CA1066981A - Detergent composition with antiredeposition properties - Google Patents

Abstract

A B S T R A C T

The invention lies in the field of laundry detergent compositions for synthetic textile fabrics, especially polyesters.
The invention is directed to a composition for washing synthetic textiles consisting of a nonionic surfactant and a minor amount, based on the surfactant, of a low molecular weight hydroxybutyl methylcellulose.
The claimed composition provides advantages in detergency and in antiredeposition over the closely related prior art compositions.

Description

~0669~1 It is known to use cellulosic polymers such as carboxymethylcellulose in detergent formulations to inhibit redeposition of soil on the fabrics being washed. Combinations of carboxymèthylcellulose and a methylhydroxyalkylcellulose have been used for the purpose in conventional phosphate-detersent composi-tions such as those described in U.S. Patents 2,886,533 and 3,523,088, also in German Patent Applications 2,138,731 and 2,340,161. U.S. Patent 3,928,213 discloses a fabric softener composition that includes an alkylcellulose or hydroxyalkyl alkyl cellulose and a non,ionic sur-factant.
Carboxymethylcellulose, while an effective redeposition inhibitor for cotton fabrics, is less effective with synthetic fabrics, particularly poly-ester. Also, in recent years the use of phosphate builders such as sodium tripolyphosphate in detergent formulations has been minimized or avoided in order to reduce the concentrations of phosphate in waste water.
A common replacement for the phosphate component in , '` detergent formulations has been sodium carbonate or a ... .
' mixture of sodium carbonate and sodium bicarbonate.
Sodium nitrilotriacetate and sodium ethylenediamine-tetraacetate have also been used as detergency builders.
Generally, the detergency of carbonate formulations is significantly poorer than that of corresponding high phosphate formulations, especially with synthetic fabrics.

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The deficiencies of the prior art compositions have been substantially overcome by the present invention, which is a detergent composition for washing a synthetic textile fabric consisting of a nonionic surfactant and ~ 5 from 0.2 - 50 percent, based on the weight of the sur-: factant of a low molecular weight hydroxybutyl methyl-cellulose having a DS of 1.5-2.5 methoxyl and an MS of 0.01 to 0.8 of hydroxybutyl groups.
~ Preferably, this combination is the essential basis of an otherwise conventional detergent composition which provides, in addition to the antisoil activity, unusually good detergency and excellent antiredeposition effect. The hydroxybutyl methylcellulose component is characterized by having a DS of about 1.5-2.5 methoxyl groups and an MS of about 0.01 to about 0.8 hydroxybutyl groups.
In addition to the above composition, the present invention is also directed to a detergent com-position for washing a synthetic textile fabric consisting Of:
(a) 7-70 percent on a dry basis of at least one nonionic surfactant which is an alkyl monoether of a polyethylene glycol of 5-20 alkylene oxide units and the alkyl group is ~ of 8-22 carbon atoms, an alkylphenyl monoether of said : 25 polyethylene glycol wherein the alkyl group is of 8-18 carbon atoms, or the condensation product of the amide of an alkanoic acid of 8-20 carbon atoms with 6-20 moles of ethylene oxide, (b) 5-30 weight percent, based on the entire composition, of sodi~m silicate having an SiO2/Na20 ratio of 2-3/1, ,. ~, 17,99lB -2-: . . , -~()66~8~
(c) up to 80 percent of a builder salt component, and (d) 0.05-5 percent based on the dry weight of total composition of a low molecular weight hydroxybutyl methylcellulose having a DS of 1.5-2.5 methoxyl, and an MS of 0.01 to about 0.8 of hydroxybutyl groups.
About 0.3-2 percent of hydroxybutyl methyl-cellulose component is usually preferred. The basic composition as outlined may also contain as an optional component 5-40 weight percent Na2So4. This new detergent formulation is particularly advantageous in washing polyester and other synthetic fabrics.
The terms DS and MS as applied above to the cellulosic polymer refer to the amounts of substitution on each anhydroglucose unit in the cellulose molecule.
DS means degree of substitution of the three hydroxyl groups on each anhydroglucose unit, to form methyl ether groups in the present case, and is an average number. For example, in the hydroxybutyl methylcellulose of this invention, an average of about 1.5-2.5 of the hydroxyl groups per anhydroglucose unit have been ether-ified to form methoxyl substituents. Best results are usually obtained when DS = 1.8-2~3.
MS means the average moles of reactant, in this case butylene oxide, combined with free hydroxyl groups per anhydroglucose unit. Since the butylene oxide reaction product itself has a reactive hydroxyl group which can react further to form a butylenoxy chain, the value of MS reflects a sum of butylenoxy ':~

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106~81 units present both as single hydroxybutyl and butylen-oxyhydroxybutyl substituents for each anhydroglucose moiety. As noted above, MS can range as high as about - 0.8 and is preferably 0.01-0.6 for this hydroxybutyl methylcellulose. Generally, best results are obtained with hydroxybutyl methylcellulose wherein the MS value is inversely proportional to the DS value. For example, a hydroxybutyl methylcellulose having a DS of 1.5 and MS of 0.4 can give good results comparable to those obtained with DS of 2 and MS of 0.01.
The hydroxybutyl methylcellulose useful in this new detergent composition is of relatively low molecular weight. This property is most readily defined by measuring the viscosity of an aqueous solu-tion. Preferred materials are those which show a viscosity of about 10-400 cps in 2 percent aqueous - solution at 20C and best results are obtained when the viscosity is in the range of 20-200 cps. Hydroxy-butyl methylcellulose can be made by conventional means such as described in Savage, U.S. Patent 2,835,666.
A liquid formulation can contain as much as 70 percent nonionic surfactant based on the total active ingredients. Dry formulations preferably contain about 7-30 percent of this component. The nonionic surfactant can be broadly defined as compounds produced by the condensation of ethylene oxide with an active hydrogen or hydroxyl group in an organic hydrophobic compound which can be aliphatic or alkyl-substituted ' .

-17,991B -4-- aromatic in nature. The length of the hydrophilic polyoxyethylene alcohol radical thereby formed on the hydrophobic and lipophilic nucleus can be readily adjusted to yield a water-soluble compound having the desired hydrophilic-lipophilic balance (I~LB). Sub-stantially any such substance which has the required stability under relatively high pH laundry conditions and good detergent properties is useful in the present invention. An HLB value in the approximate range of 12-16 is preferred for best activity as a detergent.
The nonionic surfactant is preferably any one or a mixture of two or more of the commonly avail-able higher alkyl monoethers of polyethylene glycol and the corresponding higher alkylphenyl monoethers.
These surfactants are the condensation products of about 5-20 moles of ethylene oxide with a mole of alkanol of about 8-22 carbon atoms, or with a mole of alkylphenol wherein the alkyl group is of about 8-18 carbon atoms. Some examples of the commercially available compounds of this type are the products of condensation of octyl alcohol with six moles of ethylene -~
; oxide, dodecyl alcohol with thirteen moles of ethylene oxide, dodecyl alcohol with ten moles of ethylene oxide, nonylphenol with ten moles of ethylene oxide, and octyl-phenol with nine moles of ethylene oxide.
The surfactant can also be the condensation product of a higher alkanoic acid amide of about 8-20 carbon atoms with about 6-20 moles of ethylene oxide, 17,991B -5-\

the amount of oxide be~ng roughly proportional to the molecular weight of the acid. Examples of this class include stearamide + 15 EO, lauramide + 12 EO and caprylamide + 10 EO.
Another well-known type of nonionic surfac-- tant useful in this invention is the condensation product of ethylene oxide with polypropylene glycol, for example, in the form of block copolymers. Liquid products of this kind made by condensing up to about an equal weight of ethylene oxide with a polypropylene glycol of 1500-2000 molecular weight have good de-tergent values.
Detergency builders generally can be used at a concentration of up to about 80 percent of the wei~ht of active ingredients. A liquid formulation may contain no builder component whereas a dry composi-tion can contain about 8-80 percent builder and pref-erably from about 25 percent to about 60 percent of builder is used, depending on the kind of builder, the type of formulation and its application. Any of the commonly used organic or inorganic builder salts can be used effectively. These are water-soluble salts, usually alkali metal salts, and in practice sodium salts are the standard choice. Among such salts are the phosphates, which term is used to include ortho-phosphates, pyrophosphates, polyphosphates, and phos-phonates. A phosphate builder is preferably used in a proportion of about 15-60 percent of the dry deter~ent composition, most preferably about 20-~G percent when 17,991B ~6-.

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it is the principal builder present. Other effective builders are amine polyacetates such as ethylenedi-aminetetraacetate and nitrilotriacetate. These can be used in a proportion of about 8 percent to about 50 percent, preferably about 20-30 percent of the dry composition.
,; Of particular interest in the present inven-tion are carbonate builders, partially because of limitations put in recent years on the use of phos-phates and amine polyacetates, but also because of unexpectedly good detergency found when these builders are used with this nonionic surfactant-cellulose ether combination. A sodium carbonate component can be Na2CO3 alone or it may be a mixture of Na2CO3 and NaHCO3 in order to hold the pH of the wash solution below the level provided by Na2CO3 only. An equimolar mixture of carbonate and bicarbonate (sodium sesqui-carbonate) is suitable for most applications. The total quantity of carbonate is adjusted within the defined limits according to the hardness of the local ,.
water. Usually about 50-60 percent of carbonate is employed based on the weight of dry formulation unless the water is relatively soft.
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Water-soluble silicates are useful auxiliary builders used in combination with any of the above.
Sodium silicate as previously defined is a preferred component of the claimed composition, preferably in - an amount of about 5-15 percent of the whole.
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~066981 An optional component of the formulation - is sodium sulfate (Na2S04) present in a proportion as previously defined. Best results are usually obtained when sodium sulfate is present in a propor-tion of about 5-15 percent by weight of total formu- ;
lation on a dry basis or up to about 30 percent when the formulation is to be spray dried. Sodium chloride is an inert impurity often present in minor amount.
A principal advantage of this new detergent , 10 composition is its characteristic property of imparting to a synthetic textile fiber or fabric a resistance to soiling when that fiber or fabric is contacted with an aqueous solution of the composition. Only the basic combination of nonionic surfactant with the hydroxybutyl methylcellulose is necessary in the solution to produce the antisoil effect on the contacted textile fibers. The maximum initial antisoil activity is obtained when the textile material is prewashed with either this basic solution or with a solution of the full detergent formu- ~ -lation before use, although conventional washing using this composition after soiling also builds up and main-tains a high resistance to soiling after repeated washings so that the material stays cleaner between washes .
The new detergent composition is advanta-geously used on synthetic textiles such as polyesters, polyamides, polyacrylates, and blends thereof. It is particularly useful for washing polyester fabrics.

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Compositions within the present invention . , :
were prepared and tested according to the following procedure. The results were compared to those obtained by the same procedure using somewhat similar known detergent compositions. ~ ~
The detergency measurement was made in a -soil accumulation test in which swatches of fabric 5 in. x 5 in. (12.7 cm. x 12.7 cm.) were subjected to multiple soiling-washing cycles. Antiredeposition was measured on unsoiled swatches of the same fabric put in the wash water during washing. Measurements were by reflectance. The detailed procedure was as follows:
(1) A standard soil slurry was prepared by dispersing 16 g. of <270 mesh representative vacuum cleaner house-hold dirt in 3 liters of deionized water.

(2) Eight swatches of fabric were added to 3 liters of the soil slurry and the slurry was shaken on a ' mechanical shaker for one hour.

(3) The swatches were removed and dipped twice into - 20 warm tap water to remove loose soil, excess water was squeezed out, the wet swatches were blotted on clean paper towels and dried in a forced air oven at 55C.

(4) The dried swatches were immersed in 2 percent artificial sebum (4:1 lanolin-oleic acid) solution in perchloroethylene, excess solution was squeezed out, and the wet swatches were partially air-dried in a hood, then drying was completed in a forced air oven at 55C.

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(5) Swatches soiled as described above and clean swatches of the same material were washed together in a liter of 0.2 percent solution of detergent com-position in water (150 ppm hardness) for ten minutes at 48C in a test washing machine. ~ -

(6) The washed swatches were flooded and squeezed out twice with deionized water, then washed in the washing machine for five minutes with a liter of water (150 ppm hardness) at room temperature. The swatches were removed from the rinse water, excess water was squeezed out, and they were dried at about 55C in a tumble drier.

(7) Reflectance of the dry swatches was determined using a commercial model reflectometer.
Solutions containing 0.2 percent by weight of total detergent composition were made up as follows for test and comparison purposes:
` AATCC Standard Phosphate Formulation - 0.028% linear dodecylbenzenesulfonate, Na salt 0.0046% higher linear alkyl monoether of poly-ethylene glycol 0.005% high molecular weight soap 0.096% Na tripolyphosphate 0.0194% Na silicate (SiO2/Na2O = 2.0) 0.0308% Na2S4 0.0005% sodium carboxymethylcellulose 0.0157% inerts and moisture balance 150 ppm hardness water i .

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Carbonate-built Formulation 0.04% nonionic surfactant 0.053% NaHCO
0.067% 2 3 ~ :~
0.02% Na silicate (SiO2/Na2O = 2.4/1) 0.018% Na2SO~
O.C02% hydroxybutyl methylcellulose (or Na2SO4 for a blank) balance 150 ppm hardness water . Examples 1-10 Using the standard phosphate formulation and the carbonate formulation listed above with no cellulosic polymer additive and the carbonate formu- - .
lation containing 0.002 percent of a hydroxybutyl : 15 methylcellulose with DS, MS, and viscosity values as shown, swatches of doubleknit polyester fabric were subjected to three wash cycles for determination of -.~ antiredeposition and detergency as previously described.
' The nonionic surfactant was the condensation product of a C15 (average) linear alkanol with about 9 moles of ethylene oxide.

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17, 991B -12-1~6698~ -Example 11 According to the procedure of Examples 1-10, swatches of doubleknit polyester cloth ~re ~bjected : to three wash cycles using as wash solutions the standard phosphate solution, a blank carbonate solution containing no cellulosic polymer and made up with a lower concentration - of the same nonionic surfactant, the carbonate solution :
with added 0.002 percent sodium carboxymethylcellulose, and the carbonate solution with added 0.002 percent HBMC
(1.88 DS methoxyl, 0.09 MS hydroxybutyl, 2 p0rcent vis-cosity = 67 cps). The blank carbonate solution was as shown above but contained 0.024 percent nonionic surfactant and 0.034 percent Na2SO4.
Average reflectances (2 replicates of each) of the washed swatches were as follows: - .
TABLE II : -. Reflectance Wash SolutionAntiredeposition Detergency :
AATCC Phosphate 76.4 51.8 Carbonate blank 76.1 42.5 Carbonate + CMC 75.5 40.5 Carbonate + HBMC 79.6 60.0 Examples 12-14 As described in Examples 1-10, swatches of polyester doubleknit fabric were subjected to three soiling-washing cycles for detergency effect using the 17,991B -13-:...... , ' : ~

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blan]c carbonate formulation for one set of swatches and the carbonate formulation containing 0.002 percent of a hydroxybutyl methylcellulose of DS 1.88, MS 0.09, and 2 percent viscosity 67 cps. The reflectances were measured before and after each cycle. The procedure was repeated twice as a check on accuracy. The average reflectances found are listed in Table III.
TABLE III
Example Reflectance No. Stage Blank with HBMC
12 cycle 1 clean fabric 81 81 soiled 50.9 50.5 washed 70.5 72.2 : 15 cycle 2 soiled 31.8 34.5 washed 54.0 66.0 cYcle 3 ~ r-d 24.3 35.2 `~ 20 washed 42.3 60.6 _ 13 cycle 1 clean fabric 81 81 ; soiled 51.0 51.3 washed 73.1 73.4 cYcle 2 soiled 35.5 39.0 - washed 61.7 67.4 cycle 3 soil-d 29.0 38.6 washed 51.9 67.4 14 cycle 1 clean fabric 81 81 soiled 50.3 49.2 washed 72.9 73.2 17,991B -14-10669Bl TABLE III (cont'd.) - cycle 2 soiled 33.4 39.0 washed 60.5 69.4 cycle 3-soiled 26.1 39.1 washed 47.7 66.7 It is seen from the above figures that the values from each cycle were reasonably reproducible.

The results also show consistently that the swatches washed with the cellulosic polymer are more resistant to soiling. Particularly, in each third cycle, these test swatches pick up less soil when deliberately soiled and are washed cleaner to the point where the reflectance of the washed swatches seem to be approaching a constant level as compared to the steadily deteriorating values ~ <:
for the blank swatches.
: Examples 15-18 Swatches of polyester doubleknit fabric were ; 20 washed according to the three-cycle procedure of Examples 1-10 using various concentrations of a hydroxybutyl methylcellulose (DS = 2.00, MS = 0.05, 2 percent viscosity = 100 cps) in a carbonate-nonionic surfactant formulation.
A ~uantity of 2 grams of formulation was dissolved in a liter of 150 ppm hardness water in each case. The formu-lation had the following composition:
20% by weight nonionic surfactant (same as used in Examples 1-10) -60% NaHCo~.~a2cO3 10% Na silicate (SiO2/Na2O = 2.4/1) 0-1% hydroxybutyi methylcellulose 10-99~ Wa2S04 ~ .

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The reflectance values listed in Table IV
` are those observed after the third wash cycle.
~ TABLE IV
- Example HBMC Reflectance No. wt. %Antirede~sltlonDetergency blank 0 81.6 53.2 ~: 19 0.1 85.4 56.7 0.3 86.2 64.5 21 0.5 86.0 66.1 22 1.0 85.7 67.0 .
~-~ 10 Example 19 Two swatches of new doubleknit polyester were prewashed in each of the following phosphate-containing detergent solutions, rinsed, dried, and then subjected to : a one soil cycle technique. Reflectances were measured after that one soiling cycle to measure the antisoil effect obtained.
Phos hate Blank p 20% same nonionic surfactant used in Examples 15-18 35~ Na tripolyphosphate 45% Na2SO4 .. Antisoil Phosphate Composition 20% same nonionic surfactant used in Examples 15-18 . 35% Na tripolyphosphate 44% Na2SO4 1% hydroxybutyl methylcellulose (2.08 DS CH O, 0.07 MS hydroxybutyl 74 cps, viscosity in 2~ solution) Two-gram portions of each of the above com-: positions were dissolved in one-liter portions of ~ 30 150 ppm hardness water to make up the test solutions.

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Solution l~eflectance Phosphate blank 39.0 Antisoil phosphate composition 52.8 -Example 20 Swatches of two types of polyester and nylon were prewashed in detergent solutions listed below ~ before soiling with dirty motor oil and washing to - determine relative antisoiling effects according to the following procedure.
(1) One swatch each of polyester double~nit, spun --polyester, and nylon 66 were prewashed for 10 minutes at 48C.
(2) The washed swatches were squeezed to remove excess solution and then rinsed in 250 ml deionized water for two minutes.
(3) The rinsed s~atches were squeezed and dried at about 55C in a tumble drier.
(4) The dry swatches were each soiled with 3 drops of dirty motor oil and allowed to stand for 2 hours. -(5) Reflectances of the soiled swatches were measured with a reflectometer.
(6) The combined swatches were washed in one liter of 0.11 percent solution of a commercial laundry detergent for 20 minutes at 50C, rinsed, and dried as above and reflectances were measured.
The following detergent solutions were made up in 90 ppm hardness water to contain 0.04 percent surfac-17,991B -17-', . ' ' ' ", "

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tant, 0.07 percent Na tripolyphosphate, 0.02 percent Na silicate (SiO2/Na2O = 2.4/1), ~a2SO4 as noted, and, when used, 0.002 percent antisoilant.
TABL~ VI
'rest No.Surfactant % Na~SO4 Antisoilant 1 Nonionic 0.07 none 2 " 0.068CMCa 3 " 0.068HBMC-Ab 4 " 0.068HBMC-BC
LAS 0.07 none 6 " 0.068CMCa 7 " 0.068lIBMC-A

8 " 0.068HBMC-BC

acarboxymethylcellulose, 0.7 DS sodium carboxymethyl.
bhydroxybutyl methylcellulose, 2.08 DS CH O, 0.07 MS hydroxybutyl, 74 cps (2 percent solution).
Chydroxybutyl methylcellulose, 1.53 DS CH30, o . 1 r~s hydroxybutyl, 29.5 cps (2 percent solution).
dlinear dodecylbenzene sulfonate, Na salt.
econdensation product of a C 5 linear alkanol with about 9 moles of ethylene oxlde.

neflectarce readings are reported as Q Reflectance =
Reflectance washed Reflectance soiled 'he re_ults show clearly the strong antisoil effect obtained by the combination of nonionic surfactant with the hydroxybutylated methylcellulose, particularly that with the higher DS value.

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Claims (12)

THE EMBODIMENTS OF THE INVENTION IN WHICH AN EXCLUSIVE
PROPERTY OR PRIVILEGE IS CLAIMED ARE DEFINED AS FOLLOWS:

1. A detergent composition for washing a synthetic textile fabric consisting of a nonionic surfactant and from 0.2-50 percent, based on the weight of the surfactant of a low molecular weight hydroxybutyl methylcellulose having a DS of 1.5-2.5 methoxyl and an MS of 0.01 to 0.8 of hydroxybutyl groups.

2. A detergent composition for washing a synthetic textile fabric consisting of:
(a) 7-70 percent on a dry basis of at least one nonionic surfactant which is an alkyl monoether of a polyethylene glycol of 5-20 alkylene oxide units and the alkyl group is of 8-22 carbon atoms, an alkylphenyl monoether of said polyethylene glycol wherein the alkyl group is of 8-18 carbon atoms, or the condensation product of the amide of an alkanoic acid of 8-20 carbon atoms with 6-20 moles of ethylene oxide, (b) 5-30 weight percent, based on the entire composition, of sodium silicate having an SiO2/Na2O ratio of 2-3/1, (c) up to 80 percent of a builder salt component, and (d) 0.05-5 percent based on the dry weight of total composition of a low molecular weight hydroxybutyl methylcellulose having a DS of 1.5-2.5 methoxyl, and an MS of 0.01 to about 0.8 of hydroxybutyl groups.

3. The composition of Claim 2 wherein the builder is a sodium phosphate present in a quantity of 25-60 weight percent, based on the dry composition.

4. The composition of Claim 2 wherein the builder is sodium nitrilotriacetate present in a quantity of 8-50 weight percent, based on the dry composition.

5. The composition of Claim 2 wherein the builder is a sodium carbonate present in a quantity of 20-80 weight percent, based on the dry composition.

6. The composition of Claim 5 wherein the sodium carbonate is a mixture of Na2CO3 and NaHCO3.

7. The composition of Claim 2 wherein the composition contains 5-40 weight percent of Na2SO4, based on the dry composition.

8. The composition of Claim 2 wherein the nonionic surfactant is the condensation product of an alkanol of 8-22 carbon atoms with 5-20 moles of ethylene oxide.

9. The composition of Claim 8 which con-sists of 20 percent by weight of the alkanol-ethylene oxide condensation product, 60 percent of an approximately equimolar mixture of Na2CO3 and NaHCO3, 10 percent of sodium silicate having a ratio of SiO2/Na2O of 2-3/1, 0.2-2 percent of a hydroxybutyl methylcellulose having a DS of about 1.8-2.3 and an MS of about 0.01-0.6, and 10 percent of Na2SO4.

10. The composition of Claim 2 wherein the nonionic surfactant is the block copolymer resulting from the condensation of ethylene oxide with poly-propylene glycol.

11. A method for imparting antisoil prop-erties to a synthetic textile which comprises con-tacting said textile with an aqueous solution of the composition of Claim 1.

12. The method of Claim 11 wherein the textile is a polyester fabric.