module. Prefiltration in
addition to that provided on the dye range may prevent module plugging.
The ZOPA membrane (formed on the internal surface of a single channel
stainless steel tube) achieved stable fluxes at each set of operating condi-
tions. There was no indication of plugging during the 720 hours of operation.
GENERAL- MEMBRANE PERFORMANCE
Experience indicates that the parameters that determine flux when
processing a particular fluid stream are operating time, concentration (e.g.,
recovery level), pressure, velocity, and temperature.
23
-------
TABLE 7. SUMMARY COMPARISON OF MODULES TESTED
Manufacturer
Module No.
Flow Geometry
Membrane Material
Test Operating Time
(Hours)
Permeate Processed
(Gal/ft2)
Filtration Required
Average Flux1 (GFD)
Average Color Rejec-
tion1 (%)
Average Conductivity
Rejection1 (%)
Kusters
480
External Tube
Zirconium oxide/
polyacrylate/
Carbon tube
510
275
Finer than 40
mesh screen
13
60-85
Mott-Brandon
452
Internal Tube
Zirconium oxide/
polyacrylate/
Sintered Stain-
less steel
720
900
40 mesh screen
30
>992
60-80
U.O.P.
380
Spiral Wrap
Poly(ether)
amid
520
170
Finer than
1 ym cart-
ridge
8
^99 2
>96
1 Appropriate average over test operating'time. Test conditions shown in
Figure 13 for Mott-Brandon, Figure 17 for Kusters and Figure 9 for U.O.P.
2 Exclude data taken with fiber reactive dyes. Some unexplained effect
influenced results with fiber reactive dyes. Data before and since test
reported here have not indicated any problem with fiber reactive dyes.
24
-------
Time
Flux decline with time can usually be divided into two parts: rapid
initial decline and steady long term decline.
When a new membrane is initially exposed to a waste stream a rapid flux
decline usually occurs within a short time (2). This decline may be due to a
physical or chemical 'accommodation1 between the membrane and the waste
stream. The feed constituents may alter the membrane properties either by
reaction or through formation of a self-rejecting layer.
After the rapid initial decline, a slower decline associated with
fouling, or membrane blinding, by particulates sometimes occurs. The rate
of flux decline during particulate fouling decreases with time. Because of
this characteristic, particulate fouling can sometimes be identified by a
linear plot of the logarithm of flux versus the logarithm of time.
Pressure
.Flux is expected to be a linear function of pressure. Depending on flow
configuration, velocity and concentration, nonlinearities can occur at high
pressure in the presence of large molecular weight feed solutes. At high
fluxes (at higher pressures) the large molecular weight solute forms a
boundary layer at the membrane surface with a significant resistance to
permeate flow causing an apparent decrease in permeability. This boundary
layer is dependent on the solute, flow velocity, solute concentration and
module configuration.
Velocity
Velocity effects can be characterized as either long term irreversible
effects associated with membrane fouling or short term effects which are
reversible and are associated with module hydraulics, e.g., fluid boundary
layer.
The hydrodynamic effects become particularly noticeable if the flow is
changed from turbulent to laminar. Decreasing flow velocity usually results
in a decreased flux and in some cases a decreased rejection (as observed by a
comparison between mixed feed and permeate samples).
A secondary effect of increasing velocity at a constant inlet pressure
is the reduction of module average pressure. Since pressure drop is a strong
function of the velocity, small changes in velocity in some modules may result
in large variations in module average pressure. The result is an apparent
loss in permeability with increasing velocity.
The long term effects of velocity on membrane performance usually are
associated with membrane fouling, or membrane blinding by the deposition of
particulates. If the membrane fouling is the result of particle or colloid
deposition, the rate at which the deposition occurs can be influenced by
velocity (8, 9). Higher velocities usually result in lower fouling rate.
25
-------
If feed constituents become insoluble at higher concentrations, the
precipitate can deposit on the membrane surface. Lower velocities increase
concentration polarization (10) thereby increasing the probability of
precipitates.
Concentration
Like velocity effects, concentration effects may be either short term
reversible or long term irreversible.
Short term effects are associated with the apparent lower permeability
of the more concentrated boundary layer adjacent to the membrane surface.
These effects are usually more pronounced large molecular weight species that
are present in the fluid.
Long term effects of concentration may result from the formation of
insoluble precipitates or colloids due to increasing concentration. Particles
thus formed may deposit on the membrane surface causing fouling.
Of course, concentration is related to system volumetric recovery and
thus is expected to have the most effect in downstream portions of a membrane
system.
Temperature
Experience (3, 4, 5) has shown that a plot of the logarithm of flux versus
the inverse of absolute temperature is a linear plot over a wide range of
temperatures. The slope of this plot is usually a constant for a specific
waste stream and is expected to have a value between 2000 and 4000 L. A
slope of 3000 K results in a doubling of flux with each ^25 C increase in
temperature.
TEST EQUIPMENT
High Pressure Test Unit
Shown in Figure 6 is a schematic diagram of the high pressure test unit.
The primary mechanical components of this skid-mounted hyperfiltration unit
are: (1) feed reservoir, (2) prepressurizing pump, (3) high pressure pump,
(4) heat exchanger, (5) hyperfiltration module, and (6) pressure control
valve.
The feed reservoir is a 100 liter stainless steel tank. Wastewater flow
into the tank is regulated by a liquid level control valve. A centrifugal
pump maintains a supply pressure to the suction of the Gaso positive
displacement pump.
The Gaso pump is a triplex plunger pump with stainless steel (316)
wetted parts. It has a discharge pressure of 1000 psi at a flow rate of
45 £/min with a 15-hp motor and the drive ratios now used.
26
-------
LEVEL CONTROL
CARRE Dwg. No. 152
|DYE RANGE
JET WASHER
PREPRESS URIZING
PUMP
HIGH
PRESSURE
PUMP
CONCENTRATE
Figure 6. Schematic Diagram of the High Pressure Test Unit.
-------
To protect the system, safety switches are provided to stop the motors
in the event of low suction pressure or high discharge pressure. In
addition a rupture disc pressure relief device is rated at about 1400 psi.
The heat exchanger is a concentric tube type, the outer tube is 1-inch
and the inner is 3/4-inch. The purpose of the heat exchanger is for control
of the fluid temperature in this recirculating system.
Modules of various sizes can be tested in this unit. Since the positive
displacement pump provides a constant volume of flow a manual bypass valve is
used to control the flow to a module. Two valves are in parallel following
the module. The air operated pressure control valve maintains a set
pressure (up to 1000 psi) in the system. A manual valve is for use in case
of malfunction of the automatic valve.
For testing with the pressure above 1000 psi, the high discharge pressure
safety switch can be disconnected and the system operated manually.
All pressures are indicated by bourdon-tube devices. The temperature
is indicated by thermocouple/resistance bridge devices. Grab samples can be
obtained through the indicated sample ports to provide rejection data on
specific species. This system was used primarily for testing of ZOPA and
Kusters membranes.
Low Pressure Test Unit
Shown in Figure 7 is a schematic diagram of the low pressure test unit.
The wastewater, prefiltered to module manufacturer's requirements, is intro-
duced into a 30 gallon reservoir. The reservoir supplies the suction of a
Cat positive displacement piston pump that pressurized the flow to between
50 and 400 psi. The pump produces a flow rate of 37 £/min.
The flow to the module is controlled by manual adjustment of a valve to
allow a portion of the fluid to bypass to the pump suction. The pressurized
flow from the module passes through a pressure control valve ahead of the
flow meter, The flow is then routed to either the 100 liter reservoir or
directly to the pump suction. Direct routing of the feed to the pump suction
creates a small volume system so that concentration to high recovery can be
achieved quickly.
The pressure at the module is manually controlled. The temperature of
the system is automatically controlled by regulating the flow of steam and
cooling water to the heat exchanger.
Pressures are indicated by bourdon-tube type gauges. Temperatures are ,
indicated by a thermocouple/resistance bridge devices. Sample ports for
concentrate and permeate are indicated in Figure 7.
Instruments
Conductivity measurements were made with a Balsbaugh conductivity bridge
and dip cell and color comparisons were made using a Bausch and Lomb Spec-
28
-------
LEVEL CONTROL
CONCENTRATE
LET- DOWN
o
W|DYE RANGE
iS'jET WASHER
01 FILTER
O
I
COOLING WATER
OR STEAM
FEED
RESERVOIR
IOOL
TANK
PUMP
FLOW METER
I
PRODUCT
CARRE DWG. 153
Figure 7. Schematic Diagram of the Low Pressure Test Unit.
-------
tronic 20 spectrophotometer operated at a wave length of 460 m. Permeate
flow rate was measured with a graduated cylinder and stop watch.
PROCEDURES
During the tests each module was operated at conditions representing, in
so far as practical, conditions in a full scale system. Module pressure,
flow velocities, temperature and system recoveries were varied to include
conditions expected in full scale system. Membrane flux, color, and
conductivity rejections were monitored on site. Chemical analyses were
performed on samples of concentrate and permeate to provide additional
rejection data. Periodic checks of membrane performance with a standard
reference solution of 3 g/£ sodium nitrate in tap water were made through-
out the period.
Renovation of membranes by washing was attempted periodically. In
accordance with manufacturer recommendations, the PA-300 modules were washed
with "Solution B." (a solution of 10 g/£ of EDTA and l-m£/£ of Triton X-100
in tap water with pH adjusted to 9.5 nitric acid). The membranes were
exposed to the "Solution B" for about one hour at low pressure and high
velocity at a temperature in the range of 30 C to 50 C. The flow was shut
off and the membrane was left to soak in the washing solution for
approximately one hour. The "Solution B" was then flushed out of the system
with tap water.
A clean tap water flush was performed on the zirconium oxide-
polyacrylate membranes (ZOPA and Rasters). The washing was done at low
pressure, high velocity and at temperatures in the range 30 C to 85 C.
The washing was repeated two or three times, changing the washing water
as necessary.
Both test units were continuously supplied with the fresh wash water,
unless the dye range was not in operation or processes other than dyeing were
being performed. During the periods when the range was not used for dyeing,
the permeates were returned to the reservoirs. The wash water processed in
both test units was filtered through the 100 mesh rotary screen of the jet
washer and stored in a 900 liter tank. In addition to the 100 mesh screen,
1-micron cartridge filters (Carborandum 20-inch 1-micron filter Elements No.
M39R20A) were installed in the feed line to the PA-300 testing system. The
cartridge filters were operated until differential pressure reached
recommended limits.
Feed lines to each test unit were equipped with totalizing flow meters
to facilitate system recovery calculations. Samples of product, concentrate
and feed were collected periodically in one gallon plastic bottles for
analysis and reuse evaluation. The samples for analyses were collected and
delivered to the laboratory in accordance with quality assurance procedures
approved for this project.
MEMBRANES TESTED
Table 8 summarizes the major characteristics of the three membrane
modules tested. The characteristics were provided by the vendors.
30
-------
TABLE 8. CHARACTERISTICS OF HYPERFILTRATION MEMBRANES TESTED
PA-300,
U.O.P.
ZOPA Kusters
c c
Mott-Brandon Corp. Corp.
Flow Geometry
Membrane
Material
Method of
Replacement
Prefiltration
Requirements
Maximum Temp., F
pH Range
Pressure Limita-
tions, psig
NaCL rejection at
Max. Pressure
Spiral Wound
Poly(ether)amide
Module (on-site)
1-5 microns
150-160
2-12
1000 w/S.S.
Product Tube
96.5
Tubular porous
stainless steel
Zirconium oxide-
polyacrylate
Chemically
replaced in-situ
40 mesh screen
212
4-11
1000
80-90
Carbon Tube
bundles
Zirconium oxide-
polyacrylate
Tube replacement
on-site
40 mesh screen
212
4-11
1000
.Characteristics provided by vendors
Universal Oil Products Corporation
Mott-Brandon Corporation
Kusters Corporation
31
-------
TEST RESULTS AND DISCUSSION
The objectives of these test were: (1) to determine for each membrane
the effects of time and recovery level (concentration) on both flux and
rejections, (2) to evaluate the vendor prescribed pretreatment and membrane
cleaning techniques, and (3) to generate samples of permeate and concentrate
for reuse evaluations. Results and discussion of data are presented below.
Reuse evaluations are described in Appendix C.
Results
The data obtained are presented. Summary plots showing flux and
rejections measured during the operating periods are presented as well as
plots showing the effect of pressure, temperature, and flow velocity. More
detailed performance plots and complete data are available in project report
No. 24-28. Chemical analyses of samples of feed, concentrate and permeate
water obtained in the tests are tabulated.
U.O.P. Module-
Performance summaries of the PA-300 modules nos. 90 and 380 are
presented in Figures 8 and 9, respectively. Module No. 90 operated 160 hours
during a two week period and module No. 380 operated for 520 hours during a
one month period. All feed was filtered through 1-micron polypropylene
cartridge filters.
Module No. 90 was exposed to recoveries between 0 and 80% at pressures
of 300-400 psi, temperatures of 30 to 60°C and a flow rate of 10 GPM. After
100 hours the module differential pressure began to increase while flux
increased and rejections decreased. Reversing the flow through the module
restored performance for 20 hours before failure occurred. Inspection of the
module inlet showed a visible buildup of solids.
Module No. 380 was exposed to recoveries between 0 and 96% at pressures
between 200-400 psi, a temperature of 60°C and flow rate of 7 GPM and 10 GPM.
A 1-micron cartridge filter was installed in the recirculating concentrate
line in addition to the filters on the feed line. These double filters
prevented module plugging. Pressures were varied to simulate the system
pressure at various recovery levels in a full scale system. Washing with
"Solution B" effectively restored fluxes, but subsequent exposure to dye
wash water immediately reduced fluxes to the previous levels. Color
rejection remained consistently above 99% and conductivity rejection above 96%.
Figures 10, 11, and 12 show the effects of pressure, temperature and flow
rate, respectively, on the flux of module No. 380. Figure 10 shows a
decreasing permeability with increasing recovery and time. The offset of the
lines from the origin is probably the result of plotting flux versus module
inlet pressure instead of module average pressure. Flux is a linear function
of pressure. Figure 11 shows the effect of temperature on flux at various
recovery levels. All lines are parallel with a slope of approximately 2800 K.
The effect of circulation flow rate on flux is shown on Figure 12.
32
-------
CARRE Dwg. No. 150
100
60
60
z.
o
o
ui
S40
20
O PRODUCT FLOW OR FLUX (SOLID POINTS NoN03 SOLUTION)
A CONDUCTIVITY REJECTION (SOLID POINTS NaN03 SOLUTION)
a COLOR REJECTION
50
40
u.
030
9-
8-
- O
5 -
o
0%
, /
^a>
8
o
= mCONCENTRATION
5 SCAN
O \ ^,-1
? XT >
' 1Y>^
i r^
CO fi
,25% RECOVERY ui /25% RECOVERY
/ . M _ /
11 AP = I5PSI "' INCREASING AP=30-40PS
CONCENTRATION TO
0% RECOVERY/ 79%
AP=30PSI
o PSI
P=300PSI
T=30*C
V-IOGPM
P=400PSI T=60*C V=IOGPM
10 20 30 40
PM
7/12/78
50 60, 70 80 90 100 110 120
AM PM
7/15/78 7/17/78
OPERATION TIME (HOURS!
130 140 150 1^0 170 180
7/20/78 7/24/78 7/25/78
Figure 8. Product Flow and Conducttvity and Color Rejection Versus Operation
Time for U.O.P. Module No. 90.
-------
96%
75%
>
u 50
0
o
UJ
/v- n
REJECTION (%) F
u) 5
o ^ _Q c
30
|20<
Cd
U.
J
O
~ 10
X
u.
0
f~ / WITHOUT FRESH F^D
/ WITH FRESH FEED 25%
I O MEMBRANE WASH 1
ID-D-DD-D D D D QD---CI
^ y V CONDUCTIVITY
D COLOR
PRESSURE (PS I)
, ^300 . _ 200 _ , 400
FLOW RATE (GPM)
1 n '° i 1 . 7 T 1
1 TEMPERATURE 60° C
? .
SJ '? -
SO - -O r*
i i t i i
20 _
ro
i
O
X
Q
O
1.0
O
LL.
0 ,C
O 0
PRODUCT
100 200 300
OPERATING TIME (HOURS)
400 500
CARRE Dwg. No. 166
Figure 9. Product Flow and Conductivity and Color Rejection Versus Operation
Time for U.O.P. Module No. 380.
-------
CARRE Dwg. No. 159
15 -
Q
U.
UOP PA-300
MOD. NO. 380
75% RECOVERY
96%RECOVERY(AFTER 280 HOURS)
96% RECOVERY (AFTER 440 HOURS)
100 2OO 300
PRESSURE(PSD
400
Figure 10. Flux Versus Pressure for U.O.P. Module No. 380.
35
-------
ON
20
15
S'o
o
X
2 5
UOP-PA300
MOD. NO. 380
_
-
i
-------
12.5
10.0
0 TK
' 7.5
5.0
2.5
UOP - PA 300
MOD. NO. 380
75% RECOVERY
CARRE Dwg. No. 161
5 10
CIRCULATION FLOW (GPM)
Figure 12. Flux Versus Circulation Flow for U.O.P. Module No. 380.
37
-------
Table 9 gives the filtration capacity of the 1-micron polypropylene
filters. The capacities varied widely depending on the solids loading in
the feed. The average capacity is about 315 gallons per filter cartridge.
Chemical analyses of 5 concentrate/permeate sets of samples are
presented in Table 10. Rejection of all analyses parameters are greater
than 90%.
Mott-Brandon Module
The performance summary for Mott-Brandon (MBC) ZOPA membrane module No.
452 is presented in Figure 13. The module was operated for 720 hours during
a 6 week period from July 18 to September 1. Recoveries were varied between
0 and 96%, velocities between 2 and 6 m/sec. and pressures between 200 and
1300 psi. The temperature was 85 C. The module was washed six times with
hot tap water. The only prefiltration was the 100 mesh screen on the dye
range. Fluxes were partially restored by the hot water washes.
On July 31, after about 200 hours of operation, the Kusters module No.
480 (below) was installed in the high pressure test unit. Because of the
limited flow rate capacity of this test unit pump (^45 £/min) it was necessary
to test the modules in series to assume proper flow velocities. The Mott-
Brandon tubular unit had already been tested for 200 hours and shown no
evidence of plugging, the Kusters unit was installed upstream to gain similar
experience with this unit. Since the test unit employed a high degree of
recirculation and the module recoveries are essentially zero for each pass,
the chemical composition of the feed was less than 1% difference between the
upstream and downstream module positions.
Color rejection rose on initial exposure to the dye wash water to about
99% and remained high throughout the test. Erratic behavior of flux and
rejection between 560 and 650 hours is the result of exposure to a fiber
reactive dye formulation with a pH of 9 to 10. Steady performance returned
with exposure to a direct dye formulation.
Figures 14, 15, and 16 show the effects on membrane flux of pressure,
temperature and velocity, respectively. Figure 14 shows a decreasing
permeability with increasing recovery. Nonlinear response of flux to pressure
is seen at pressures greater than 1100 psi. Figure 15 shows the effects of
temperature on flux. All lines are parallel with a slope of about. 2800 K.
The effect of velocity on flux is seen in Figure 16.
Chemical analyses of six concentrate and permeate samples are given in
Table 11. The COD and total solids rejections at all recovery levels are
^,90%.
Chemical analyses of two concentrate and permeate samples are given in
Table 12. The COD and total solids rejections at all recovery levels are
^90%. ' -
Kusters Module
The Kusters Module No. 480 was installed in the high pressure test unit,
upstream of the Mott-Brandon module, on July 31. The two were then operated
simultaneously under the same conditions until August 31. The operating
38
-------
TABLE 9. THE CAPACITY OF THE CORBORUNDUM FILTER ELEMENTS
FILTER NUMBER CAPACITY3 (gallons)
1st Filter
2nd Filter
3rd Filter
4th Filter
5th Filter
6th Filter
7th Filter
8th Filter
9th Filter
10th Filter
llth Filter
12th Filter.
662 gallon
335 gallon
278 gallon
215 gallon
440 gallon
176 gallon
181 gallon
118 gallon
351 gallon
216 gallon
374 gallon
432 gallon
Gallons of wash water, prefiltered
through a 100-mesh screen, at 20 psi
differential pressure.
39
-------
TABLE 10. CHEMICAL ANLAYSIS OF CONCENTRATE AND PERMEATE FOR NODDLE NO. 'S 90 AND 380
KECOVERY LEVEL
SAMI'I.E TYl'E
ANI) NUMBKK
DATK TAKEN
COD, ing/*
Conduct I vlty ,
|ililho/i:m
I'll
Hariluesa , lujj/t
Dibbolvcd Sulidu,
niB/l
Tuta 1 !jol ids, '
uiB/1
Vol Ul le ik. Uclu.
mg/Jt
Suspends. 1 Sul.Ldu,
iiiJi/H
Chromium, my/fc
Iron, ui8/t
Calcium, liiy/36
Ma(.;neijluiii, in^/Ji
25^ -
Cuncen.
#1158
7/14//H
5JO
«20
7.7
14
518
5^0
Vi6
V
0.186
0.520
3.200
2.AOO
('90
Purmeate
«J157
7/14//B
4
J5
5.9
(I
5
5
5
0
0.00 'I
o . o i y
0.008
0.00'J
2.")% -
#1168
7/1B/78
260
195
7.1
19
316
320
177
I,
0.021.
0.9/0
2.160
2.880
#90
Permeatu
#1169
7/18/78
16
12
6.0
0
26
26
. u
0
0.001
0.020
0.005
0.006
75%
Cuncen.
#1380
7/26/78
560
840
7.2
79
H17
830
388
13
0.025
0.180
17.500
9 . 800
- //380
Permeate
#1181
7/26/78
23
17
5.6
0
24
32
21
8
0.003
0.034
0.002
0.011
75% -
Concen .
#1185
7/28/78
1270
1200
7.2
83
1571
1580
779
9
0.320
0.550
25 . 300
10.800
#380
Permeate
#1186
7/28/78
8
19
5.4
0
1 1
15
11
4
0.013
0.045
0.002
0.005
96% -
Concen .
#1204
8/11/78
1530
1990
7.6
125
2445
2470
1140
25
3.300
1.050
31.000
22.400
#380
Penriuate
#1205
8/11/78
10
21
6.4
0
15
28
21
0
0 . 002
0.02'j
0.003
0.005
-------
LJ 50
>
o
o
UJ
J
25V,
UNKNOWN RECOVERY
O MEMBRANE WASH
WITHOUT FRESH FEED
WITH FRESH FEED
CARRE Dwg. No. 167
50L
10
SOLID POINTS INDICATE
NaN03 REFERENCE DATA
18
VELOCITY (FPS)
8
8 6
V CONDUCTIVITY
D COLOR
8
TEMPERATURE 85°C
PRESSURE SOOpsi
I
I
100
200
300 400 5OO
OPERATING TIME (HOURS)
600
700
Figure 13. Product Flow and Conductivity and Color Rejection Versus Operation
Time for Mott-Brandon Module Mo. 452.
750
-------
50
40
u.
o
X
ID
20
10
ZOPA MOD. NO. 452
T » 85'C
D 25% RECOVERY, 8 FPS, 85*C
O 75% RECOVERY, 8 FPS, 85°C
96% RECOVERY, 18 FPS, 85°C
A 75%RECOVERY, 18 FPS, 85°C
O 25% RECOVERY, 18 FPS, 85°C
200
400
600 800 1000
PRESSURE (PSD
1200 1400
CARRE DWG. 157
Figure 14. Flux Versus Pressure for Mott-Brandon Module No. 452.
-------
GJ
40
30
20
o
u.
10
75% RECOVERY (AFTER 160 HOURS OPERATION, 18 FPS)
MOO. NO. 452
800 PSI
25% RECOVERY
'AFTER 60 HOURS OPERATION 18 FPS)
25% (AFTER 550 HOURS OPERATION 8 FPS)
~-96% RECOVERY.
' AF'ER 2SO HOURS OPERATION 18 FPS)
2.8
2.9
3.0
3.1
3.2
TEMP( °K x I03)
3.3
90
80
70
60 50
TEMP. (°C)
40
Figure 15. Flux Versus Temperature for Mott-Brandon Module No. 452.
60
CARRE DWG. 158
-------
30
~ 20
o
u.
x
10
ZOPA MOD. NO. 452
75% RECOVERY
85° C, 800 PSI
CARRE Dwg. No. 155
1
10 15
VELOCITY (FPS)
20
Figure 16. Flux Versus Flow Velocity for Mott-Brandon Module No. 452.
44
-------
TAIlLli 11. CHEMICAL ANI.AYSl'.S OK CONCENTRATE AND PERMEATE SAMPLES FOR HUTT-UKANUUN MODULE NO. 452
On
ItKCOVEKY LEVEL
SAMPLE TYPE
AND NUMBEU
DATE TAKEN
CUU,,»B/*
Conductivity,
tiinlio/cm
I'll
Hardness, mg/ll
Dlssoiveil Solids,
nig/Ji
Tumi Solids,
Volutl !e Soil da,
Suspended Solids,
nig/ It
Chromium, mg/Ji
C0|>|>t:r,mg/l
Iron, mg/J.
Calcium, mg/jt
Magnesium, mg/ii
25!
Conceit.
01170
7/18/78
150
135
6.5
13
187
200
104
13
0.041
-*
0.240
.1.710
1 .750
I
Permeate
01171
7/18/78
38
35
7.0
0
45
45
37
0
0.002
_*
0.018
0.017
0.030
2
Concen .
01173
7/21/78
470
315
7.0
29
459
470
288
11
0.020
-A
0.560
2.800
4.780
5%
Permeate
011.74
7/21/78
46
67
7.4
0
42
51
37
9
0.003
-A
0.015
0.037
0.240
757
011.77
7/26/78
570
570
7.1
75
710
750
405
40
0.051
-*
0 . 660
16.40 -
9.40
01178
7/26/78
38
120
7.1.
0
.67
80
37
13
0.004
-*
0.026
0.32
0.39
75
01185
7/28/78
1320
815
6.9
84
1330
1360
791
30
0.340
_*
1.900
31 . 20
10.60
Z
011.86
7/28/78
69
162
7.2
0
122
124
52
'2
0.004
-A
0.024
0.23
0.29
965
011.89
8/3/78
4270
1700
5.1
232
3280
3330
2)50
50
0.010
-A
1.300
40.00
31 .40
/
Permeate
0.1190
8/3/78
180
255
5.6
2.5
250
250
118
0
0.027
-*
0.016
o . 4 n
0.76
25
01217
8/29/78
336
395
7.7
18
487
494
281
7
-.A
0.483
-A
4.00
2.87
"L
01218
8/29/78
24
8ft
7.4
0
45
45
18
0
-*
0.009
-ft
0.017')
0 . 0 JO
-------
TABLE 12. CHEMICAL ANALYSIS OF CONCENTRATE AND PERMEATE SAMPLES FOR KUSTERS
MODULE NO. 480
Recovery Level
96%
25%
Sample Type
and Number
Date Taken
Concentrate
#1189
8/3/78
Permeate
#1191
8/3/78
Concentrate
#1217
8/29/78
Permeate
#1204A
8/28/78
COD, mg/£
Conductivity, ymho/cm
PH
Hardness, mg/£
Dissolved Solids, mg/£.
Total Solids, mg/Jl
Volatile Solids, mg/£
Suspended Solids, mg/Jl
Zinc, mg/ £
Chromium, mg/£
Copper, mg/£
Iron, mg/£
Calcium, mg/£
Magnesium, mg/£
4270
1700
5.1
232
3230
3330
2150
50
_*
0.010
_*
1.300
40.00
31.40
140
255
5.7
2.5
120
120
118
0
_*
0.003
_*
0.008
0.56
0.75
336
395
7.7
18
487
494
281
7
0.131
_*
0.483
_*
4.00
2.87
56
87
7.5
0
155
157
2
0.007
_*
0.008
-*
0.14
0.16
*Not analyzed.
46
-------
conditions for the Kusters module required testing in the high pressure test
unit. The flow rate specification was such that it was not possible to
divide the 45 &/min output of the test pump between the Kusters module and
the MBC (above) module. After consultation with the Kusters technical repre-
sentative, it was decided to place the module in series upstream of the MBC
module. This, would provide comparable data since the MBC module has already.
been operated for 200 hours as the only module in the unit. Figure 17 shows
flux and rejection performance of the module No. 480 during the 510 hours of
operation. Recovery values were varied between 0 and 85%, pressures between
400 and 130 psi and volume flow rates between 5 GPM and 12 GPM. The
temperature was 85 C. Feed prefiltration was the 100 mesh screen.
At 510 hours the module was removed from service after its differential
pressure rose to 90 psi. Four hot tap water washes were performed. Between
the 390 and 470 hour points the membrane was exposed to wash water from a
fiber reactive dye formulation at pH of 9 to 10 and exhibited erratic
rejection behavior. Stable operation was restored with a tap water wash.
Color rejection remained about 99% throughout the tests.
Figures 18 and 19 show the effects of pressure and temperature on flux.
A nonlinear response of flux to pressure is seen at pressures greater than
900 psi. The higher permeability for 96% test occurred first. Like other
modules tested, temperature effects generated parallel lines with a slope of
about 2800 K (Figure 19).
Discussion
The results are generally those expected for membrane processing of the
dye wash water. The formulation contained several low molecular weight
species, i.e., the dyes and most of the auxiliary chemicals. The use of the
guar gum thickener in the dye pad introduced a high molecular weight
constituent which influenced flux performance.
Operation Time and Concentration-
The long periods of time are required to concentrate the test solution
to high values of recovery. Therefore the effects of concentration are
sometimes not differentiated from the effect of operation time. An increase
in recovery level (concentration) generally results in a decrease in flux.
These decreases may be irreversible; therefore, the flux observed at 25%
recovery after operation at 96% recovery may be lower than the flux initially
observed at 25%. This membrane 'memory' necessitates a careful examination
of the membrane history before conclusions are made concerning membrane flux.
U.O.P. modules Figure 8 shows the flux history of module No. 90. The
67% reduction in flux in the first 20 hours of operation was accelerated by
the increase in recovery to 25%. The washing at 65 hours operation restored
the flux, but the flux declined quickly after subsequent exposure to the
effluent stream.
Figure 9 shows the history of module No. 380. After the failure of
module No. 90, a 1-micron cartridge filter was installed in the recirculation
line in addition to the 1-micron filter at the system supply line. This
second filter removed particulate build-up within the system. A flux decline
47
-------
100
50
100
96%
UNKNOWN
WITHOUT FRESH FEED>
WITH FRESH FEED /75%
O MEMBRANE WASH
25%
25%
_q%_y
25% 25%
O
O OO
D- DDDO-n
£
z
o
o 80
UJ
12
DC.
i
60
A
X
^\* ~i ^i ft Jk^ ^
- j£ Ar' A^^------1^ A
A CONDUCTIVITY
L D COLOR £
PRESSURE (PSD £
820
FLOW RATE (6PM)
11 ..5 .III,5,,4,,
^ A,
!\ * ^
^ \ A Hz
k ' 860 890
A 1
" 1
5 .1
i
TEMPERATURE 85 C
.200
g 50
^
t 40
^L.
< 30
o
I20
.
UL
10
-
i
.1
i
l
-\
1-
\
_ ^x>-5> o^*^"*- o ooo ^^^
1 1 1 1
150 1
_i
1
»
100 3
H
0
50 §
0 100 200 300 400 500
OPERATING TIME (HRS)
CARRE Owg. No. 168
Figure 17.
Product Flow and Conductivity and Color Rejection Versus
Operation Time for Kusters Module No. 480.
48
-------
20
15
Q
U_
X
=? 10
KUSTERS HF MOD. NO. 480
96% RECOVERY, 11 GPM,85°cP
25% RECOVERY,
85°C
5 GPM
75% RECOVERY,
85eC
5 GPM
I
I
I
I
200 400
Figure 18. Flux Versus Pressure for Kusters Module No. 480.
600 800 1000
PRESSURE, PSI
1200 1400
CARRE DWG. 156
-------
70
60
50
40
30
o
u.
20
10
KUSTER HF
MOD. NO. 480
3g/| NaN03, 820 PSI, IIGPM
(NEW MODULE)
25% RECOVERY, 820 PSI, 5 GPM
(360 HOURS OF OPERATION)
96% RECOVERY, 820 PSI, IIGPM
(90 HOURS OF OPERATION)
2.8
2.9
H-
90
70
3.2
3.3
40
80
60 50
TEMP. (°C)
Figure 19. Flux Versus Temperature for Kusters Module No. 480.
30
CARRE DWG 154
-------
similar to the initial decline seen in Figure 8 was again observed. Following
the washing of the membrane with tap water, the pressure was lowered from
300 psi to 200 psi. Over the next 300 hours of operation, the flux declined
from about 10 GFD to 5 GFD. A wash with UOP "Solution B" resulted in a flux
increase. Operation thereafter at a pressure of 400 psi produced a flux
decline from 22 GFD to 12 GFD.
A flux increase is sometimes observed for recirculation without the
addition of fresh feed. The operating period between 275 hours and 340 hours
shows this effect. The flux increase at the 465 hour mark is attributable
to a combination of washing the membrane, raising the pressures and reducing
the concentration.
Experience suggests that when 500 gallons of fresh effluent per square
foot of membrane area is processed, values of flux and rejection are usually
stable. Sometimes stable performance is achieved for shorter periods of
operation, however.
The module No. 380 processed only 125 gallons of effluent per square
foot of membrane area. The results presented in Figure 9 indicate stable
values of flux and rejection. The previous experience with module No. 90
indicates that prefiltration requirements- for the spiral configuration should
be examined carefully.
Mott-Brandon moduleFigure 13 shows the history of Mott-Brandon module
No. 452 over 700 hours of operation time. The initial decrease in flux from
greater than 100 GFD to 50 GFD occurred during the first 20 hours of exposure
to the dye wash water. A recovery (concentration) increase to 25% resulted
in another rapid flux reduction to (>30 GFD) at the 20 hour point. Periodic
tests with a standard sodium nitrate solution showed this initial loss in
flux was not recovered by tap water washing. Color rejection rose signifi-
cantly during the initial flux decline period while conductivity rejection
increased slowly.
Operation without the addition of fresh feed resulted in a flux increase
with time. Periodic washing of the membrane with tap water resulted in a
partial restoration of flux each time. It appears that the tap water washing
may be sufficient to maintain flux at a relatively constant value.
Color rejection remained high throughout the test period. Conductivity
rejection remained constant at near 80% except during high pH operation.
Operation at 25% recovery between 340 hours and 390 hours indicate a
lower flux than operation at the 75% recovery level between 100 and 180 hours
previously. This reduction in flux is probably due to the 96% recovery level
operation between 225 and 285 hours.
During the 700 hours of testing the Mott-Brandon module processed 760
gallons of effluent per square foot of membrane area.
Kusters moduleThe Kusters module was installed, in series, upstream of
the Mott-Brandon module on July 31, 1978. Its performance is shown in Figure
51
-------
17. The two membranes were operated at the same conditions until September 1,
when the Kusters module was removed for repairs after the module pressure
drop unexpectedly rose. The Kusters module displayed an initial flux decline
in the first 30 hours from 70 GFD (with salt water) to 30 GFD. The processing
of fiber reactive (high pH) dye wash water resulted in erratic conductivity
performance while color rejection remained high.
The Kusters membrane is a zirconium oxide-polyacrylate membrane similar
to the ZOPA membrane, therefore, qualitatively similar performance would be
expected. Dissimilarities in performance may be attributed to differing
hydrodynamic conditions that exist in flux through tubes and flow outside
tubes in tube bundles. Hot tap water washes partially restored fluxes.
The Kusters module 488 processes 275 gallons of effluent per square
foot of membrane area. The increase in module pressure drop seen at 500 hours
indicates prefiltration requirements should be examined carefully.
Pressure
Flux is expected to be a linear function pressure unless boundary
layer resistances to permeate flow become significant compared to membrane
resistances. Nonlinearities were seen at high pressures with the Mott-
Brandon and Kugters module. The U.O.P. modules were not operated at
sufficiently high pressures to observe this phenomenon.
U.O.P. modulesFlux versus module inlet pressure shown in Figure 10.
The permeability decreases with increasing time and concentration. The
change in permeability from 0.034 to 0.029 GFD/psi during 160 hours of
operation is probably a time effect due to fouling or compaction. The offset
of the lines from the origin are the result of either inaccuracy in the date
or of plotting versus inlet pressure rather than average module pressure.
Mptt-Brandon moduleFigure 14 shows the nonlinearities of flux versus
pressure at approximately 1100 psi where boundary layer flux resistance
become significant compared to membrane resistance.
The initial permeability at 25% recovery and 60 hours, is 0.05 GFD/psi.
At 530 hours the 25% recovery permeability was 0.035 GFD/psi following an
exposure at 96% at 275 hours. The lower permeability is believed to be a
result of the intervening exposure to higher concentration.
Kusters moduleFigure 38 shows the nonlinearities of flux versus
pressure at approximately 900 psi. A higher permeability is shown for 96%
recovery at 275 hours. The lower permeability is believed to be a result of
the intervening exposure to the higher concentrations.
Temperature-
Figures 11, 15, and 19 show the logarithm of-flux plotted versus the
inverse of absolute temperature for the three membranes. The slope is
nearly constant for all membranes with a value near 2800 K. Therefore a
rise in temperature from 56 to 85 C or from 36 to 60 C would result in a
doubling of flux.
52
-------
Velocity
Figures 12 and 16 show the short term effect of velocity on flux. The
reason for the shapes of the curve is unclear, but it should be noted that
the velocity scans were performed with a constant inlet pressure. In Figure
12 the secondary effect resulting from increasing pressure drop with
increasing velocity probably influenced the low flux at the highest velocity.
Long term velocity effect as seen in the flux versus time plots (Figures
8, 9, 13, and 17) are minimal in the range of velocities observed.
53
-------
SECTION 7
ECONOMICS
The economics of recovery are based on a comparison of the operating
cost of the recovery system and the savings due to recycle. Of course,
both savings and costs are only estimates at this Phase in the studies. It
is the purpose of Phase II and Phase III of this demonstration project to
generate empirical data on the economics. In this section are presented
estimates of savings for reduced use of energy, water, and chemicals due to
recycle. The operating costs for the membrane recovery unit are estimated
by the equipment vendors. The payback period is based on the quoted installed
costs for the ZOPA membrane system minus the $85,000 estimated to be non-
representative for a typical commercial installation.
SAVINGS
The basis for the calculation of the potential savings is the 1979
La France operating budget. Since the membrane system was designed to
handle the dye range production based on 120 hours per week including 33%
down time, the savings are estimated on this same basis. The savings
estimates are tabulated in Table 13.
Reduced Water Reuse
The annual savings of $22,870 attributed to reduced water use is about
equally divided between water supply and waste treatment cost, i.e., $11,570
and $11,300 respectively. These savings are realized from reduced energy
and chemical requirements. Since the water system facilities are already in
place at La France, recycle will reduce neither the depreciation nor the labor
cost. For a new plant, both the capital and labor requirement for water
supply and waste treatment would be effected by the degree of water recycle
in the plant.
It is expected that additional treatment facilities will be required at
La France to comply with scheduled future effluent guidelines. Closed cycle
operation of the dye range will reduce the cost of these tertiary or
additional treatment facilities. However, no estimate of these cost
reductions has been made and no credit has been taken for these potential
savings.
Reduced Energy Use
The annual savings of $62,000 attributed to reduced energy use is
essentially all due to recycle of hot process water; 96% recycle is assumed.
54
-------
The reduced chemical cost for boiler make-up water treatment of $2,000 is the
proportionate part of the annual plant budget for this item.
Reduced Dye Formulation Chemicals Use
The actual budget for dyes and chemicals is proprietary information. The
savings are estimated based on the 1979 budget. The reuse scenario is that
the production will be scheduled so that the concentrate from light shades
can be recycled to darker shades. In a normal shift, eight production runs
so scheduled will yield 87% recycle of concentrate even if the concentrate
from the last run must be discharged for disposal. (Disposal will be studied -
during Phase II and Phase III).
The technical feasibility of recycling the concentrate was studied
(Appendix C). Additional tests are scheduled in Phase II to establish
procedures for scheduling and handling the concentrate to accomplish the
reuse. The potential savings of chemicals, and their indirect energy
equivalence, is a major factor in the economics of this project. The
practicality of chemical recycle is a major question to be answered in
this demonstration.
Since the reuse plan calls for recycle only within a single 8-hour
production shift, the build-up of extraneous materials is not expected to
interfere with the planned reuse. However, any build-up will be monitored.
OPERATING COSTS
The operating costs are estimates as supplied by Mott-Brandon Corporation
in response to the invitation to bid. Of course, it is the purpose of this
demonstration to obtain actual data during Phase III. The major cost items
are labor (including payroll tax), electric power and general maintenance.
The annual operating cost is estimated to be $16,510. The breakdown per
category is given in Table 14.
PAYBACK PERIOD
The payback period for the $400,000 installed cost of the recovery
system, calculated by the standard method employed by Riegel Textile Corpora-
tion is 3.8 years. If reuse of dye does not prove to be practical the period
is 5.2 years. While the actual payback formula is proprietary, it does contain
provisions for taxes: and the interest cost of money.
55
-------
TABLE 13. ESTIMATED ANNUAL SAVINGS1 DUE TO RECYCLE
Reduced Water Use $
Water Treatment 11,570
Waste Treatment 11,300
Reduced Energy Use
Hot Water Recycle 60,000
Boiler Feed Chemicals 2,000
Reduced Dye Formulation Chemical Use
Dyes 61,631
Auxiliary Chemicals 95,053
Total Savings $241,554
1Based on 1979 operating budget.
TABLE 14. ESTIMATED MEMBRANE SYSTEM1 OPERATING COSTS2
1.
2.
3.
4.
5.
6.
Operator Labor (6 man-months/year)
Cleaning Chemicals
Electric Power (40 horsepower) 3
Maintenance Parts
Payroll Tax
Total Costs
$ 7,000
700
5,010
3,000
800
$16,510
^Based on equipment vendor estimate.
2Based on 1979 operating budget.
3Based on 2.8 per kilowatt hour; February 1979.
56
-------
REFERENCES
1. Brandon, C. A. and J. L. Gaddis. Full-Scale Demonstration of Hyperfiltra-
tion for Closed-Cycle Textile Dyeing Facility. Desalination, 23: 19-28,
1977.
2. Brandon, C. A. and M. Samfield. Applications of High-Temperature
Hyperfiltration Unit Textile Processes for Direct Recycle. Desalination,
24: 97-112, 1978.
3. Brandon, C. A. and J. J. Porter. Hyperfiltration for Renovation of
Textile Finishing Plant Wastewater. EPA-600/2-76-060, U.S. Environmental
Protection Agency, Research Triangle Park, NC, 1976, 147 pp.
4. Brandon, C. A., J. J. Porter, and D. K. Todd. Hyperfiltration for
Renovation of Composite Wastewater at Eight Textile Plants. EPA-600/2-78-
047, U.S. Environmental Protection Agency, Research Triangle Park, NC,
1978, 237 pp.
5. U.S. Environmental Protection Agency Grant No. R803875, Dr. Max Samfield,
Project Officer, Industrial Environmental Research Laboratory, Research
Triangle Park, NC.
6. U.S. Environmental Protection Agency Grant No. R805182, Dr. Max Samfield,
Project Officer, Industrial Environmental Research Laboratory, Research
Triangle Park, NC.
7. U.S. Environmental Protection Agency Grant No. R805777, Dr. Max Samfield,
Project Officer, Industrial Environmental Research Laboratory, Research
Triangle Park, NC.
8. Todd, D. K. An Experimental Investigation of Flux Decline of Dynamically
Formed Zirconium Oxide-Polyacrylate Membranes Exposed in an Annular
Geometry to Suspensions of Particulates Circulated at Different Axial
Velocities. Masters Thesis, Clemson University, Clemson, SC, 1977, 51 pp.
9. Sheppard, J. D. and D. G. Thomas. Effect of High Axial Velocity on
Performance of Cellulose Acetate Hyperfiltration Membranes. Desalination,
8: 1-12, 1970.
10. Johnson, J. S., Jr. Polyelectrolytes in Aqueous Solutions. Reverse Osmosis
Membrane Research, 379-403. H. K. Lonsdale and H. E. Podall, ed. Plenum
Press, 1972.
57
-------
APPENDIX A. DYE RANGE EFFLUENT CHEMICAL ANALYSES
TABLE Al. VARIATION IN DYE RANGE EFFLUENT WITH TIME FOR AUTOMOTIVE FABRIC
Suspended
Sampling Time Solids Conductivity
Point (min.) (mg/£) (umho/cm) pH
Jet Washer 0
30
60
90
120
150
180
210
composite
Dip Box 0
30
60
90
120
150
180
210
composite
Wash Box 1 0
30
60
90
120
150
180
210
composite
Fix Bath 0
30
60
90
120
150
180
210
composite
23
65
60
68
62
64
60
64
63
13
61
60
60
68
68
58
66
64
19
55
52
58
58
54
56
56
55
24
47
59
55
56
42
57
53
60
200
290
290
290
300
320
315
315
300
160
320
350
350
360
340
370
380
350
130
240
190
235
230
225
230
230
225
8400
7000
5400 .
4100
3700
6500
4900
4300
5300
7.4
7.4
7.5
7.4
7.4
7.4
7.4
7.4
7.5
7.6
7.4
7.6
. 7.5
7.6
7.6
7.6
7.5
7.6
7.2
7.2
7.3
7.3
7.3
7.3
7.3
7.3
7.3
4.6
4.7
4.8
5.0
5.2
5.0
5.2
5.4
4.9
Optical
Density
0.45
0.80
0.78
0.78
0.85
0.84
0.85
0.85
0.82
0.33
1.02
1.10
1.20
1.20
1.16
1.16
1.20
1.16
0.40
1.06
1.14
1.30
1.20
1.24
1.28
1.16
1.22
0.26
0.28
0.25
0.41
0.39
0.27
0.32
0.41
0.34
58
-------
TABLE A2. CHARACTERIZATION OF DYE RANGE EFFLUENTS FOR AUTOMOTIVE FORMULA'9917
(DIRECT AND ACID DYES) FEBRUARY 9, 1978
ASSAY
BOD , mg/Jl
COD, mg/Jl
Conductivity, ymho/cm
Alkalinity, mg/Jl
Color, ADMI
Hardness, mg/Jl
pH
Phenols, mg/Jl
TOC, mg/Jl
Total Solids, mg/Jl
Suspended Solids, mg/Jl
Dissolved, mg/Jl
Chromium, mg/Jl
Copper, mg/Jl
Iron , mg/ Jl
Manganese, mg/Jl
Nickel, mg/Jl
Zinc, mg/Jl
Magnesium
Calcium, mg/il
Pad
3850
35,400
6500
930
186600
<25
8.1
3.9
12060
20760
2100
18660
25
32
2.8
0.23
<0.08
2.3
5.5
10
Steamer
__
81
54
40
9.2
39
18
21
Jet
Washer
50
460
250
50
690
10
7.4
0.09
90
300
31
269
0.052
0.14
0.10
0.09
<0.01
0.13
1.2
2.1
Wash
Box #1
100
650
250
35
1360
5
7.8
0.06
190
520
37
483
0.19
0.24
0.32
0.06
<0.01
0.18
1.1
1.7
Fix
Bath
380
3200
3200
100
420
700
4.9
0.31
140
6900
50
6850
0.028
0.03
1.2
3.8
0.02
1.4
115
8
59
-------
TABLE A3. CHARACTERIZATION OF DYE RANGE EFFLUENTS FOR AUTOMOTIVE FORMULA 9917
(DIRECT AND ACID DYES) MARCH 16, 1978
ASSAY
BOD,., mg/£
COD; ing/ 4
Conductivity, pmho/cm
Alkalinity, mg/£
Color, ADMI
Hardness , mg/ £
PH
Phenols, mg/£
TOC, mg/£
Total Solids, mg/£
Suspended Solids, mg/£
Dissolved Solids, mg/£
Chromium, rag/ H
Copper, mg/&
Iron, mg/Jl
Manganese, mg/Jl
Nickel, mg/£
Zinc, mg/£
Magnesium, mg/&
Calcium, mg/&
Pad
7400
37300
5200
660
175500
*
7.8
2.1
15700
20500
1680
18820
28
24
2.9
0.04
<0.001
2.6
3.1
2.3
Jet
Washer
850
290
30
1020
9.5
7.6
0.07
240
530
33
497
0.09
0.28
0.09
0.04
0.001
0.32
1.1'
0.95
Dip
Box
_
1260
320
28
80
6
7.6
0.05
470
810
58
752
0.2
0.29
0.15
0.04
<0.001
0.49
1.0
0.93
Wash
Box #1
1120
230
1320
7.3
660
57
603
__
Fix
Bath
3310
3200
180
5.0
780
6980
87
6893
0.02
0.025
1.15
0.35
<0.001
208
816
9.5
*Dye interferes with method.
60
-------
TABLE A4. CHARACTERIZATION OF DYE RANGE EFFLUENTS FOR AUTOMOTIVE FORMULA 9342
(DIRECT AND ACID DYES) APRIL 25, 1978
ASSAY
BOD , mg/£
COD, mg/2,
Conductivity, ymho/cm
Alkalinity, mg/£
Color, ADMI
Hardness, mg/&
PH
Phenols, mg/£
TOC, mg/£
Total Solids, mg/£
Suspended Solids, mg/&
Dissolved Solids, mg/£
Chromium, mg/&
Copper, mg/£
Iron, mg/£
Manganese, mg/£
Nickel, mg/£
Zinc, rog/£
Magnesium, mg/£
Calcium, mg/£
Pad
1900
22160
3000
725
40190
*
7.8
1.70
4880
11270
710
10560
19
18
3.5
0.14
<0.04
5.1
4
7
Jet
Washer
480
210
45
285
14
7.3
0.31
183
400
20
380
0.10
0.11
0.09
0.05
<0.005
0.17
1.0
2
Dip
Box
__
500
200
45
270
14
7.3
154
363
12
351
0.10
0.10
0.16
0.07
<0.005
0.2
2
2.1
Wash
Box #1
__
464
160
365
7.6
325
12
313
Fix
Bath
560
1700
74
5.6
96
2000
2
1998
0.008
0.04
1.0
0.46
<0.005
1.4
152
16
*Dye Interferes with method.
61
-------
TABLE A5. CHARACTERIZATION OF DYE RANGE EFFLUENTS FOR DIRECT DYE FORMULA 9811,
MARCH 2, 1978
ASSAY
BOD , mg/Jl
COD, mg/£
Conductivity, ymho/cm
Alkalinity, mg/Jl
Color, ADMI
Hardness, mg/Jl
PH
Phenols, mg/Jl
TOC, mg/Jl
Total Solids, mg/Jl
Suspended Solids, mg/Jl
Dissolved Solids, mg/Jl
Chromium, mg/ Jl
Copper, mg/Jl
Iron, mg/Jl
Manganese, mg/Jl
Nickel, mg/Jl
Zinc, mg/Jl
Magnesium, mg/Jl
Calcium, mg/Jl
Pad
2600
11040
1950
130
49100
*
6.2
<0.01
2050
5630
950
4680
<0.05
31
1.0
0.18
<0.07
0.06
7.5
6.0
Jet
Washer
44
150
110
22
90
10
7.2
<0.01
42
190
3
187
0.001
0.11
0.04
0.027
<0.01
0.02 .
3.0
1.6
Dip
Box
85
400
300
24
62
53
7.1
<0.01
97
470
53
417
0.004
0.21
0.09
0.080
<0.01
0.04
16
1.6
Wash
Box #1
170
740
210
24
440
13
7.1
<0.01
165
420
30
390
0.003
0.42
0.13
0.070
<0.01
0.04
3.6
0.9
Fix
Bath
110
970
1750
19
44
560
4.6
<0,01
215
3020
29
2991
0.004
0.09
0.38
0.20
0.01
0.06
1900
15
*Dye interferes with method.
62
-------
83IP
TABLE A6.
CHARACTERIZATION OF DYE RANGE EFFLUENTS FOR DIRECT DYE FORMULA 9821,
30.IAH SYCI :j? ASSAY-"-1" q-f'Pad * Washer
±>eS I-i -coS xoS
BOD , mg/A
COD, mg/£
Conductivity , 'iimho/cm
Alaklinity, ragy"]!.
Color, ADMI ""
Hatdness, mg/£
p'H"
'-Ptfenols, mg/£
TOG, mg/£
"Total Solids, mg/£
-^Suspended Solids, mg/£
Dissolved Solids, mg/£
*- Chromium, mg/£
*' Copper, mg/£
Iron, mg/5,
Manganese, mg/£
Nickel , mg/ H
Zinc, mg/Ji
Magnesium, mg/£
Calcium, mg/£
2660
9040
4350
330
82530
JL
6.4
0.25
1730
9010
1230
8780
0.062
18
0.72
0.17
<0.036
0.56
33
7.4
430
575
130
106
27.5
6.4
0.001
188
724
24
700
<0.003
0.13
0.14
0.08
<0.004
0.09
42
3.7
Dip
Box
800
800
190
222
61.1
6.4
313
1160
36
1124
0.003
0.22
0.14
0.12
0.007
0.11
17
6.2
Wash
Box //I
830
750
248
6.4
1170
64
1106
__
Fix -
Bath
430
1250
178
6.1
154
1480
36
1444
0.003
0.05
0.048
0.26
0.007
0.52
169
10
*Dye interferes with method.
63
-------
TABLE A7. CHARACTERIZATION OF DYE RANGE EFFLUENTS FOR DIRECT DYE FORMULA 9168
MAY 1, 1978
ASSAY
BOD , ing/ A
COD, mg/X,
Conductivity, ymho/cm
Alkalinity, mg/Jl
Color, ADMI
Hardness, mg/&
PH
Phenols, mg/£.
TOC, mg/Jl
Total Solids , mg/ £
Suspended Solids, mg/fi,
Dissolved Solids, mg/£
Chromium, mg/ H
Copper, mg/2.
Iron, mg/£
Manganese, mg/£
Nickel, mg/£.
Zinc, mg/fc
Magnesium, mg/£
Calcium, mg/Jl
Pad
1650
9680
5300
310
117590
*
6.3
0.52
2670
10040
1725
8315
0.2
26
1.0
0.22
0.036
0.56
24
12
Jet
Washer
__
252
410
83
140
12.7
6.3
0.22
100
440
23
417
0.003
0.12
4.4
0.13
0.004
0:06
4.3
2.5
Dip
Box
__
670
950
176
280
53.7
6.3
290
1200
35
1165
0.003
0.4
0.14
0.11
0.029
0.13
17
5.9
Wash
Box #1
870
810
770
6.3
1200
79
1121
~
Fix
Bath
_
385
1010
62
6.2
256
1100
37
1063
<0.003
0.07
0.1
0.20
0.018
0.31
85
7.2
*Dye interferes with method.
64
-------
TABLE A8. CHARACTERIZATION OF DYE RANGE EFFLUENTS FOR ACRYLIC FORMULA 8951
(BASIC DYES) MARCH 14, 1978
ASSAY
BOD mg/£
COD, mg/£
Conductivity, ^mho/cm
Alkalinity, mg/il
Color, ADMI
Hardness, mg/&
PH
Phenols, mg/Jl
TOC, mg/il
Total Solids, mg/il
Suspended Solids, mg/J>.
Dissolved Solids, mg/Jl
Chromium, mg/£
Copper, mg/£
Iron, mg/Jl
Manganese, mg/£
Nickel, mg/£
Zinc, mg/£
Magnesium, rog/j!,
Calcium, mg/Jl
Pad
16400
43100
4000
*
191000
A
4.4
0.18
4580
16140
5150
10990
0.03
21
1.2
0.14
0.04
1.8
2.7
6.5
Jet
Washer
200
620
240
41
970
o**
6.7
<0.01
170
370
1
370
<0.001
0.055
0.05
0.04
0.004
0.07
3.2
1.3
Dip
Box
180
520
190
34
890
1.5
7.1
<0.01
150
340
4
336
0.002
0.039
0.05
0.04
0.001
0.04
3.3
1.3
Wash
Box #1
175
560
130
21
1100
o**
7.1
150
320
16
304
0.003
0.053
0.46
0.04
<0.001
0.05
1.5
1.5
Fix
Bath
110
380
460
32
180
63
7.0
120
660
72
588
0.003
0.058
0.11
0.09
<0.001
0.06
18
2.4
* Dye interferes with methods-.
** Zero by method.
65
-------
TABLE A9. CHARACTERIZATION OF DYE RANGE EFFLUENTS FOR ACRYLIC FORMULA 8960
(BASIC DYES) APRIL 25, 1978
ASSAY
BOD , mg/£
COD, mg/£
Conductivity, umho/cm
Alkalinity, mg/£
Color, ADMI
Hardness, tng/&
pH
Phenols, mg/£
TOG, mg/Jl
Total Solids, mg/£
Suspended Solids, mg/£
Dissolved Solids, mg/£
Chromium, mg/£
Copper, mg/£
Iron, mg/£
Manganese, mg/£
Nickel, mg/Jl
Zinc, mg/Jl
Magnesium, rag/£
Calcium, mg/£
Pad
9400
47360
6500
0*
146970
**
3.6
0.378
8540
58370
3160
55210
<0.042
34
1.1
1.0
<0.04
9
11
12
Jet
Washer
1730
660
60
6300
133
4.8
0.016
410
1210
14
1196
<0.004
0.42
0.16
0.08
<0.005
0.96
6
4.2
Dip
Box
1300
540
64
850
78
4.9
430
910
15
895
<0.004
0.22
0.11
0.09
<0.005
0.57
5
4.8
Wash
Box #1
1390
390
5230
5.3
870
36
834
Fix
Bath
144
130
.
470
7.2
180
155
14
141
0.004
0.07
0.10
0.06
<0.005
0.06
1.0
2.1
*Zero by method.
**Dye interferes with method.
66
-------
TABLE A10. CHARACTERIZATION OF DYE RANGE EFFLUENTS FOR ACRYLIC FORMULA 8956
MAY 11, 1978
ASSAY
BOD , rag/Jl
COD, mg/£
Conductivity, umho/cm
Alkalinity, mg/£
Color, ADMI
Hardness, mg/£
PH
Phenols, mg/ a
TOC, mg/£
Total Solids, mg/£
Suspended Solids, mg/£
Dissolved Solids, mg/£
Chromium, mg/£
Copper, mg/£
Iron, mg/£
Manganese, mg/£
Nickel, mg/£
Zinc, rag/ H
Magnesium, mg/£
Calcium, mg/£
Pad
11400
25400
1580
*
56030
**
3.8
0.15
7130
11120
1880
9240
0.025
5.56
0.76
0.14
0.159.
6.57
5.6
5.93
Jet
Washer
__
800
210
1.0
790
8.8
5.10
0.05
240
490
9
481
0.005
0.041
0.093
0.20
0.016
0.24
2.32
4.55
Dip
Box
. __
790
200
5.0
535
12.5
5.30
240
480
11
469
0.005
0.030
0.090
0.17
0.01
0.12
2.96
4.00
Wash
Box #1
__
800
170
600
5.70
470
26
444
^^
Fix
Bath
__
95
90
122
.
6.75
50
133
15
118
0.050
0.041
0.54
0.10
0.10
0.10
1.16
1.93
*Zero by method.
**Dye interferes with method.
67
-------
TABLE All. CHARACTERIZATION OF DYE RANGE EFFLUENTS FOR FORMULA 996 (FIBER
REACTIVE), FEBRUARY 1, 1978
ASSAY
BOD , mg/£
COD; mg/£
Con due t tvi.ty , ymho /cm
Alkalinity, mg/£
Color, ADMI
Hardness, mg/£
PH
Phenols, mg/£
TOC, mg/£
Total Solids, mg/&
Suspended Solids, mg/5,
Dissolved Solids, mg/j!,
Chromium, mg/Z
Copper, mg/£
Iron, mg/£
Manganese, mg/£
Nickel, mg/£
Zinc, mg/£
Magnesium, mg/£
Calcium, mg/£
Pad
1200
14150
28000
20400
4400
48
10.8
0.05
7500
40240
160
40080
0.043
0.114
0.067
0.104
0.12
0.122
12
6.4
Steamer
6
12
130
8
9.6
50
<1
50
Jet
Washer
58
630
1550
700
1400
6
10.6
0.01
230
1240
6
1234
0.002
0.012
0.052
0.08
0.01
0.044
1.4
0.8
Wash
Box #1
39
340
280
83
1490
2
10.0
<0.01
80
270
10
260
0.001
0.005
0.074
0.04
0.005
0.019
0.8
0.5
Wash
Box #2
5
31
95
16
125
1
8.0
<0.01
11
74
3
71
0.001
0.002
0.050
0.02
<0.005
0.005
0.7
0.2
68
-------
TABLE A12. CHARACTERIZATION OF DYE RANGE EFFLUENTS FOR FORMULA 995 (FIBER
REACTIVE), MARCH 13, 1978
ASSAY
BOD , mg/£
COD, mg/£
Conductivity, ymho/cm
Alkalinity, mg/£
Color, ADMI
Hardness, mg/£
PH
Phenols, mg/£
TOC, mg/£
Total Solids, mg/£
Suspended Solids, mg/£
Dissolved Solids, tag/ H
Chromium, mg/£
Copper, mg/Jl
Iron , mg/ H
Manganese, mg/£
Nickel, mg/£
Zinc, mg/£
Magnesium, mg/Jl
Calcium, mg/Jl
Pad
900
8150
2250
18000
36750
*
10.9
0.042
1850
26600
291
26309
0.01
0.19
0.85
0.09
0.2
0.34
5.8
5.6
Jet
Washer
400
1500
650
450
3
10.8
0.013
120
1000
22
978
0.001
0.007
0.11
0.04
0.004
0.02
0.9
1.4
Dip
Box
220
820
370
7.5
10.7
80
600
11
589
0.001
0.011
0.05
0.03
<0.001
0.02
0.6
1.1
Wash
Box #1
330
420
2450
**
10.4
160
370
19
352
<0.001
0.009
0.7
0.02
<0.001
0.03
0.5
1.0
Fix
Bath
660
700
110
130
6.2
240
1070
11
1062
0.001
0.007
0.08
0.11
<0.001
0.05
6.8
4.2
*Dye interferes with method.
**Zero by method.
69
-------
APPENDIX B. MODIFIED WASHING PROCEDURE TESTS
Test of high temperature washing have shown that by lowering the rinse
water flow rate by about 50% there is no decrease in cloth quality. Increasing
the rinse water temperature from 40 C to 60 C, the cloth quality is improved
over standard washing conditions with no effect on fabric shade. Further
increase in temperature to 82 C (180 F) still improves the cloth quality,
but results in shade reduction to be below standard with some standard dye
formulations. The amount of additional dye required ranges between 0 and 20%.
CURRENT WASHING EFFECTIVENESS
The effectiveness of the current washing procedures was determined. On
24 production runs samples of cloth were taken: one at the exit of the steamer
(prior to washing) and the second just prior to the fix bath (after washing was
complete). The 8 inch x 8 inch square samples were washed in a series of one-
liter baths. The wash water was collected and analyzed for conductivity, color
and dissolved solids. Table Bl shows results for the twenty-four sets of
samples. The removal percentage is calculated by the expression:
_ . /a/> -,nn /, Amount Removal from Cloth Sample Washed on Range s
Removal (%) = 100 (1 - -r = r= ^rrr^: -r-9)
Amount Removal from Cloth Sample Prior to Washing
on Range.
The results indicate that 32% of the removable color is removed in the
wash boxes and 72% of the dissolved solids" are removed. The average solids
removed from the cloth is 7.35 grams per yard. Dissolved solids were measured
rather than total solids due to the fraying of the patches during washing
giving erratic total solids data. The results show considerable variation
from one sample to another. The variations would not be correlated by fabric
pattern or dye color code.
HIGH TEMPERATURE, LOW FLOW RATE WASHING TESTS
The washing effectiveness of the continuous dye range at various rinse
water flow rates, flow arrangements and temperatures was evaluated. Five
pieces (approx. 55 yards each) of cotton/rayon cloth were dyed using a dark
brown shade selected by the dye house supervisors as a critical test of
temperature effects.
The first piece of cloth was dyed using normal water flow rate,
arrangement, temperature, and range speed. The second piece was dyed using
a lower water flow rate with normal temperature and complete counterflow to
the jet washer; the third piece was dyed using the lower water flow rates
with 140 F water temperature and complete counterflow; the fourth piece was
70
-------
dyed using the lower water flow rate and 160 F water temperature and complete
counterflow; and the fifth piece of cloth was dyed using the lower water flow
with 180 F water temperature and complete counterflow.
Patch samples were taken at various points along the washer sections.
The patches were washed in the laboratory using the procedures described
above. Table B2 shows the washing effectiveness results obtained from .
analysis of the laboratory wash water. The results indicate little effect
of flow rate or temperature on removal of dissolved solids from the fabric.
Surface color removal is significantly increased at high temperature. Surface
color removal is desirable in that the crocking property of the fabric is
improved. However, excessive color removal may result in requiring additional
dye for some shades.
71
-------
TABLE Bl. WASHING EFFECTIVENESS AS DETERMINED BY DAILY PATCH SAMPLES FROM
NORMAL PRODUCTION RUNS DURING THE PERIOD 3/21/78 to A/20/78.
PATCH
NO.
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
21
22
23
24
25
PATTERN
CODE
1174
1203
1198
1174
1174
1175
1222
416
416
1175
1174
1198
1152
1211
1211
1211
1211
1174
1174
' 1152
1174
1112
1112
1174
COLOR
CODE
689
249
736
338
111
901
338
703
225
737
336
089
224
2249
8149
133
010
133
717
234
3325
402
133
249
SURFACE
COLOR
REMOVED
%
28
23
18
44
45
67
29
25
61
3
20
38
41
89
16
26 .
20
10
42
26
14
22
23
16
DISSOLVED (1)
SOLIDS
REMOVED
%
99
88
83
67
57
73
93
76
69
96
79
81
95
89
90
62
70
80
72
33
30
16
57
67
DISSOLVED (1)
SOLIDS
REMOVED
gm/yd
10
21
8.7
7.4
3.6
2.3
11.3
2.7
3.1
14
11
4.6
15
3.8
3.2
4.4
3.9
8.3
7.0
2.8
1.5
1.0
6.8
19
AVERAGES
32
72
735
'Removal percentages determined by comparison between results of laboratory
washings of patches taken at the exit of the steamer and jus.t prior to the
fix bath.
72
-------
TABLE B2. WASHING EFFECTIVENESS WITH VARYING WASH WATER FLOWRATE
AND TEMPERATURE
Total Range Surface Dissolved Solids Dissolved Solids
Temperature Flowrate Color Removed Removed Removed
°C fc/min % % gm/yd
43 370 - 47 8.9
43 190 47 51 10.3
60 190 42 48 8.7
71 190 53 44 6.9
82 190 64 51 10.0
73
-------
APPENDIX C. REUSE EVALUATION
The purpose of the reuse evaluation tasks conducted by Texidyne, Inc.
were to evaluate the recovery and reuse potential of concentrate and permeate
generated by hyperfiltration and ultrafiltration of dye range effluents.
The following evaluations were conducted to evaluate the recovery
potential of membrane concentrate and permeate:
1) Fabric samples were dyed in the La France dye lab using membrane
water samples to estimate dye recovery potential.
2) Feed, concentrate and product samples were analyzed in the Texidyne
laboratory to determine chemical recovery and reuse.
3) Certain tests (e.g., viscosity and foaming measurements) were
conducted in the Texidyne laboratory to estimate membrane recovery
of dye bath auxiliaries.
4) Analyses of process chemicals were conducted at Texidyne to deter-
mine the suitability of recovery/recycle.
All reuse tests conducted were on a laboratory scale and must be verified
during plant scale trials. The ultimate reuse and recovery potential of a
given waste stream can only be determined during a long-term operation of the
membrane treatment system. However, certain preliminary evaluations were made
under the limitations of short-term tests.
Concentrates and permeates generated by membrane treatment of dye range
wash water were evaluated for reuse potential.
Three dye pad additives pad thickeners, dyes, and foaming agents
are found in most dye pad formulations used at La France. One objective of
the reuse tests was to determine if these additives could be recovered in
hyperfiltration concentrates.
Mass balances studied have shown that 35-45% of the dyes and chemicals
applied to the fabric in the pad bath are rinsed out in the wash boxes.
This means that 35-45% of the process chemicals used on the dye range at La
France are theoretically available for recovery. High temperature counter-
flow washing should remove essentially all of the dye bath auxiliaries from
the fabric. Factors limiting recovery potential include degradation of
process chemicals, build-up impurities, and the development of satisfactory
reuse procedures and production schedules.
Some estimates of chemical, recovery can be made based on membrane
performance, reuse tests, and characteristics of the process chemicals.
Estimates of process chemical recovery from the continuous dye range at La
France are listed in Table Cl. « .-
"-.-'- 74
-------
TABLE Cl. ESTIMATE OF CHEMICAL RECOVERY VALUE IN LA. FRANCE DYE RANGE RINSE
WATER HYPERFILTRATION CONCENTRATES
ft
Chemical % Savings from Recycle
Pad Thickener (guar gum) Inconclusive
Dyes 0-15%°,
Foaming Agents 40-60%
Salt 60-80%e
a
.Expressed as a percent of chemicals applied to fabric.
Recovery of pad thickener cannot be determined during short-term tests.
,Dye savings will depend on compatibilities of pad formulas.
Based on foam tests.
3
Salt is not added to all pad formulations. Recovery data is based on
membrane salt rejection performance.
75
-------
One specific dye pad additive evaluated for recovery was the dye pad
thickener. The thickener used at this textile plant was an industrial grade
guar gum. A-Brookfield Viscometer was used in laboratory tests to measure
guar gum concentrations. Attempts to estimate thickener concentrations in
membrane concentrations using viscosity measurements were unsuccessful. This
is not surprising since the dye range rinse water was circulated through the
membrane for periods of up to seven days at elevated temperatures (160-180 F).
A full-scale membrane system with shorter residence time may improve guar
gum recovery.
Product water samples were evaluated in the La France laboratory for
reuse as process water. The laboratory dyeings indicate that hyperfiltration
is more suitable than ultrafiltration for recycle of hot dye range wash water.
Ultrafiltration products are not suitable for use as general process water
because of poor color (dye) rejection. The residual dye in the product could
effect the shades of subsequent dyeings.
Hyperfiltration product water was found to be suitable for reuse as
general process water. This was found to be suitable for use as process water
to prepare dye formulations and for use as hot wash water. Average permeate
characteristics, compared to the plant tap water characteristics, are shown
in Table C2.
Foaming agents in concentrate waters were estimated using a semiquanti-
tative test. Water samples were agitated in a graduated cylinder and the
resulting foam height was measured as an estimate of foaming agent concentra-
tions. The results, Table C3, show that foaming agents were rejected by the
membrane. The foaming agents appear to be relatively stable at the tempera-
ture conditions of the membrane system.
Concentrate samples generated by membrane treatment 'of dye range wash
water were evaluated in the La France dye lab for dye recovery. The
laboratory dyeings showed that considerable dye could be recovered in the
concentrate water. However, the savings due to the dye reuse can only be
determined during a long series of production runs. The scheduling of
production shades will optimize the value of recovering dyes for reuse.
Test results are presented in Table C4.
76
-------
TABLE C2. COMPARISON OF AVERAGE DYE RANGE WASH WATER HYPERFILTRATION PERMEATE
WATERS AND LA FRANCE PROCESS WATER
a b
Permeate Waters Process Waters
7/18/78-8/31/78 7/78-8/78
COD, mg/£
Conductivity, ymho/cm
Hardness, mg/£
pH
Total Solids, mg/Jl
Suspended Solids, mg/£
Dissolved Solids, mg/£
Volatile Solids, mg/£
Chromium, mg/£
Iron , rag/ I
Calcium, mg/£
Magnesium, mg/£
50
101
2
6.5
78
5
73
39
0.006
0.047
0.57
0.46
9
90
9
7.05
60
3
57
18
0.002
0.022
2.36
1.00
^Represents an average of 14 samples.
Represents an average of 8 samples.
77
-------
TABLE C3. FOAMING AGENT REUSE EVALUATION
Sample Description Foam Height1
Pad Formulation 20
Pad, diluted 1/2
w/deionized water 34
Pad, diluted 1/4
w/deionized water 34
Feed 17
Concentrate . 27
Product <1
Measured in a graduated cylinder. Heights
reported are relative.
78
-------
TABLE C4, SUMMARY OF REUSE EVALUATIONS: DYE PAD FORMULATION RESIDUAL
Sample No.
Sample Description
Reuse Evaluation/Recovery Potential
1093
Dye Pad Drop Mixture
1100
vO
Dye Pad Drop Mixture
UF Concentrate
1098
1099
Dye Pad Drop Mixture
UF Produce
A sample of wastewater taken from a mixture of
dye pad residues was evaluated for color in the
La France laboratory. The composite residue gave
an olive color when applied to a velour fabric
with the Laboratory Kusters pad. The addition
of yellow (4 g/£) and grey (4.2 g/&) dye to the
pad mixture gave a commercial shade (Pat. 1112).
The concentrate from an ultrafilter separation of
the above dye pad mixture (1093) was padded with
the laboratory dye machine to evaluate color yield.
The color obtained was approximately four times
as dark as sample 1093 and had the same shade.
This result indicates that pad mixture can be
concentrated by ultrafiltration. However, the dyes
were not separated from the pad thickener.
Sample 1098 contained no color. Apparently the
dye auxiliaries formed a rejecting layer on the
membrane since UF membranes do not normally reject
dyes. Sample 1099 contained a small amount of
color. These waters could be used to prepare a
pad formulation, but have no dye value.
-------
TABLE C5. ANALYTICAL DATA: DYE PAD FORMULATION MEMBRANE SAMPLES
ASSAY
#1093
SAMPLE NUMBER
#1098 #1099
#1100
BOD , mg/£
COD? mg/£
Conductivity, umho/cm
PH
Phenols, mg/£
Dissolved Solids, mg/£
Total Solids, mg/£
Suspended Solids, mg/Jl
Zinc, mg/Jl
Chromium, mg/£
Copper, mg/£
Iron, mg/£
6931
920
630
1138
1550
7.1
.224
996
1021
25
4.6
0.014
1.40
0.059
960
1684
2350
7.1
.206
1892
1906
14
0.70
0.017
3.83
0.210
4000
14,592
3125
7.1
.326
9962
10,367
405
1.9
0.11
31.3
2.41
80
-------
TABLE C6. SUMMARY OF REUSE EVALUATIONS:
FROM MEMBRANE SCREENING TEST
DYE RANGE WASH WATER SAMPLES
Sample No,
Sample Description
Reuse Evaluation/Recovery Potential
1061
Dye Rinse UF
Concentrate
oo
1062
Dye Rinse UF
Product
1140
1141
Dye Rinse HF
Concentrate
Dye Rinse HF
Product
This concentrate water contained significant
amounts of acid and direct dyes. This concen-
trate was used to develop a production shade.
No problems were observed, although more dye
(0.637% OWF) was required for the concentrate
bath than for the normal production dyeing
(0.599% OWF). For this particular shade a
negative dye savings was realized because the
dye shades were not compatible.
The product water contained approximately 20%
as much dye as the concentrate (1061). This
amount of dye would prohibit the use of this
product sample as general process water. Water
analyses also indicate that this water would
not be suitable for general process use (total
solids = 270 rog/Jl, COD = 350 mg/£).
A large quantity of direct red dye was recovered
in this concentrate, A deep red dye formula was
developed from this water with a resulting dye
savings of approximately 10%.
This product water contained a small amount of
direct dye. Overall water quality was good,
and this water should be suitable for most
process requirements-.
-------
TABLE C6, CONTINUED
Sample No. Sample Description Reuse Evaluation/Recovery Potential
1087 Dye Rinse HF This rinsewater concentrate water contained a
Concentrate mixture of dyes that stained a test cloth of a
tan shade. Dye savings would result if this
concentrate was used to develop a darker tan
or brown shade.
1088 Dye Rinse HF This product water was equal to, or superior to,
Product the quality of textile plant tap water. Can be
used in all process applications requiring tap
N> water.
-------
TABLE C7.
ANALYTICAL DATA:
SCREENING TEST
DYE WASH WATER SAMPLES FROM MEMBRANE
SAMPLE NUMBER
ASSAY
BOD , mg/£
COD; mg/x,
Conductivity, ymho/cm
pH
Phenols, mg/£
Dissolved Solids, mg/&
Total Solids, mg/&
Suspended Solids, mg/£
Zinc, mg/£
Chromium, mg/ H
Copper, mg/£
Iron, mg/£
#1061
960
2627
240
8.2
.060
1659
1711
52
2.99
0.17
0.19
4.75
#1062
120
346
170
8.2
.040
266
269
3
0.03
0.006
0.03
0.04
#1087
289
853
369
7.3
0.06
790
798
5
0.56
0.042
0.237
0.53
#1088
<1
50
85
7.5
0.002
68
68
<1
0.029
0.003
0.014
0.024
83
-------
TABLE C7. CONTINUED
SAMPLE
SAMPLE NUMBER
#1140 #1141
COD, mg/£ 1344 43
Conductivity, ymho/cm 1100 200
pH 6.6 7.0
Dissolved Solids, mg/£ 1561 127
Suspended Solids, mg/£ 15 6
Chromium, mg/£ 0.035 0.0035
Iron, mg/SL 0.67 0.068
Calcium, mg/Jl 24.6 0.535
Magnesium, mg/£ 17.0 0.70
84
-------
TABLE C8. SUMMARY OF REUSE EVALUATIONS:
LONG TERM MEMBRANE TESTS
WASH WATER SAMPLES FROM
Sample No.
Sample Description
Reuse Evaluation/Recovery Potential
OC
1174
1181
1186
1188
1190
1191
1203
1207
1180
1185
1187
Dye Rinse HF
Products
Dye Rinse HF
Concentrate
Dye Rinse HF
Dye Rinse HF
Concentrate
Product sample 1190 and 1191 had a pink color or
tint. No other product samples contained any
measurable dyes. The product waters were equal
or superior to the quality of plant tap water.
These waters are suitable for general process use.
The concentrate water contained only a small amount
of red dye and gave a pink pastel shade when used
for a laboratory Kusters dyeing. No trouble was
encountered when the sample was used to prepare a
compatible plant formulation. This concentrate has
minimal dye recovery value; recovery of auxiliaries
(e.g., foaming agents) may be significant.
This concentrate was essentially colorless. The
rinse water probably came from a pastel shade,
because very little dye was removed in the rinse
water. This concentrate should be compatible with
most production shades.
This sample contained a small amount of dyes that
tinted the test fabric green. This concentrate
should be compatible with most medium -and dark
production shades.
-------
TABLE C8. CONTINUED
Sample No.
Sample Description
Reuse Evaluation/Recovery Potential
00
1189
1202
1211
Dye Rinse HF
Concentrate
Dye Rinse HP
Concentrate
Dye Range HF
Concentrate
This concentrate contained a significant amount
of acid red and direct red dyes. The residual
dye concentration was approximately 10-15% of the
dye required to match production shade.
This concentrate water contained a mixture of dyes
that gave a grey shade on the test fabric. Dye
savings will be realized if the concentrate is
used to dye a grey to black shade.
The concentrate contained no measurable dye
concentration. This type of concentrate is
compatible with most production formulas. Recycle
value is the recovery of foaming agents and other
dye pad auxiliaries.
-------
TABLE C9. ANALYTICAL DATA: DYE WASH WATER SAMPLES
FROM LONG-TERM MEMBRANE TESTS
ASSAY
#1174
SAMPLE NUMBER
#1181 #1186 #1188
#1190
COD, mg/X 46 23 69 8 180
Conductivity, umho/cm 67 17 162 19 255
Hardness, mg/X, Qa Qa 0& 0* 2.5
pH 7.4 5.6 7.2 5.4 5.6
Dissolved Solids, mg/X, 42 24 122 11 250
Total Solids, mg/X, 51 32 124 15 250
Suspended Solids, mg/X, 9 8 2 4 <1
Chromium, mg/X, 0.003 0.003 0.004 0.013 0.027
Iron, mg/X, 0.015 0.034 0.024 0.045 0.016
Calcium, mg/X, 0.037 0.002 0.23 0.002 0.43
Magnesium, mg/X, 0.24 0.011 0.29 0.005 0.76
Volatile Solids, mg/X, 37 21 52 11 118
0 by method.
87
-------
TABLE C9. CONTINUED
ASSAY
#1191
SAMPLE NUMBER
#1203 #1207
COD, mg/Jl 140 29 40
Conductivity, pmho/cm 255 19 670
Hardness, mg/£ 2.5 Oa 0
pH 5.7 5.6 11.2
Dissolved Solids, mg/£ 120 25 250
Total Solids, mg/£ 120 38 250
Suspended Solids, mg/£ <1 13 <1
Chromium, mg/£ 0.003 0.003 0.222
Iron, mg/£ 0.008 0.016 0.069
Calcium, mg/£ 0.56 0.008 0.005
Magnesium, mg/£ 0.75 0.006 0.054
Volatile Solids, mg/£ 76 37 44
0 by method.
88
-------
TABLE C9. CONTINUED
ASSAY
SAMPLE NUMBER
#1202 #1211
BOD , mg/£ 74
COD, mg/£ 1770 296
Conductivity, umho/cm 1980 380
Hardness, mg/£ 130 17
pH 7.4 7.35
Dissolved Solids, mg/£ 2465 417
Total Solids, mg/A 2480 423
Suspended Solids, mg/S, 15 6
Zinc, mg/& 0.202
Chromium, mg/£ 3.8
Copper, mg/Ji 0.483
Iron, mg/X, 0.59
Calcium, mg/5, 27.0 4.67
Magnesium, mg/fc 22.0 3.00
Volatile Solids, mg/£ 1170 203
89
-------
TABLE CIO. IDENTIFICATION OF MEMBRANES USED TO GENERATE
WATER SAMPLES EVALUATED FOR REUSE
SAMPLE NUMBER
MEMBRANE
TYPE OF SAMPLE
1093
1098
1099
1100
1061
1062
1087
1088
1140
1141
1174
1181
1186
1188
1190
1191
1203
1207
1180
1185
1187
1189
1202
1211
_
Mott-Brandon UF
GCDM Co.1 UF
2
Mott-Brandon UF
Mott-Brandon UF
Mott-Brandon HF
Mott-Brandon HF
Mott-Brandon HF
Mott-Brandon HF
Mott-Brandon HF
UOP HF
Mott-Brandon HF
UOP HF
Mott-Brandon HF
Kusters HF
UOP HF
Mott-Brandon HF
UOP HF
Mott-Brandon HF
UOP HF
M-B/Kusters3 HF
UOP HF
M-B/ Kusters3 HF
Raw Range Rinse Water
Product
Product
Concentrate
Concentrate
Product
Concentrate
Product
Concentrate
Product
Product
Product
Product
Product
Product
Product
Product
Product
Concentrate
Concentrate
Concentrate
Concentrate
Concentrate
1GCDM Co., Gaston County Dyeing Machine Company
Concentrate from feed ($1093) with Both Mott-Brandon UF and GCDM Co. UF used
simultaneously.
Concentrate with both Mott-Brandon HF and Kusters HF used simultaneously.
90
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TECHNICAL REPORT DATA
(Please read instructions on the reverse before completing}
1. REPORT NO.
EPA-600/2-80-055
2.
3. RECIPIENT'S ACCESSION NO.
4. TITLE AND SUBTITLE
Closed-cycle Textile Dyeing: Full-scale
Hyperfiltration Demonstration (Design)
5. REPORT DATE
March 1980
6. PERFORMING ORGANIZATION CODE
7. AUTHOR(S)
Craig A. Brandon (Carre, Inc.)
8. PERFORMING ORGANIZATION REPORT NO.
9. PERFORMING ORGANIZATION NAME AND ADDRESS
LaFrance Industries
LaFrance, South Carolina 29656
10. PROGRAM ELEMENT NO.
1BB610
11. CONTRACT/GRANT NO.
Grant No. S805182
12. SPONSORING AGENCY NAME AND ADDRESS
EPA, Office of Research and Development
Industrial Environmental Research Laboratory
Research Triangle Park, NC 27711
13. TYPE OF REPORT AND PERIOD COVERED
Phase; 9/77-4/79
14. SPONSORING AGENCY CODE
EPA/600/13
15. SUPPLEMENTARY NOTES IERL-RTP project officer is Max Samfield, Mail Drop 62, 919/
541-2547. EPA-600/2-76-060 is a related report.
16. ABSTRACT
report des cribes the first (design) phase of a full-scale demonstration
of hyperfiltration for closed-cycle operations of a LaFrance Industries dye house.
(The remaining three phases are installation, operation, and maintenance.) The
decision to demonstrate the process was based on earlier projects that showed hyper
filtration to be potentially economical for recycle /reuse of energy, water, and chem-
icals in textile preparation, dyeing, and wet finishing. On-site pilot tests of three
hyperfiltration modules led to the selection of the Mott-Brandon ZOPA module.
Representative wash waters from LaFrance dyeing operations were characterized as
a basis for demonstration equipment design. The dye range is to be converted to
counterflow with a water flow rate of 50 gpm at 82 C , with 96% of the wash water
recovered as permeate for direct recycle. Reuse and/or disposal of the concentrate
and dye pad residuals will require further study. Payback period, without credit for
chemicals recovery, is estimated to be 5.2 years.
17.
KEY WORDS AND DOCUMENT ANALYSIS
DESCRIPTORS
b.lDENTIFIERS/OPEN ENDED TERMS
c. COSATI Field/Group
Pollution
Textile Finishing
Dyeing
Filtration
Regeneration
Pollution Control
Stationary Sources
Closed Cycle Systems
Hyperfiltration
13B
13H
07D
18. DISTRIBUTION STATEMENT
Release to Public
19. SECURITY CLASS (ThisReport)
Unclassified
21. NO. OF PAGES
100
20. SECURITY CLASS (This page)
Unclassified
22. PRICE
EPA Form 2220-1 (9-73)
91
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