United States
 Environmental Protection
 Agency
Industrial Environmental Research
Laboratory
Research Triangle Park NC 27711
 Research and Development
EPA-600/S2-80-209  July 1981
Project  Summary
Textile  Warp Size  Reclamation
Using  Thermal  Precipitation
W. S. Perkins, R. P. Walker, and L J. Hirth
  The report describes a novel method
for reclaiming size based on precipita-
tion of the size material by heating the
desize washwater. The method uses
hydroxypropyl  cellulose  (HPC)  or
hydroxypropyl  methylcellulose
(HPMC) which are soluble in cool
water but  insoluble in warm water.
Reclaiming size would eliminate most
of the  BOD  typically resulting from
sizing and  desizing. Since maximum
system  temperature with HPC  is
about 50°C, compared to 95°C for a
conventional system,  considerable
energy  is  conserved.  Strength and
elongation  of yarns sized with virgin
HPC and with reclaimed HPC were not
significantly different from those of
yarns sized with the conventional size,
polyvinyl alcohol (PVA),  at  similar
add-on  levels. Abrasion resistance of
yarns sized with HPC was lower than
that of yarns sized with PVA at similar
add-on levels. Weaving of  HPC-sized
50/50  polyester/cotton yarns in the
laboratory was successful. In produc-
tion weaving of percale sheeting, HPC
accumulated on  the shuttle caused
poor weaving efficiency. The capital
investment for reclaiming HPC using
thermal  precipitation is much lower
than for reclaiming PVA using ultra-
filtration. Operating costs for recover-
ing HPC by thermal precipitation and
for recovering PVA by ultrafiltration
represent a savings over conventional
sizing and desizing without reclaiming
size.
  This Project Summary was develop-
ed by EPA's Industrial Environmental
Research Laboratory,  Research Tri-
angle Park, NC, to announce key find-
ings of the research project that is fully
documented in a separate report of the
same title (see Project Report ordering
information at back).
Introduction
  Virtually all textile yarns which are to
be woven into the lengthwise direction
(warp) in a  fabric are coated  with a
protective material, called size, during
the slashing process. The purpose of
this size  is to improve the performance
of the yarn in the weaving process. In
most cases the size material is removed
from the woven fabric in the finishing
plant. Published data indicate that 45%
to 75% of the BOD load from a woven
fabrics finishing plant results from this
warp size which is removed from the
fabric.
  A process to recover and recycle the
warp size used in textile processes has
the potential to lower the BOD and COD
of textile finishing plant effluents more
than any other single change in textile
processing. Such a process has been
the objective of much  development
work in recent years. The following are
specific examples of approaches to size
recovery  and recycle:

 (1)  Recovery of carboxymethyl cellu-
     lose by  chemical  precipitation
     from the desize wastewater has
     been studied but not commercial-
     ized.

 (2)  Recovery of polyvinyl (PVA) by
     chemical precipitation has also
     been subject to investigation.

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 (3)  Studies of recovery of warp size
     via  solvent sizing  and desizing
     have been made. A solvent sizing
     and solvent desizing system has
     been  developed by two Italian
     machinery companies.

 (4)  Recovery  of   polyvinyl  alcohol
     (PVA)by ultrafiltration  of the de-
     size wastewater has been subject
     to considerable development, and
     commercial processes have now
     been operating for  several years.

  The tremendous  interest of the U.S.
textile industry in recycle of warp size is
understandable since  the  economic
outlook for such a  development is as
favorable  as are  the environmental
considerations. The size material adds
no value to the product (fabric), since it
is normally removed in desizing  and
disposed  of in a wastewater treatment
facility. Therefore, the size material it-
self adds to the cost of fabric production.
A process for recovery and reuse of size
material  may  prove profitable  to the
textile  mill through reduced  fabric
production cost if  a high  degree  of
recovery of the size material is obtained.
  Therefore, a size reclamation process
offers  the potential for  a modification
from which the mill may realize a direct
return  on  investment. This approach
should be considerably more attractive
to management than the prospect  of
construction  of additional  treatment
facilities which may become obsolete as
the 1983 Effluent Guidelines are imple-
 mented.  Further,  size  recycling will
allow the industry room for expansion
 and growth without great capital invest-
 ment  for  wastewater  treatment
facilities  since recovery and recycle of
warp  sizes will   allow increases  in
 production without large increases in
effluent loads.
  The  size reclamation system which is
the subject of this report uses a size
 material   selected  from a  group  of
 polymers having the unusual property
 of  being soluble   in water  at room
 temperature  but  insoluble at  some
 higher  temperature.  Hydroxypropyl-
 cellulose (HPC) is such a polymer. HPC
 is soluble in  water  at temperatures
 below 43°C  (109°F)  but  becomes
 almost completely  insoluble in water at
 temperatures   above  45°C  (113°F).
 Hydroxypropylmethylcellulose  (HPMC)
 also exhibits this  "reverse  solubility"
 property  but at a  higher precipitation
 temperature than  is required for HPC.
 Most of  the work  done in this  project
was concerned with HPC rather than
HPMC and  except where otherwise
specified the discussions pertain to HPC
rather than HPMC.
  Precipitation of HPC or HPMC from
desize wastewater can be accomplished
by heating the desize wastewater.  A
schematic diagram of the desizing and
recovery system  is shown in Figure  1.
Application of the  size material to the
warp yarn in slashing and washing  of
the size material  from the woven fabric
in desizing  is done with water at a
temperature {lower  than 43°C.  The
desize washwater containing HPC at a
concentration of  0.5 to 1.5% by weight
is filtered to remove insoluble impurities
and heated to above 45°C to precipitate
the HPC. The precipitated HPC is then
separated from most of the water. The
HPC redissolves when cooled to yield a
solution concentrated enough to reuse
in slashing. The recovered water can be
cooled to below 43°C and reused in the
desize washer.
  This report describes both laboratory
and  in-plant work  concerned with the
development of a process utilizing HPC
as the warp size with the objective  of
reclaiming the HPC using the thermal
precipitation principle. Work was  per-
formed in the following areas:
       Fabric in
              (1)   Utility and performance of HPC as\
                   a textile warp size.

              (2)   Design and operation of a thermal
                   precipitation  size   reclamation
                   system.

              (3)   Economics of size reclamation by
                   thermal precipitation.

             Conclusions
               Hydroxypropylcellulose (HPC)  is
             soluble  in water at room temperature
             but becomes virtually insoluble in water
             at a  temperature  greater than about
             43°C. HPC can be precipitated from
             water by heating the water to above the
             precipitation temperature. The HPC can
             then  be separated from  most of the
             water by settling, filtration, or centrifu-
             gation. Therefore, a dilute solution such
             as is obtainable in a conventional desize
             washer can  be  concentrated  to  the
             extent required for use of the material in
             a conventional slashing process. More
             than 90% of the HPC in a 1.0% solution
             of desize washwater can be obtained at
             up  to 25% concentration in the re-
             claimed  solution   using  a  recovery
             system  based on settling of the HPC in
             warm water. Hydroxypropylmethylcel-|
             lulose (HPMC) also exhibitsthistherman
                      Fabric out
       Desize Washwaste
          11.0% size)
   Desize
water at 40°C
Reclaimed Water
 Filter for
 fiber and
 \insoluble
 impurities]
                                                                      Fresh
                                                                      Water
                   \fapprox. 10%
                    of total)
                                  Cooling
                                     of
                                 reclaimed}
                                   water
                     Heats to
                       45°C
              Water/
               Size
            Separator
      Reclaimed
                                                     Water
                                               Concentrated
                                              size to slasher
                                                 (8 - 10%)
Figure  1.    Schematic of desize and recovery system.

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 precipitation phenomenon, but at about
 65°C.
  Textile  yarns  consisting of  100%
 cotton or 50% polyester and 50% cotton
 can be sized with HPC  or HPMC. The
 physical properties of yarns sized with
 HPC  or  HPMC  are adequate for  the
 yarns to be woven  into fabric. The
 tensile strength of yarn sized with HPC
 is appreciably higher than that of un-
 sized yarn and is not significantly differ-
 ent from the tensile strength  of yarns
 sized  with  the   conventional  size,
 polyvinyl alcohol (PVA), at the same size
 add-on.  The  abrasion  resistence  of
 yarns sized with  HPC is higher than
 that of unsized yarns. The magnitude of
 the improvement in abrasion resistance
 depends on the size add-on level. The
 abrasion resistance of yarns sized with
 PVA  is higher than that of yarns sized
 with  HPC at the same add-on  level.
  Clear flexible films are formed upon
 evaporation of the water from  aqueous
 solutions of HPC. Clear films  are pro-
 duced even when  the temperature is
 higher than that which causes the HPC
 to precipitate from water.  The  strength
 of HPC films is similar to that of conven-
 tional sizes such as starch and  carboxy-
 methylcellulose. The elongation of films
 of HPC is intermediate between that of
 conventional size, starch,  and  PVA.
  Yarns sized with HPC can be woven
 into  fabric.  On  50-inch  wide  looms
 weaving at 215 filling  insertions per
 minute, the contact of the shuttle with
 the yarn results in an accumulation of
 HPC on the shuttle. The accumulation of
 HPC  on the shuttle is undesirable be-
 cause it eventually interferes  with the
 passage of the shuttle into the yarn shed
 causing excessive yarn breaks  near the
 sides of the loom. The accumulated size
 material   may  also be  periodically
 stripped away  from  the  shuttle  and
 become woven into the fabric causing a
 fabric defect. This accumulation of HPC
 on the shuttle does not occur  to a dis-
 ruptive degree on 24-inch looms weav-
 ing at 175 filling insertions per minute.
 Whether this accumulation of size on
 the shuttle also occurs with HPMC on
 50-inch  looms is not known,  but the
 accumulation of HPMC does not occur
 to a disruptive degree on 24-inch looms
 weaving at 175 filling  insertions per
 minute.
  HPC reclaimed from woven fabric has
 tensile strength and  elongation  not
 appreciably different from that of virgin
 HPC. Yarns sized with reclaimed HPC
 have abrasion  resistance not  appreci-
 ably different from that of similar yarns
sized with virgin HPC. Pure HPC may be
more flexible than is desirable in a size
material. HPC softens dramatically at
high relative humidity,  and its  effec-
tiveness as a warp size deteriorates.
  Fabrics containing HPC can be rapidly
desized using room-temperature water.
The rate of removal of HPC from a poly-
ester/cotton fabric is  as rapid at 25°C
(77°F)  as the removal of PVA at 95°C
(203°F). Water used for desizing and
subsequently separated from the HPC in
the recovery system is suitable for reuse
in desizing. The content of impurities in
desize  washwater increases with each
reuse  cycle.  A steady  state  level  of
impurities is reached if a fraction of the
desize washwater is discharged at each
cycle.
  Thermally precipitated HPC particles
have a  negative zeta potential in water.
Consequently, coagulation and settling
of HPC  particles is enhanced by addition
of cations such as  Ca+*  or Al+++. The
addition of cations  does not have an
appreciable effecton the settling rate of
particles   of  thermally  precipitated
HPMC.
  Virgin HPC is resistant to biodegrada-
tion and solutions can be stored for long
periods. Reclaimed  HPC  solutions  are
subject to  biodegradation because  of
the  presence  of natural  impurities
removed  from  the fabric.  Reclaimed
HPC solutions can  be preserved with
agents typically used for preservation of
textile chemicals.  HPC is stable for long
periods at the temperature necessary
for its reclamation.
  The  capital investment for  reclama-
tion of HPC by thermal precipitation is
about one-third of that for reclamation
of polyvinyl alcohol by ultrafiltration.
The  operating costs  including size
material costs for a system based on
reclamation of HPC by thermal precipi-
tation  is  slightly  higher than  for  a
system based on reclamation by PVA by
ultrafiltration. The payback period for a
thermal precipitation  system  is  about
one-third  of that for  an  ultrafiltration
system. Because of the value of the re-
claimed  material,  size  reclamation
systems based on thermal precipitation
and ultrafiltration both operate at lower
costs  than  a  conventional   desizing
system not involving size reclamation.
  A  desize  and  reclamation system
using  HPC  operates  at a maximum
water  temperature  of  about  50°C
whereas a system using PVA operates
at a temperature of about 95°C. The
result  is  an  energy savings  of  about
0.655 x 106 Btu  per 100 Ib. of fabric
desized.


Recommendations
  Size reclamation is  an economical
approach to chemical and water  con-
servation and will reduce the pollution
load from most woven fabrics finishing
plants. The size reclamation  technique
that is most applicable to a  particular
mill must be selected based  on factors
peculiar to that mill. A critical compari-
son of all size reclamation techniques is
not presently available, but  such  a
comparison   would   be  useful   for
decision makers in the textile industry.
  Size reclamation using thermal pre-
cipitation appears to be technically and
economically feasible at present only for
selected types of plants. Those plants
weaving cotton or polyester/cotton on
narrow looms can probably use hydrox-
ypropylcellulose as the warp size. This
size can be recovered by thermal precip-
itation and reused for sizing. HPC may
also be useful in shuttleless weaving.
The possibility of using HPC as a size in
be useful  in shuttleless weaving. The
possibility of using HPC as a size in
machines using projectile, rapier and air
jet filling insertion mechanisms should
be investigated. HPC is not recommend-
ed for weaving of 50-inch wide fabrics
at a speed of 215 picks per minute using
shuttle looms at the current stage in its
development as a warp size.
  The greatest deficiency of HPC  as a
warp  size is insufficient hardness. The
possibility of chemical modification of
the material  to  make this property
suitable for warp sizing purposes should
be investigated. This work would best be
done  by a  chemical company experi-
enced in  evaluation  of  polymers for
warp  sizing.
  HPC accumulates  on the shuttle
during the weaving of 50-inch wide
fabrics if the shuttle is made  of wood or
of laminated cotton fabric  composite
materials. Shuttles made of other mate-
rials should be tested to determine if the
accumulation  of  HPC  occurs.
  Hot melt sizmg  is a developing tech-
nology for the textile  industry.  The
process applies a molten size to the yarn
and uses no water. The first production
model hot melt sizing machine will be
available in the near future. Since HPC
is a thermoplastic material its applica-
bility as a hot melt size should be inves-
tigated.  Conventional  recoverable size
materials such as  PVA and CMC are not
applicable bythe hot melttechnique and
* U.8. OOVEBHMEHIPRIKTIHO OFFICE «61 -757-012/72Z8

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    size   materials  which   have  been
    developed especially for hot melt sizing
    are  not  recoverable.  Therefore, the
    availability of the recoverable hot melt
    size would be highly desirable.
           Warren S. Perkins. Robert P. Walker, and Leo J. Hirth are with Auburn University,
             Auburn, AL 36830.
           Max Samfield is the EPA Project Officer (see below).
           The complete report, entitled "Textile Warp Size Reclamation Using Thermal
             Precipitation," (Order No. PB 81-129 041; Cost: $8.00, subject to change) will
             be available only from:
                  National Technical Information Service
                  5285 Port Royal Road
                  Springfield, VA  22161
                  Telephone: 703-487-4650
           The EPA Project Officer can be contacted at:
                  Industrial Environmental Research Laboratory
                  U.S. Environmental Protection Agency
                  Research Triangle Park, NC 27711
                   f
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