Note: Descriptions are shown in the official language in which they were submitted.
~ W095/35363 2 1 9 2 9 4 7 r~ 78
METHOD OF CREATING A 6TONEWASHED APPEARANCE IN WET-PROCESSED FAERICS.
,
The invention relates to methods for producing a
stonewashed effect in fabrics and garments while reducing
redeposition of dye on the treated materials.
Wet-processing of fabrics and garments to produce a
variety of visual effects enhancing the appeal of the treated
materials is a well known practice. This practice is
particularly popular when the garments are indigo dyed and/or the
garments are constructed from denim fabric, as with jeans,
jackets, skirts, etc., as well as certain avv~ssoLies and various
non-garment items similarly constructed.
Of the more popular wet-processing ~LvceduL~s, abrasion
of indigo dyed garments or "stonewashing" has become commercially
widespread. For purposes of clarity, and to be consistent with
industry terminology, "st~n?w-~hing" is considered a process
whereby color is removed from a cellulosic garment or fabric by
the -- -n;nAl abrasion of pumice stcnes or other abrasive
materials, usually in a water bath in a tumbler or washer, such
that localized abrasion creates lighter spots or areas on the
surface of said fabric or garment leaving a relatively untouched
background. Further, pLocesses which produce a similar
appearance to said abraded fabric or ~L ts by chemical or
enzymatic means, or combinations of the above with or without
AnicAl abrasion, are included in the definition of
stonewashing as it is accepted in the industry.
The most common class of enzyme used to impart the
modified appearance is cellulase. C~ lAce enzymes are
W095/35363 2 1 92q47 P~ 78
typically divided into two groups: tho8e with greatest activity
at a neutral pH range (pH about 6 to 8), and those with greatest
activity in the acid pH range (pH about 4 to 6). These ranges
Le~. ~s~l~L the pH values of optimum performance, even though each
type of enzyme has some activity outside it_ stated pH range.
Both types are commonly used to impart the "stonewashed"
appearance and both have advantages and disadvantages.
One of the advantages of the neutral cellulase
LLe~ i5 that only a moderate amount of indigo dye removed
during the washing process is redeposited onto the white portions
of the fabric, thus producing stnnowqchPd denim garments that
have bright, clean appearing highlighted areas. The major
disadvantage is that, typically, a neutral cellulase enzyme will
react somewhat slower than an acid ~P~ lAce enzyme, thus
lengthening processing times.
A major ~dvantage of the acid cellulase treatments is
that the reaction on fabric is much faster than a neutral
cellulase enzyme. A reaction time of two to five times faster
than a similar treatment with a neutral rP~ lAce enzyme is not
, r,. The major di~dv~ y~ is that a greater amount of dye
is redeposited onto the garments due in part to the lower
solubility of indigo at the lower pH.
Methods and compositions for chemically stonewashing
fabrics or garments generally are set forth in, for example, U.S.
Patent Nos. 4,832,864, 4,912,056, 5,006,126 and 5,122,159.
Improved compositions and techniques are required, however, for
processing dyed material with fast-acting acid cPllnlAce enzyme
LL~al Ls while reducing the quantity of redeposited dye, thus
~ W095/35363 2 1 92947 ~I/U~ '78
rapidly yielding garments with areas of bright, clean contrast
and an attractive stonewashed appearance.
It is the object of the present invention to provide
a method of wet-processing dyed cellulosic fabrics and garments
to chemically create a stonewashed appearance in a rapid and
effective manner.
It is a further object of the present invention to
provide a method as aforesaid which yields fabrics and garments
having bright and clean appearing highlighted areas of color
variation where dye has been removed.
It is yet a further object of the present invention to
provide a method as aforesaid wherein fast-acting acid cellulase
enzymes can be utilized as the principal dye-removing agents and
yet redeposition of dye on the treated material is substantially
avoided.
Still another object of the present invention is to
provide a method as aforesaid which is particularly well-adapted
for processing indigo dyed denim fabrics or garments.
In keeping with these objects and others which will
become apparent hereinafter, the present invention resides in an
improved method for treating dyed fabric, either in unsewn form
or in the form of a garment, to produce a sfon~ ~h~d effect by
treating said fabric with a water-based composition having an
acidic pH and including at least one acid cellulase enzyme and
a dye redeposition inhibiting additive selected from the group
~ consisting of natural and synthetic inorganic silicates,
polyalkylene oxide polymers, acrylic polymers (homopolymers and
copolymers) and natural, synthetic and semisynthetic
W095/35363 2 ~ 929~7 ~ 78
polysaccharides, in~ ing natural and synthetic gums. The novel
method utilizing the foregoing additives enables the use of fast-
acting acid cP~ ace enzymes to remove dye and cause the desired
loc~li7ed variations in color density while substantially
preventing "backstaining", the redeposition of dye (particularly
indigo dye) from the low pH wash water onto the treated fabric.
The improved wet ~Loc~Ccing method of the invention
involves contacting dyed cellulosic fabrics, principally cotton
denim fabrics, with an aqueous or water-based solution containing
(a) a cellulase enzyme having greatest activity in the acid pH
rnnge, and (b) a dye redeposition inhibiting additive, as well
as optionally other conventional additives such as buffers,
surfactants, enzyme activators, 501nhil i7ing agents and the like.
The fabric is tumbled or agitated together with the aqueous
solution.
The fabric treated in accordance with the invention may
be in unsewn form or sewn in the form of a garment or other
article ~ of sewn fabric, preferably a new (unworn)
garment or article
The term "stonewashed appearance" as u5ed herein refers
to an appearance including local areas of variation in color
density on the surface of dyed c~ sic fabrics, resembling the
appearance created by mechanical abrasion of the fabric with
pumice or other "stones".
Stonewashing is normally carried out in commercial
washing ~-~h;n~c, cylindrical tumblers, converted dryers or
similar pieces of equipment. The ne~s~ry parameters for
practice of the subject method are that there must be a means to
~ WO95/35363 2 I 9 2 q 4 7 . ~./~ ' . 78
contain the wash liquor during the process, along with the
garments, fabric, or items being stzr qhe~, such that they and
the enzymes and other processing chemicals can make constant or
intermittent contact. Further, there must be a means of
introducing mechanical energy into the system, allowing the
surfaces of the items to be stonewashed to rub against other
surfaces, including other fabrics or items being stonewashed.
This, in the case of a washing machine or tumbler, is
accomplished by rotating the cylinder containing the garments,
etc. at such a speed as to allow the garments to move about
inside and rub against each other. In the case of a paddle dye
machine, this i6 accomplished by an external paddle wheel mounted
at or near the surface of the process li~uor. The paddle turns
and creates a circulating current. The current and/or the paddle
catches the garments and forces them along in such a way as to
rub over other y~L Ls and the paddle, creating the nP~c~ry
mechanical action on the goods.
The stonewash process typically consists of several
*steps, rather than a single exposure to cellulase enzyme and/or
pumice stones. The garments are first typically desized using
ta) amylase enzymes and a~Lfa~L~I-Lc, (b) oxidizers, alkalis, and
surfactants, (c) solvents and surfactants or (d) hot water. This
is fL~~~IlLly, but not n~c~cF~rily, followed by one or more
rinses. The abrasion step normally follows, where the cellulase
enzyme and other auxiliary ~h~mio~lc are used to create the
abraded appearance. This is the step during which the dye
redeposition ~Le~.lLing additives would normally be present
according to the invention. Following abrasion there is
21 92947
W095135363 PCT~S95/06S78
sometimes a bleach step (only if the overall color is to be
lightened), an antichlor step (only if a bleach step is used),
a clean-up step where detergents and brighteners are frequently
added to wash away exces6 1006e dye, one or more rinse6, and a
final softener application. Subsequently, the garments are
extracted to remove excess water, then dried and pressed.
~lthough the preferred point to introduce the additives to
prevent dye redeposition is with the cellulase enzyme, the
additives may provide some benefit if added to the desize
operation, the rinses before or ~fter the abrasion, in the clean-
up step, or in multiple steps.
While indigo dye is by far the most common dye used on
~t ~h~ fabrics and garments, the s~-r -h concept applies
to any fabric, garment, or article which is made from cellulosic
fibers, yarns, or threads, in whole or in part, and is dyed,
pigmented, or otherwise colored in such a way as to have a
differential of color between the surface and the center of said
fibers, threads or yarns, whether the colorant is a vat dye (such
as indigo), a pigment (or pigment dye), a sulfur dye, or another
classification of dyestuff. The key concept is that the fibers
or yarns are "ring dyed", named for the resulting appearance of
~ ~ ~ e~Lion of the dyed fi~er, being more heavily dyed on the
outermost ring of the fiber, less heavily dyed tor not dyed at
all) at the center core. The stonewashing process damages the
out ~ portion of the cellulosic fibers, ~Ypos;nq the undyed
(or lighter-dyed) centers of the fibers.
The dye redeposition or backstaining preventing
additives to be used in the novel methods are selected from the
group consisting of natural and synthetic inorganic silicates,
~ W095/35363 - 2 1 9 2 9 4 7 P~ . 78
such as zeoliteG, kaolin and bentonite clays; polyalkylene oxide
polymers, ;nr~ ;ng polyalkylene oxide polyamine copolymers;
acrylic homopolymers and copolymers; and natural, synthetic and
semisynthetic polysaccharides, such as natural and synthetic gums
and cellulosic polymers.
Representative generic ~LLU~ULeS for several
categories of dye redeposition preventing additives to be used
in the methods of the invention include but are not limited to,
the following:
Na~nral/Synthetic Innr~An;c Silicates
Al20~45iO2-H20, R+n(Al~Mg)nsi~O~o(OH~nH20 n20
H2Al2Si208-H20
Na20Al203(5iO2) (HzO)y
[Al2034SiO2H20]R' where R is an organo group.
Polyalkyl~nen~ide Polym~
PolyAm; nnethnxylates
H- (OCH2CH2) y~ (OCHCH3CH2) ~ (CH2CH3CHO) ~- (CH2CH20) y
NCH2CH2N
H-(OCH2CH2)y~(0CHCH CH2)~ (cH2cH3cHo)~-(cH2cH2o)y
Polye~hyl~n~ Ox;de Polymers
~ ( CH2CH20 ) ~n
Polyet~ylene Glycol Poly
HO(CH2CH20)nN
21 92947
W0~13~363 P~~ 7
Polysacch~ride Polymers
Methylcellulose
Cl H5 H b i H,C H
~\ J~ CH H
/~_H / ~ \ /~ //
CH,~ _ _ n-2CH,
~d,oxy~l~v~l~et~ylcellulose
~CH, ~ n O ~ H
~ ~o HO;~ ~ ~f OH
HO CH HO- H ~~~~
CH C}ICH,\ /CH3CHCH. H H O
bH ~' - ~ CH; ~ n-2 CH,
~ WO 9S/3S363 2 1 q 2 't 4 7 P~l/u........ -~78
~ nt.h ~ n Gl lm
CH,OH CH,OH
~'
Cl~,OCCH, OH
H
CooclMc)
'MC~_X~, K, :~C~
COO MX O CH. o/~
CH
W095l35363 2 1 9 2 9 4 7 . ~ 9 . --~8
Acrylic Homo~olymers an~ Copolymers
[(CH2CH)n] where molecular weight
i5 2 ~iO,OOO.
C=O
OH
[ (CHzCH~ n] crosslinked w/polyalkenyl-
I polyether where molecular
C=O weight is 2 50,000.
OH
[(CH2CH)n]-[(CH2CH)n] where the ratios of ethyl
l l acrylate to acrylic acid are
C=o C=O variable and having a
l l molecular weight 2 50,000.
OH OCH2CH3
ICH3
[(CH2C)n]~[CH2CH)n] where the ratios of ethyl
I \ acrylate and methacrylic acid
C=O C=O are variable and molecular
l l weight 2 50,000.
OH OCH2CH3
The following are illu6trative examples of _
or materials identified by brand name, supplier and/or chemical
name or ~Llu~LuLe, which have been found effective as additives
to ~L~"~ I.ing solutions in preventing the redeposition even of
dyes, such as indigo, which are poorly soluble in acidic
solutions:
W095/35363 l ~ 2 q 4 7 r~ r78
Product 1 ~ SLLuul -~1 Inforr-tion
Natural and Semisynthetic
Polysarrh~rides
KELZANTM Xanthan gum
tMerCk & Co., Rahway, N.J.)
Rhamsan gum
Welan gum
Guar gum
Locust Bean gum (principally, galact~ nn~n
KELGINTM MV, KELGINTM LV Sodium Alginate
(Merck & Co.)
Other alginic acid metal salts
KELACIDTM Alginic acid (polymannuronic
(Merck & Co.) acid + polyguluronic aoid)
NATROSOLTM 250 HR HydLu~yetllylcellulose
(Aqualon Co., Wilmington, DE)
METHOCEL~ E5, E4M Hydsvxy~uLu~ylmethylcellulose
(The Dow Chemical Co.,
Midland, MI)
MT~orFTTM HB-lOO HydLu~yBuLylmethylcellulose
(The Dow Chemical Co.)
Gelatin
Casein
Na~nral/Synthetic Inn~nic Silicates
Kaolin H2Al25i20pH2o
Fullers Earth Colloidal Aluminum Silicate
VALFORrM 150 Na2OAl203(5iO2)x(H2o~y
(PQ Corp.
Valley Forge, Pa.)
N~'~ 34, 38, SD-1, SD-2 Organically modified
(Rheox, Inc., Hightstown, NJ) montmorillonite where
; montmorillonite = Al2034SiO2H20
Bentonites Al203-4SiO2H20~
R'33(Al,Mg)2Si~O1O(OH)2-nH2o
W095~363 2- 1 92~47 ~ 78
12
T~r~ATT~T~M 200 Smectite clay (Magnesium-
(American Colloid Co., aluminum-silicate mineral)
Arlington Heights, IL~
ZEOSYL~ llOSD, DIAFIL~ 810 Hydrated amorphous sio2
(J.M. Huber Corp., Borger, TX)
nYukl~ R
(Dry Branch Kaolin Co.,
Dry Branch, GA)
Montmorillonites
Polyalkylene O~;de polyln~rs
TETRONIC~ 908, H~OCH~CH~y-(OCHCH,CH~ (c~lr~ru~)l-cH2cHlo)y-H
1508 NCH2CH2N
~BASF Co~.) H-(OCH~CH~y~OCHCH~CH~ ~ r~n)l CH~CH2O)~-H
POLYOX~ WSR N-10, WSR N-3000 (CH2CH2O)n
WSR N-750
(Union Carbide Corp.
Danbury, Conn.)
C ~ ~ 400, 4600, 20M HO-(CH2CH2O)nH
(Union Carbide Chemicals
& Plastics)
Acrylic Pol~n~rs
CARBOPOL~ 907,910 Acrylic acid, homopolymer
(The B.F. Goodrich Co., t (CH2CHCOOH)o ]
Akron, OH)
CARBOPOL~ 614,615 High MW Polyacrylic acid
(The B.F. Goodrich Co.) ~r~ ' w/poly~lkenylpoly~ther
CARBOPOL~ 613,1622 Croecl~nkD~ acrylic copolymers
(The B.F. Goodrich Co.)
CARBOPOL~ 681 X-l Acrylic polymer: ethyl
(The B.F. Goodrich Co.) acrylate (formulated)
SOKALAN~ PA 70-PN, 110S Linear Polyacrylic acid,
(BASF AG, (MW: 70,000 h 250,000)
Ludwigshaten, Germany)
SOKAI~M HP-22 CAS #25820-49-9 (copolymer)
(BASF AG)
COLLOID 117/50,207
COLLOID X-0125-KN 706
SU~ t SHEET (RULE 26)
2 1 92947
~ W095/35363 1 3 .~~ 78
GOODRITE~ K-7600 N Linear polyacrylic acid,
(B.F. Goodrich Co.) sodium salt (MM:60,000)
PARAGUM~ 511
~ (Para-Chem Southern, Inc.
Si ville, S.C.)
ALCOGUN~ L-11, L-15, L-27 Ethyl acrylAte ' yl$c acid
L-37
(National Starch and OhPm;
Corp., Bridgewater, NJ)
ALCOGU~N L--83 Ethyl ~Icrylate:methyl methacrylAte:
(National Starch and ChPmi QA1 v Ll.a~lylic acid terpolymer
Corp.)
ACUSOLll~ 842 Ethyl acrylate:methdcrylic acid
(Rohm and Haas Co.,
ph; 1 AdPlrh; A, PA)
ACUMER~ 8100
(Rohm and Haas Co.)
UCAR~ 102, 104, 107 Dinonylphenolethoxylate/
(Union Carbide Corp., TMN adduct, + ethyl acrylate, +
Danbury, CT) meth_crylic acid polymer ~
UCAR~ 146 Butyl acrylate + styrene
(Union Carbide Corp.) methacrylic acid polymer (~ ,
UCAR~ 106 HE Acrylic polymer - (trnde aecret~
(Union Carbide Corp.)
TANOL~ 731-D & 850 Acrylic acid polymer
(Rohm and Haas Co.)
NEROPAN~ VD Acetic acid ethenyl ~~ter polymer
with oxirane (C,H602C2H~O)x
Suitable cPl 1111ACe enzymes for use in the novel
st-r ' ;ng method include any cplllllAcpc~ including those
pLod~d from fungal or bacterial sources that are optimally
active in acidic solutions in degrading cPlllllosi~ fibers.
Illustrative examples o~ such acid cPll-1lA-e enzymes include
CYTOLASE~ and IndiAge~ enzymes (produced by GPnPn~r, Inc.,
South San Francisco, California) and CELLUSOFT~ and DENIMAXu
(produced by Novo Nordisk, Danbury, Conn.) which are derived from
a strain of Trichoderr- lon~ihraohiA~llm (formerly T- rQ~i)-
SUBSTITUTE SHEET (RULE26)
W095/35363 2 I q 2 9 4 7 Icl/~z,~C r78
14
It is to be understood, however, that the invention i8
not limited to any particular c~ llAr~e enzymes or any particular
sources for such enzymes, but instead comprehends the use of any
enzymes with c~ ce degrading activity r-Ylm;zed in an acidic
medium, which may be defined as a medium with a pH less than 7.0,
but preferably within a p~ range of about 4 to about 6.
To achieve the objects of the invention, it i5
necessary that the dye redeposition or backstaining inhibiting
additives be present in the fabric LL~ai L solution in a weight
(w/w) concentration not less than about 0.005%. This minimum
level may vary ~p~n~ing on the clas5 of additives utilized. For
example, the following are representative cu..~nLLation ranges
for the various classes of redeposition preventing additives,
based on experimental test results:
Natural/synthetic inorganic silicates: .025 - 5.0%
Polyalkyleneoxide polymers: .025 - 2.5%
Polysaccharide polymers: .005 - 5.0%
Acrylic homopolymers and copolymers: .005 - 8.0%
It should be stressed that the above weight
cu.,cel.LLa~ion ranges are based on the total weight of wash liquor
in which the fabric is immersed and/or tumbled. The invention
is not limited, however, to any specific method, sequence or
formulation for adding the ~cfi~ntlAl , c of the invention,
i.e. the acid cellulase enzymes and anti-redeposition additives
to the wash liquor. For example, the enzymes and anti-
redeposition additives can first be blended with suitable
solvents and other optional ingredients, with the resultant
formulation (in liquid, con1e~-L-ate, gel or other form) being
added to the wash water, or the individual _ , Ls can be
~ W09S/3S363 21 92947 P~
separately added in dry or fluid fo7-m to the wash water.
The water-based compositions used in the novel method
of the invention may include not merely appropriate weight
cù--~ellL~tions of acid cn~ Ace enzymes and anti-backstaining
additives but also optional additional ingredients such as
buffers to maintain the pH of the composition at a fairly stable
level, surfactants to increase the wettability of the aqueous
solution, promoting the activity of the enzyme in the treated
fabric; solvents to help dissolve or disperse the enzymes and
surfactants; cellulase activators; antioxidants; solubilizers;
and builder c l~nnnts such as divalent sequestering agents.
n_~L~e"~tive examples of these optional ingredients include the
following:
Sl7rfac7-~7nts - polyethylene oxide polymers, polyproplene
oxide polymers, ethylene oxide-propylene oxide block copolymers,
ethoxylated Cl~8 alkyl phenols and ethoxylated Cll8 aliphatic
alcohols.
Solvent~7 - ethylene glycol, propylene glycol, and
oligomers and higher polymers of ethylene or propylene glycol in
the form of polyethylene or polypropylene glycols, alcohols,
terpenes, and aliphatic, aromatic and naphthenic hyd~u~,bol-s~
CPllul~7ce nn7~me act;var~7rs - proteins, cobalt and its
salts, magnesium and its salts, calcium and its salts, potassium
and its salts, sodium and its salts or - ~ crh;7rides such as
mannose and xylose.
~ nti~ir7;7nts - tert-butyll-y~Lo~y~oluene, 4,4'-
butyli-7nnnhi~(6-tert-butyl-3-methylphenol), 2,2'-butyli~7nnnb;~7(6-
tert-butyl-4-methylphenol), ~ ~-o~-yLenated cresol, distyrenated
cresol, ~ ~yL~nated phenol, distyrenated phenol and 1,1-bis(4-
W095/35363 21 92q47 . I/~ 78
Ly dL UXy ~henyl)cyclohexane.
soluhili7Prs - lower alcohols such as ethanol,
bPn70n~ 1fonate salts, lower alkylhPn7~nPslllfonate salts such
as p-tolupnpclllfonate salts, glycols such as propylene glycol,
acetylhPn7~nesulfonate salts, acetamides, pyridinedicarboxylic
acid amides, benzoate salts and urea.
Builders - organic phosphates, phosphonates,
phosphonocarboxylates, amino-polyacetates, polyacrylic acids;
non-dissociating polymers such as polyethylene glycol, polyvinyl
alcohol and polyvinyl pyrrolidone, and salts of dicarboxylic,
diglycolic and sulfonated carboxylic acids, borates, citrates and
mixtures thereof.
The enzyme compositions used in the novel methods may
be in any conventional form, including liquids, th;~konP~
liquids, cunu~,.LL~tes, gels or solids. Various such compositions
have been disclosed in the prior art and are known to those of
skill in the formulation of textile treatment and processing
pl u~lu~;~2. .
The following are representative examples of water-
based compositions according to the present invention for use in
the novel method of treating dyed fabric or y~L Ls to produce
a stonewashed appearance while substantially preventing
redeposition of dye onto the treated material. These examples
are not intended, however, to limit the invention in any way or
to set forth ingredients, materials or ~ul,c~"LL~ion ranges which
must be used exclusively to practice the invention.
Examples 1-7 de~ine compositions for use in the present
invention which contain an acid cPllnl~e enzyme derived from
lon~ihrarhi~tn~, a buffer comprising 31.2% sodium acetate, 23.3
~ W095/3S363 2 1 9 2 9 4 7 ~ 78
acetic acid and 45.5% water, the specified dye redeposition
preventing additive and water, quantity sufficient to 100% by
weight.
~AMPL~ 1
%
Bnzyme - 1.0
Buffer - 2.0
BENTONITE~ - 0.1
Ex~MPLF. 2
Enzyme - O.125
Buffer - 50.0
ZEOSYL~ 110 SD - 0.5
Ex~MPLR 3
Enzyme - 0.25
Buffer - 50.0
TETRONIC~ 908 - 0.5
RXAMPLr' 4
Enzyme - 0.75
Buffer - 2.0
POLYOX~ WSRN-750 - 0.1
~X~MPLR 5
Enzyme - 0,5
Buffer - 0,5
POLYOX~ WSRN-3000 - 0.5
~X~MPL~ 6
Enzyme - 0,75
Buffer - 2.0
CARBOPOL~ 910 - 0.1
EX~MPr.r~. 7
Enzyme - 0,5
Buffer - 0.5
CARBOPOL~ 910 - 0.5
EX~MPL~ 8
W095/35363 21 92947 r~ 78
18
Laboratory testing was performed utilizing the
compositions of Examples 1-7 in the wet processing of indigo dyed
denim fabric to quantify the anti-backstaining benefit of each
additive. The method used to determine changes in
antibackstaining characteristics was to measure the Total Color
Difference (~E) on a HunterLab 0/45 D25-PC2 Colorimeter,
available from Hunter Associates Laboratory, Inc., Reston, VA.
This in~Lr, ~ reads three opponent-color scales, where L
repre6ents black _ white (where black=0 and white=loO), a
represents red ~ green (where +a = red, and -a = green), and b
represents yellow _ blue (where +b = yellow, and -b = blue). ~E
is calculated by the following formula:
~E = [t~L)2 + t~)2 (~)2]1~2
Initial and final L,a,b readings are performed at the same
location on individual test swatches.
Testing was performed in a Launder-Ometer, available
from Atlas Electric Devices Co., Chicago, IL. The Launder-Ometer
is an AATCC-a~lov~d standard laboratory washing machine which
rotates (at 40 + 2 rpm) up to 20 - 3 in. X 8 in. stainless steel
cannisters (1.2 liter capacity) in a thermostatically controlled
water bath. Each canister contained 200g. of one test solution
of Examples 1-9, one - 4 in. X 4 in. white cotton swatch, one -
4 in. X 4 in. desized 14 oz. indigo denim swatch, and 45 - .25
in. stainless steel balls.
The pH of each test solution was adjusted to 5.0 ~ 0.1
units. Each canister was sealed and rotated in the Launder-
ometer at 132 + 2~F for 60 or 75 minutes. At the conclusion of
the test, the fabric swatches were removed and rinsed in a
-
~ W095/35363 2 1 9 2 9 4 7 1 ~ n
19
Kenmore (Series 60) home washer at a low water level for a six
minute cycle. At the completion of the spin cycle, all test
~ swatches were dried in a conventional domestic dryer. Final
L,A,b readings were taken and the Total Color Difference (QE) was
calculated for the white test swatches. Percent ; u~ t (%I)
in ~E for each test solution in comparison with control solution
(the same concentrations of enzyme and buffer without the
antibackstaining additives) was calculated as follows:
QE~
%I = ~ x 100
\ QE~Il
Using the above described test method, Table A lists
percentage ill~,U~UV~ t values for the various backstaining
inhibiting additives used in Examples 1-7.
TABLE A
Test Solution Ti-- /m;n.) ~ ~I
Ex. 1 60 21
Ex. 2 60 23
Ex. 3 75 15
Ex. 4 60 24
Ex. 5 75 23
Ex. 6 60 33
~ Ex. 7 75 69
~095/35363 2 ~ 9294 7 ~ u~ . 78 ~
E~MPL~ g
Twenty four pounds (24 lb.) of previously desized denim
jeans plus a white cotton test swatch were placed in a 125 lb.
capacity ~ilnor open-pocket washer-extractor. The machine was
filled with 35 gallons of water znd heated to 138~F ~59OC). The
specified antibackstaining additive and 21.7 ml. of acid
c~ ce enzyme per kg. of denim were then added to the washer
and tumbled for twenty five minutes. An acetate buffer was also
in~ P~ to control the p~ at 5.1 + 0.1 units. The wash liquor
was dumped and the contents of the washer were rinsed at 140~F
~600C) then 110~F (43OC) in 37 gallons of water. The garments
and test swatches were then dried and final L,a,b readings were
taken. Table B indicates the additive doses and the respective
~E values.
TABLE B
~ltive ~Q&~ ~-
(gm. additive/kg. denim)
None - Control - 34.8
Xanthan Gum 10.61 24.5 (%I=29.6)
Sodium Alginate 10.45 24.8 (~I=28.7)
EYAMPL~ 10
Twenty one pounds (21 lb.) of denim ~eans plus a white
cotton test swatch were placed in an 85 lb. capacity Unimac open-
pocket ~L~L-~L~ctor. The machine was filled with 38 gallons
of 140~F (600C) water containing an amylase enzyme desizing
stripper. After 12 minutes, the ~ci~ing solution was drained.
~ W095/35363 2 1 q2947
The machine was filled with 42 gallons of 1200F (490C) water for
a 2 mLnute rinse. The washer was again filled with 42 gallons
of 140~F (600C) water. The antibackstaining additive and 18.6
ml. of acid r~ ce enzyme per kg. of denim were then added to
the washer and tumbled for twenty minutes. An acetate buffer was
also included to control the pH to 5.1. The wash liquor was then
dumped and the contents of the washer were rinsed three
successive times at 120~F (490C) in 68 gallons of water. The
garments and test swatches were then dried and final L,a,b
reading were taken. Table C indicates the additive doses and the
respective ~E values.
~;tive LQfi~ ~E
(gm. additive/kg. denim)
None - Control - 29.9
Ethylacrylate:
methacrylic acid
copolymer 3.57 22.1 (%I=26.1)
It has thus been shown that there are provided methods
which achieve the various objects of the invention and which are
well adapted to meet the conditions of practical use.
As various possible l~ho~ 5 might be made of the
above invention, and as various changes might be made in the
r~ s set forth above, it is to be understood that all
matters herein described are to be interpreted as illustrative
and not in a limiting sense.
What is claimed as new and desired to be protected by
Letters Patent is set forth in the following claims.
