United States
                     Environmental Protection
                     Agency
                     Industrial Environmental
                     Research Laboratory
                     Research Triangle Park NC 27711
                     Research and Development
                     EPA-600/S2-84-100 July 1984
SER&          Project  Summary
                     Investigation of  Textile  Dyebath
                     Reconstitution  and  Reuse
                     Jon F. Bergenthal and Anthony J. Tawa
                       About 80% of textile finishing mills
                     discharge their wastewater to publicly
                     owned treatment works. Most of the
                     wastewater receives little or no  pre-
                     treatment before discharge. A variety of
                     wastewater recycle/reuse technolo-
                     gies, allowing these mills to reduce the
                     amount of wastewater and pollutants
                     discharged, were described in an earlier
                     (Phase I arid II) report.
                       This  two-volume (Phase III) report
                     examines in detail one of these recycle
                     technologies, dyebath reconstitution
                     and reuse. This technology is considered
                     promising for several reasons: signifi-
                     cant environmental benefits, potential
                     for widespread application, low capital
                     cost, cost savings in textile dyeing,
                     and economic attractiveness.
                       Volume 1 gives results of a detailed
                     investigation of dyebath reconstitution
                     and reuse at a carpet mill. The results of
                     bench-, pilot-, and full-scale testing are
                     presented. Wastewater data document-
                     ing the pollutant reductions achieved
                     through dyebath reuse are presented.
                     The economic feasibility of implement-
                     ing the technology full-scale is addressed.
                       Volume 2 gives detailed procedures
                     and methods for implementing dyebath
                     reconstitution and reuse. It can be used
                     as an operations manual for other mills
                     wishing to investigate this technology.
                       This Project Summary was developed
                     by EPA's Industrial Environmental
                     Research Laboratory, Research Triangle
                     Park, NC, to announce key findings of
                     the research project that is fully docu-
                     mented in a separate report of the same
                     title (see Project Report ordering
                     information at back).
                     Introduction
                       Over 100 x 10'
                     wastewater is discharged annually in the
gal. (3.8 x 10s m3) of
U.S. from the finishing of textile products.
An estimated  80% of textile finishing
mills discharge their wastewater to
publicly owned treatment works (POTWs).
Most of this wastewater receives either
no treatment or only primary treatment
(e.g., settling, screening, equalization, or
neutralization)  before being discharged to
municipal sewers.
  Major textile  finishing operations
include fiber preparation (desizing,
scouring, mercerizing,  bleaching), fiber
coloring (dyeing, printing), and functional
finishing. Wastewater  results primarily
from preparation  and coloring.
  Many wastewater recycle/reuse tech-
nologies, allowing reuse of these waste-
waters, are described in detail in an ear-
lier report. One  of these  technologies,
dyebath reconstitution and reuse, ap-
pears to offer  significant environmental
benefits  and substantial cost savings to
the industry, and also has the potential
for widespread use within the industry.
This report investigates dyebath reconsti-
tution and reuse  in detail.

Textile Dyeing
  The vast majority of textile products are
colored by dyeing. In 1980, about 7.8 x
109 Ib (3.5 x 109  kg) of fibers were dyed.
For this dyeing, 171 x 106 lb(7.8x 10* kg)
ofdyestuffsand1.28x109lb(5.8x108kg)
of additives (auxiliary  chemicals) were
used. Most  auxiliary chemicals do not
exhaust during  dyeing and are thus
discharged with the dyeing wastewater.
Dyestuffs, however, generally exhaust to
over 90% during dyeing. The often quoted
value for average dyestuff  exhaustion
during dyeing  is  95%. Assuming a 95%
exhaustion rate  for the  dyestuffs still
leaves about 8.5 x 106 Ib (3.9 x 106 kg) of
dyestuffs discharged annually in dyeing
wastewater.

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  Dyeing can involve either continuous
or batch operations. About half of the
textile fibers dyed in the U.S. are batch
dyed. Certain products (e.g., knit fabrics,
hosiery, and yarn) are almost exclusively
dyed  using  batch processes.  Large
amounts of  carpet and some woven
fabrics are also batch dyed. Batch dyeing
remains popular due to its flexibility,
short-run capability, and ease of control.
Batch processes, however, are generally
inefficient in their use of water and auxil-
iary chemicals.
  In typical batch dyeing, 1 -5 gal. (0.004-
0.02 m3) of water is used as dye liquor for
each  pound  (0.45 kg) of fiber dyed.
Auxiliary chemicals and dyes are added to
this dye liquor. Auxiliary chemicals can
include  exhaust agents, leveling agents,
buffers, pH control chemicals,  retarding
agents,  wetting  and dispersing agents,
carriers, softeners,  lubricants, and pene-
trants.  The total amount of  auxiliary
chemicals added will vary depending on
the fiber and dyestuff  types, but will
generally range from a few percent of the
fiber weight (2 or 3% o.w.f—of weight of
fiber)  to as  much  as  50% where high
concentrations of exhaust agents are
required. Dyestuff quantities are generally
a few (less than 4) percent of the fiber
weight. After adding auxiliary chemicals
and dyes, the dyebath  temperature is
raised to (and held  at) the desired dyeing
temperature until dyeing is complete and
a level dyeing is achieved. The exhausted
dyebath, now containing  only a few
percent of the original quantity of dyestuff
but still most of the auxiliary chemicals, is
dropped, and the dyed product is rinsed
with fresh water.

Dyebath  Reuse
  The exhausted dyebath may be used for
subsequent dyeings, thus using  the
auxiliary chemicals for  more  than one
cycle of dyeing. This results in production
cost savings and  also decreases  the
volume of  wastewater and  quantity of
pollutants discharged. To reuse  the
dyebath, a  method  was needed for
analyzing  the exhausted dyebath to
determine  the quantities of  dyestuffs
remaining and thereby the quantities to
add for the next  dyeing.
  Much of  the development  of  the
dyebath analytical techniques and recon-
stitution methods was performed at the
School of  Textile  Engineering at  the
Georgia Institute of Technology in  the
1970s. The success of this development-
al work led to several full-scale demon-
strations, also by Georgia Tech.
  The  work  under Phase III  of EPA's
Textile  Wastewater Recycle/Reuse pro-
ject expands on earlier work on dyebath
reconstitution and reuse:
 1. It examines the application of dyebath
    reuse at a mill that is fairly typical of
    many dyehouses, yet is not a "per-
    fect" candidate for this technology.
    • Dye formulations had to be modi-
      fied to use a smaller number of
    •  dyestuffs before reconstitution
      became technically feasible.
    • Quality  control  requirements are
      strict at this mill, thus posing a stiff
      test of the ability of dyebath reuse
      to produce acceptable dyeings.
    • Overflow rinsing is typically used
      at this mill, thereby affecting not
      only the dyebath analysis/recon-
      stitution methods,  but  also the
      economics of dyebath reuse.
 2. It presents a detailed examination of
    the techniques used not only in full-
    scale testing but also in the develop-
    ment and testing of the technology at
    this mill. These techniques can be
    directly applied by other mills wish-
    ing to examine  the  feasibility of
    dyebath reuse.
 3. It presents the first development of
    environmental  data for  this  waste-
    water recycle/reuse technology.
    Thus, the  environmental benefits of
    dyebath reuse can be  quantified for
    the first time.
 4. It  updates the equipment used in
    dyebath analysis to include a modern
    desktop computer, a  commercially
    available interface for the spectro-
    photometer/computer, and software
    written in  the  BASIC computer
    language to allow for greater  com-
    prehension and  adaptability to a
    variety of desktop computers.
  Volume 1  of  this  report details the
results of a  study  of  dyebath  reuse
implementation at a carpet mill. Volume 2
is  a dyebath reuse operations manual,
providing information  on the technology
to mills interested in adopting dyebath
reuse.


Dyebath Reuse Studies

  To  develop  information on  full-scale
implementation and costs  of dyebath re-
constitution and reuse, a demonstration
of the technology was performed at a
carpet mill, Mill C-2 of earlier studies. Mill
C-2 performs  atmospheric batch dyeing
primarily of nylon carpet, discharging
about 1 x 106  gal./day of wastewater to
the municipal  collection system.
  Two popular, large-volume carpet styles
were selected for dyeing using dyebath
reuse procedures. The dye recipes for
these styles had recently been reformu-
lated to utilize a small number of dyestuffs.
Many of the different shades now have
recipes  containing  varying amounts of
the same three dyestuffs. This is an
essential step in implementing dyebath
reuse since the residual dyes in the dye-
bath from the just completed dyeing must
be the same ones that are to be used in
dyeing the next shade.
  The dyebath was analyzed using a visi-
ble-light spectrophotometer. Dyestuff ab-
sorbance coefficients were determined in
the laboratory for  each dyestuff. These
coefficients are the k-values in the Lam-
bert-Beer equation:
               A = kC
 where A - absorbance of the dyestuff,
 and C  = concentration of the dyestuff.
These values were then used to analyze
exhausted  dyebaths  to determine  the
amounts of dyestuffs that remained at the
end of a dyeing. A desktop computer was
programmed  to perform all the calcula-
tions needed to determine how much dye
remained in  a used  dyebath  and how
much had to be added to perform the next
dyeing.  In this way, the actual procedures
needed  to reuse a dyebath could be carried
out in only a few  minutes by dyehouse
personnel.
  Twenty-six series of dyeings were per-
formed with  dyebath  reuse, each series
consisting of 5-10 dyeings using the same
dyebath.
  The first 15  series (bench-scale dye-
ings) provided  opportunities to become
familiar with dyebath reuse concepts and
procedures, to test the shade-matching
capability of dyebath reuse, and to resolve
problems while still on a small scale. Six
shades from each of the two carpet styles
were selected for dyeing. For each shade,
the dyebath was reused until a  series  of
five dyeings was completed. This accounted
for the first  12 series. The final three
bench-scale  series each started with a
light shade and gradually progressed  to
darker shades as the dyebath was reused.
The dyed carpet samples from these bench-
scale dyeings were analyzed with a Diano/
Hardy II spectrophotometer to  evaluate
the  ability  of dyebath reuse to produce
acceptable shade matches. Results were
very good.
   Following  the success  of the bench-
scale dyeings,  eight  additional dyebath
reuse series  were conducted using a
pilot-scale  beck(vat). The pilot-scale beck
and dyeing procedures more closely re-
semble full-scale dyeing than bench-scale
dyeing. Thus, the pilot-scale dyeing would
provide an  opportunity to test dyebath
reuse under conditions that approximate
full-scale dyeing, and resolve any prob-

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 ems. Both single- and multi-shade series
 were dyed for each  carpet style. The
 ihade matching, levelness, and color fast-
 ness results (primary measures of product
 quality) of the dyed samples were very
 jood.
  The final three series were full-scale
 dyeings conducted in a 6,000-gal. (22,700-1)
 atmospheric beck. The first series had
 o be aborted after three dyeings due to
 an unexpected yarn lot change. The re-
 naming two series were  multi-shade
 Jyeing  series  consisting of 6  and 10
 Jyeings, respectively. The process was
 nonitored carefully to calculate  the sav-
 ngs in water, energy, dye, and chemical
 jse due to dyebath reuse. Shades were
 natched successfully in all dyeings. The
 :arpets produced were of  first quality.
 3oth the number of adds and redyes were
 vithin the mill's typical  frequency for
 hese styles. Thus, the full-scale experi-
 nents demonstrated  that  the  ease  of
 )btaining satisfactory dyeings with re-
 :onstituted baths was comparable, if not
 superior, to that of conventional dyeing.

 Environmental Benefits
  Wastewater samples  were collected
 luring both the pilot- and full-scale dye-
 ngs. Results of the full-scale data (below)
 :haracterize the potential environmental
 senefits of dyebath reuse:
                  Percent Reduction
                     in Discharge
 3ollutant         Series 25 Series 26
:low (gal./lb)
BOD
:OD
rss
TDS
'henolics
Total-P
24
13
32
47
25
0
28
34
33
33
0
43
0
44
The concentrations of various pollutants
in the dyebath increased as the dyebath
was reused. This is suspected to be due to
the buildup of yarn finishes that  are
removed from  the carpet during dyeing.
Despite these higher concentrations, the
net effect of dyebath reuse is to  reduce
the mass of pollutants actually discharged,
as compared to conventional dyeing. The
lack  of suspended  solids reduction in
Series  26 is an exception to this observa-
tion that cannot be explained. This  net
reduction is due to the smaller amounts
of auxiliary dyeing chemicals needed to
perform reuse  dyeings.
  The  larger reductions in wastewater
volume and pollutant discharge in Series
26, as compared to Series 25, were due to
attempts to reduce the volume of over-
flow cooling water used in the dye cycle.
Less cooling water results in less dilution
of the dy.ebath. Consequently, smaller
amounts of auxiliary chemicals are needed
to reconstitute the dyebath for reuse. This
results in both  wateruse/discharge and
pollutant discharge reductions. Further
optimization in this area will  result in
even greater environmental benefits.

Economic Analysis
  In general, dyebath reuse has favorable
economics due to its relatively low capital
cost and significant cost savings. Payback
periods of about 1 year are common for
this technology.
  An economic analysis was conducted
for dyebath reuse implementation at Mill
C-2. The  cost  savings due  to  dyebath
reuse were calculated  based  on  data
collected during the full-scale tests. The
calculated savings averaged $23.85 and
$28.60 per dye cycle for the two carpet
styles, or about $0.011 to $0.012/lb of
carpet. About 65% of these savings are
due to reduced auxiliary chemical require-
ments. Energy  savings account for an-
other 20%. Water and sewer use savings
account for  the remaining 15%. Future
optimization of  the reuse dyeing proce-
dure, by reducing the amount of overflow
cooling water used, could easily increase
the per-cycle cost savings to over $30.
  Operating costs for dyebath reuse are
relatively low. Yearly operating  costs of
$5,000  were  estimated for Mill  C-2,
based on 2,400 reuse dyeings per year.
This results in operating costs of about $2
per cycle.
  Capital costs for  equipping two  dye-
becks at Mill C-2 for dyebath reuse were
estimated to  be $70,500. This  cost
includes a pump, an elevated 6,000-gal.
(22,700-1) storage tank, piping, valves,
controls, and  analytical equipment
including  a spectrophotometer and a
computer.
  With  an allowance of  $10,000 for
developmental  costs, the net payback
period is calculated to be 1.5 years:
Capital Cost      $70,500
Development Cost   10,000
Total Capital      $80,500

Yearly Savings    $60,000
                 (based on $25/cycle)
Yearly O&M Costs   5,000
Net Savings      $55,000
Payback Period =
80,500 = 1.5 years
55,000
Outlook for Use in Industry
  As noted earlier, batch dyeing accounts
for  half of the total amount of textile
                      dyeing. Due to the higher water  and
                      chemical  usage of batch  dyeing, well
                      over half of the wastewater volume and
                      pollutant  loading  from dyeing results
                      from batch dyeing.
                        In certain industry sectors,  dyeing is
                      performed  almost  exclusively  by  batch
                      operations: mills in these sectors can be
                      regarded as potential users of dyebath
                      reuse technology. These sectors include
                      knit fabric,  hosiery, and yarn finishing. A
                      large amount of carpet  dyeing  is  still
                      performed  in batch operations, although
                      there is a trend toward producing more
                      continuous-dyed/printed carpeting. Most
                      large woven-fabric finishing mills employ
                      continuous dyeing, though some smaller
                      mills still  have significant batch dyeing
                      operations. Overall, many mills can
                      potentially adopt this recycle technology.
                        Dyebath reuse  has been  tested or
                      demonstrated with a  wide variety of
                      products and textile  fibers,  including
                      nylon hosiery and carpet; polyester fabric,
                      carpet, and yarn; acrylic yarn; and cotton
                      fabric.  Dyestuff classes that have been
                      tested or demonstrated include acid,
                      basic, direct, disperse, and reactive.
                        At many mills, not all production will be
                      amenable to dyeing  by dyebath reuse.
                      However, eve.n the conversion of  a few
                      machines to this recycle technology will
                      have substantial cost and environmental
                      benefits. A mill that is ideally  suited to
                      employ dyebath reuse technology will
                      generally dedicate only half of its  dye
                      machines  to reuse dyeing, to ensure
                      maintenance of flexibility  in production.
                        The major obstacle to further use of this
                      technology appears to be the lack of
                      detailed information on evaluating and
                      implementing the technology. Volume 2
                      is an operations manual that should fill
                      this gap.
Operations Manual
  The operations manual (Volume 2) first
introduces the reader to the concepts and
procedures  of  dyebath reuse. It  then
presents a  procedure  that  allows the
reader to determine if dyebath reuse is
applicable to his dyehouse. A preliminary
economic analysis can also be conducted.
  The next topic is the development of an
evaluation program.  Suggestions are
given on the content and scope of tests
necessary to evaluate the feasibility of
dyebath reuse.
  Subsequent sections  of the manual
introduce the concept of light absorbance
and how it is used to analyze dyebathsfor
their dyestuff content. The procedures for
analyzing and reconstituting dyebaths for
additional  dyeings are then presented.

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   Specifications for equipment and supplies
   are provided.
     The use  of  desktop computers  to
   perform  the calculations  for dyebath
   reuse is  discussed. Equipment is listed,
   and a dyebath reuse computer program
   written in BASIC is provided.
     The final sections of the manual
   discuss laboratory and full-scale dyebath
   reuse experiments.  Troubleshooting
   guides are provided. Options and sugges-
   tions for full-scale design and implemen-
   tation of  dyebath reuse are given.
     The manual provides enough informa-
   tion and guidance to assist textile mill
   operators who are interested  in evalua-
   ting or implementing this technology.
          J. Bergenthal and A. Tawa are with Sverdrup and Parcel and Associates, Inc.,
            St. Louis, MO 63101.
          Robert V. Hendriks is the EPA Project Officer (see below).
          The complete report consists of two volumes, entitled "Investigation of Textile
            Dyebath Reconstitution and Reuse:"
              "Volume 1. Technical Report," (Order No. PB 84-206 465; Cost: $16.00)
              "Volume 2. Operational Manual," (Order No. PB 84-206 473; Cost: $ 16.0O)
          The above reports will be available only from: (cost subject to change)
                  National Technical Information Service
                  5285 Port Royal Road
                  Springfield, VA 22161
                  Telephone: 703-487-4650
          The EPA Project Officer can be contacted at:
                  Industrial Environmental Research Laboratory
                  U.S. Environmental Protection Agency
                  Research Triangle Park, NC 27711
                                                                                  US GOVERNMENT PRINTING OFFICE. 1984—759-015/7753
United States
Environmental Protection
Agency
Center for Environmental Research
Information
Cincinnati OH 45268
Official Business
Penalty for Private Use $300
              CHICAGO  1L  60604

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