US2369399A - Process for sheening pile fabrics - Google Patents

Description

manual-"eh. 13, 1945 UNITED "STATES PATENT- OFFICE,"

2,369,399 V raocass roa' sesame rm; FABRICS James Douglas MacMahon, Niagara Falls, and Lorenzo D. Taylor, Lewiston, N. .Y., assignors to The Mathieson Alkali Works, Inc., New York, N. Y., acorporation of Virginia No Drawing.

- l6 Claims.

This invention relates to an improved process for sheening pile fabrics, and more particularly to a method for sheening the pile of wool rugs,

- carpets, and fabrics of a like nature, all of which will be referred to herein as woolrugs.

The process commonly known as frug sheening has come to be of'increasing importance in the manufacture of pile fabrics. The methods of/treatment .known tow and used by the'art, most of which have involved treatments with solutions containing bleaching powder or sodium hypo- Application October 21, 1942, Serial No. 462,838

c1, a-12s) plishes this by providing a chemical treatment which producesa minimum loss of fiber strength and at the same time produces a uniform maximum sheen without altering or destroying the coloror the texture of the fabric. This invention, furthermore, provides a processwhich is v easily operated and controlled.

We have found-that a high degree of sheen may be attained and the disadvantages hitherto involved either-eliminated or minimized by subjecting the pile 'of the rug to treatment in an chlorite, have not, in spite of. attempts at rigid' control, produced completely satisfactory results. Operators employing the methods, of the art or variations of them haveencountered numerous difliculties and found'that they possss many serious disadvantages. Outstanding among these have been the inability of such methods to give reproducible results. This-is a particular disadvantage in themanufacture of carpets where a certain pattern and flnish must remain substan-' tially uniform throughout a large quantity ofmaterial which is manufactured over a long period of time. For various reasons which are more fully discussed below, it has been very difaqueous solution containing droxyl ions and peroxide in concentrations wit n the limits prescribed below, the presence of the peroxide and of the hydroxyl ions within the prescribed limits of concentrations being the prerequisites for the v effectivenessof the sheening solution.

fic'ult if not impossible to obtain a constant sheen and a uniform shade of color by the use of the methods of sheening known to the art. In many cases ithas been found that a treatment appropriate to produce the desired sheen also causes a phate, sodium perborate, sodium percarbonate,

and the like, being examples of such persalts. Organic peracids' and their salts also serve as' 9' sources of hydrogenperoxide, peracetic acid, perloss or fading of the color in the pile and thus in the fabric itself, or sometimes introduces an entirely different tint in the starting color. A further, outstanding difllculty has been that 'a serious loss of tensile strength of the pile often accompanies the sheening process. This, of course; greatly reduces the-life of the fabric by loweringits resistance to wear. Certain of the known methods have also been found to possess a-tendency to remove the twist from the yarn, thus making sheeningdifilcult and causing the The peroxide may be supplied to the solution by dissolving'th'erein a peroxide forming material which may be or a ic Or inorganic in character.

Inorganic peroxide forming materials include the peroxides such as hydrogen peroxide, alkali metal peroxides (sodium peroxide for example), alkaline earth metal peroxides (barium peroxide for example) and persalts which in aqueous solutions form hydrogen peroxide, sodium perphosbenzoic acid, sodium peracetate. and sodium perbenzoate being examples of such organic materials. P Organic and organo-metallic salts of hy- Y 'drogen peroxide, such as tetramethyl ammonium peroxide and triethyltin peroxide may also be used for this purpose. a

' ness of the peroxide solution may be supplied by i finished product to have anundesirable fuzzy appearance. This tends to disturb the original demarkations inthe patterns. Further disadvantages which the proposed methodsiof sheening have failed to overcome are the-running together of colors in pattern fabrics; uneven or streaky sheening, and variations in color or degree of sheen from the top of the Pile to the bottom.

- It is the primary object of the present inven-.- titon to provide a chemical method of pile fabric sheening which will eliminate or minimizeitheabove recited difflculties and disadvantages which attend the, use of the methods knowntothe art. The process of the' present invention accomgeneral, salts of strong bases and weak acids, 1 whether organic or; inorganic, hydrolyze in water The hydroxyl ions essential for the effectiveany suitable hydroxyl forming compoundcapable of producing hydroxyl ions in such concentrations as to provide a pH within the range prescribed hereinafter. Thus, inorganicbases such as the alkali and alkaline earth hydroxides (sodium hydroxide, calcium hydroxide, etc., for exam- .ple) may be used as the source of hydroxyl ions.

Organic bases and organo-metallic bases which are sufficiently soluble in water also may e used as a source of the hydroxyl ions. Tetramethyl ammonium hydroxide-and triethyltin hydroxide are illustrative examples of such compounds. In

to form free hydroxyl ions and these salts may also'be used as a source of hydroxyl ions. Tri- I sodium phosphate, sodium carbonate. sodium tetraborate, sodium acetate, and the like, are ap propriate examples of such salts. Hydroxyl ions may also be supplied by hydrolysis of the peroxide forming material where such material hydrolyzes in water to form hydroxyl ions. Thus,

in an operation employing hydrogen peroxide, I

H202, as the source of peroxide, the hydroxyl ion 1 -concentration mayv be supplied for example by an alkali metal hydroxide, supch as sodium hydroxide. In operations in which alkaline perox- 7 be added with advantage.

It has been found that in most cases best results are obtained when the solution is main-=' tained at a-temperature'between about 50 and 120 F., and when the period of treatment is from about 15 minutes to about one hour. The treatment in an; alkaline solution containing peroxide maybe followed by rinsing and souring steps in accordance with known methods.

Wool fiber is composed of a cortex covered with epithelial scales. While we are unable to state definitely the course of the chemical reaction occurring between a substance such as bleaching powder and a wool fiber, itappears that the imbricated or serrated surface of the fiber is first attacked and the protectlng scales removed. This exposes the fibrous materialitself to the destructive action of the chemicals in the treating solution and the resulting damaged fiber is unsatisfactory for many purposes, in-

aseasee even a very rlight discoloration of the wool by the hypochlorite is objectionable; and (3) on rugs having colors unusually difficult to maintain in the presence of any hypochlorite treatment, for examplecertain greens containing.

varying amounts of yellow. In, theseinstarices the peroxide treatment ofthe present, invention does not produce the discolorations encountered in the use of a hypochlorlte. i

In the improved sheening process of the present invention, optimum results with respect to the attainment of a maximum sheen concurrently with-a minimum effect on the color andpile are attained by the proper proportioning of hydroxyl ion and peroxideconcentrations within the limits given below and by the choice of thevmost advantageous time and temperature for ide. We have found that a hydroxyl ion concentration within a certain upper and lower limit should be employed in the practice of the invention. should have as its lower limit a pH of about 7.5; and as itsupper limit a, pH of about 13, While .the foregoing represents the lower and upper limits of hydroxyl ion concentrations to be emrug with an aqueous solution containing hydroxyl ions and peroxide as hereindescribed on the other hand apparently does not destroy the epithelial scales or attack the fiber directly, thus eliminating the disadvantages attending the destructive action on the pile itself. We are unable to state definitely the reasons for the improved results obtained by the use of the herein described process, but it would appear that the reaction taking place is a very limited one which tends to change the imbricated surface of the fiplo'yed, we have found that in the practice of the invention there appears to be an optimum inner range, having as its lower limit a pH of about 10 and as its upper limit a. pH of about 12.5.

Substantially no sheening occurs at pH values below about 7.5 even iwith large concentrations of peroxide.

i'de, near the upper 1 it of peroxide concentraher to a relatively smooth surface which has an increased tendency to reflect directly rather than scatter light rays. In this way the desired sheen is imparted to ,the fabric. It is to be understood, however, that our invention is not limited to any particular hypothesis as to the mechanism of the process.

As indicatedabove the difficulties encountered in producing or enhancing the sheen on wool rugs are more pronounced with certain weights of rug and colors than with others. An improved process for sheening the pile of wool rugs which involves a two-stage treatment comprising treating the fabric for a limited period of time with a dilute caustic solution and thereafter .be used to better advantage on (1) rugs having a natural wool (undyed) ,background because of the fact that any hypochlorite treatment tends to some extent to discolor the undyed wool, thereby altering slightly the-color of the rug; (2)

rugsdyed a very light shade of color in which the pH of the treating solution is at least 7.5 but below about 10. It is more economical to use a treating solution having-a pH of at least 10 or higher because more reasonable concentrations of peroxide are elfective at such pH values. The alkalinity of the treating solution produces deleterious effects on the pile when pH values substantially exceed the upper limit of about 13. Thus, at such high pH values the pile tends to become untwisted and the rug'is rendered fuzzy and'difllcult to shear. The color of a rug is also adversely affected by too high an alkalinity, green rugs for example becoming increasingly yellow. It is advantageous, however, to use as high a pH as is consistent with the texture and color of the rug being treated because the re quiredeffectiveconcentration of peroxide, which is relatively expensive with respect to the hydroxyl ion forming material, is lower at relatively high pH' values. With a given quantity of peroxide, s'heening is more pronounced as the'pH increases to about 12.5. We prefer, therefore, to

operate in a pH range between about 10 and attain the most effective about 12.5 in order to and economical results. 7 n

The alkalinity of the treating solution generally decreases during the sheening operation so that an initial pH of about 7.5 to 10 may decrease to a value below 7.5 and even decrease to the acid side during the sheening operation, under which latter conditions little or no sheening takes place.

We have found it to be advantageous to buffer g the treating solution'where its initial pH'is be- The aqueous solution employed Conside able quantities of perox- I tween about 7.5 and in order to obtain maximum sheening eflectiveness. We have found in.

actual practice that a bufiered treating solution having an initial pH of 8.0 drifted only to a pH of 7.55 during the treatment and that wholly eflective sheening was thus obtained. Any compound capable of acting as a butler in analkaline solution and inert ,with respect to peroxide may be used. Acetic acid and a NaaI-IPO4-KH2PO4 mixture are examples of buffers which may be used with advantage in accordance with our inthe, peroxygen group, O2e-, contained in the amount of the peroxygen compound used. By reference herein and in the appended claims to the concentration of the peroxygen compound .in terms of the equivalent of the peroxygen group, or to the peroxygen group concentration, we do not intend to indicate that either the particular peroxygen compound or the peroxygen group is present, as such, in the solution in the specified concentration. It will be understood that in thus defining the concentration of the peroxygen compound in the solution, we include all of the peroxygen group present and capable of reaction whether atany given instance it be in the form ascasea of the peroxygencompound, peroxide ion, hydrogen peroxide, .or in any other form. By thus defining the concentration of the peroxygen comsuch as whether the peroxygen compound is pre'sent, as such, or reacts in the form of an ion or, in the case of a salt, the extent of hydrolysis at any given timeor the degree of ionization. of hydrogen peroxide which may be produced by such hydrolysis.

As above defined, oxygen compound in the treating solution of the invention should be equivalent to a concentration of the peroxygen group, -Oz, falling within an outer range of about 0.14" gram per liter to not more than about 2.8 grams per liter. We have found that there is a preferred inner range adapted to give a maximum sheen with minimum color change and pile degradation in the case of tions in which the peroxygen group, concentration range is from about 0.55 gram per liter to about 2.2 gramsper liter. The outer range corresponds to about 0.5 to 10 grams perliter of 100 volume hydrogen peroxide" solution, while the inner range corresponds to about 2 to 8 grams per liter of 100 volume hydrogen peroxide" solution. The designation 100 volume peroxide is used in the trade to indicate that one volume of the aqueous solution employed is capable of liberating 100 volumes of oxygen. Such a solution is approximately 27-28% hydrogen peroxide, H202, by 'weight. In cases where per salts or other sources of peroxide are useddirectly, the limits of hydroxyl and peroxygen group concentrations should also be within the the concentration of the per- In general it may be said that best results are' drogen peroxide).

some rugs.

ing a peroxygen group concentration below about 0.55 gram per liter (about 2 grams per liter of IOU-volume hydrogen peroxide) it is necessary to use a relatively high concentration of hydroxyl ions in order to obtain satisfactory results.

Hence, we prefer to use a minimum of about 0.55

gram per liter of the peroxygen group even though in some cases a peroxygen group concentration as low as 0.14 gram per liter may serve. Relatively large concentrations of the peroxygen compound are required, to obtain good sheening, in treating solutions having a pH value within 'the lower portion of the permissible pH range. However, concentrations of the peroxygen group higher than about 2.8 grams per liter (about 10 grams per liter of 100-volumehydrogen peroxide) tend to aflect adversely the texture and color of We prefer to use treating solutions containing not more than about 2.2 grams per liter of the peroxygen group (about 8 grams per liter of 100-volume hydrogen peroxide), peroxygen group concentrations approximating this preferred upper limit being'capable of effecting satisfactory sheening without adverse action on sensitive colors in treating. solutions having pH values approaching the lower limit of the per-- missible pH range. The temperature of the solution during treatment is advantageously maintained between about and about 120 F., but as in the case of the concentrations of the reactants the temperature value giving the maximum sheen with the minimum of harmful efiects'must be determined for each particular type and color of rug.

obtained by operating at approximately room temperature, 1. e. within the range to 95 F.

, a number of types of rugs 'when treated in solulimits just stated. In certain instances, it is desirable to maintain a hydroxyl ion concentration in excess of that provided by hydrolysis of an alkaline peroxide or per salt where such material is used as the-source of the peroxygen group. This may be accomplished by adding the necessary quantity of an alkali metal hydroxide, but

With certain types and colors, however, varia-' tions within this restricted range produce undesirable results. For example, one sample of green rug tested acquired an excellent sheen without harm to the color or pile when treated for 45 minutes ina solution at 65 F., whereas a similar sample when treated at F. suffered a color change. In the case of a blue rug treated at the same two temperatures, however, the sample had of varying the time of treatment, it was found that on one specific type of .rug, and using a solution having a sodium hydroxide concentration of 2.5 g. p. l. and a peroxygen group concentration (supplied by H202) of 0.75 g. p. 1., a change in reaction time from 30 minutes to 60 minutes had no visible effect on the results. When, however, solutions having a sodiumhythe total hydroxyl ion concentrationfincluding With treating solutions havthe same rug, an increase in treating time from 30 minutes to 60 minutes improved both the sheen and the pile.

After treatment with an aqueous solution can- -tainlng hydroxyl ions and a peroxygen compound,

the rug is with advantage drained and then rinsed with water at approximately room temperature. Que or two water rinses may be desirable. The rug may then be given a sour" treatment for about minutes with any appropriate acid solution such as a solution containing 2 cc. per" liter formic acid. The rug should then be dried at a moderate temperature, for example at 140 F.

We have also found that with many types of rug marked advantages result from the addi= tional incorporation in the treating solutions of a synthetic organic water-soluble detergent or wetting agent, referred to herein as detergents,

- selected from the class consisting of higher organic sulfates, 'sulfonates and quaternary ammonium compounds free of fatty acid ester substituents. With certain types of rug, for esaznple, a treatment with an alkaline peroxide solution containing such a synthetic organic detergent results in an increased sheen compared to that obtatined with the same solution not containing the detergent without materially affecting the pile or color. In several instances, we have found that the sheen is not only better but the condition of the pile is also much better. The

I presence of such a synthetic organic detergent in the alkaline peroxide treating solutions also gives markedly improved results over the treat-- ing solutions without the detergent when applied to rugs having a weak pile, and particularly when the treatment is carried out in a, washwheel.

The detergent or wetting agent to be employed is preferably a sulfated, sulfonated or quaternary ammonium higher organic compound and must be one which is not affected by alkali within the concentration range and under the conditions of the process. -It must be free of fatty acid ester substituents which in an alkaline solution such as is here used would undergo reaction to form ordinary alkali soaps which are difficult to remove from the fabric and would be deposited in the pile as fatty acids during the usually employed acid souring treatment. As

examples of satisfactory higher organic sulfates,

sulfonates and quaternary ammonium compounds may be mentioned the primary aliphatic sulfates (alcohol esters) such as sodium lauryl sulfate, sodium oleyl sulfate and sodium stearyl sulfate, sulfonates of alkylated benzene such as sodium decyl benzene sulfonate and sodium dodecyl benzene sulfonate, the dialkyl esters, diamyl and dioctyl for example, of sodium sulfosuccinic acid, sulfonates of higheraliphatic hydrocarbons such as sodium hexadecyl sulfonate, the secondary aliphatic sulfates (alcohol esters) such as sodium-2 methyl pentane-4 sulfate, and related compounds known to the industry under the trade name of Tergitols, and quaternary ammonium compounds such as trimethyl octyl ammonium chloride, for example. It is to be understood that other compounds than those just mentioned are suitable provided they are higher organic sulfates, sulfonates or quaternary ammonium compounds free of fatty acid ester substituents. Other detergents or wetting agents such as sodium boro cetyl sulfate, sodium dimethyl dodecyl sulfate, sodium sulfoethyl methyl oleylamide and sodium amyl naphthalene sulfodz-oxide concentration of 3.5 g. p. l. were used on nate may also be used advantageously. It will also be apparent that mixtures of such detergents or wetting agents or compositions consisting essentially of one or more of such detergents a or wetting agents may also be used in the process. Sodium lauryl sulfate, sodium oleyl sulfate and sodium sulfonates of alkylated benzenes including sodium decyl benzene sulfonate and so- 7 dium dodecyl benzene sulfonate have been found 10; to be of particular advantage.

The requirements as to peroxygen compound but the concentration may advantageously be within the range 0.1 to 1.0 gram per liter. More is generally not deleterious. In most cases a dego tergent concentration within the range 0.1 to 0.5'

gram per liter will serve to produce the aforementioned improved results. Any variation in the pH of the treating solution caused by the addition of the detergent should be compensated for 9,5 to produce a treating solution having a pH within the specified range in accordance with our invention.

The following specific examples will serv to illustrate the process of the invention, but are notv so to be considered as in any way limiting the scope of the invention. The rugs used in these examples were manufactured by a commercial rug manufacturer, and were cut into 6-inch square pieces for testing under varying conditions.

Example I A Wilton rug having a blue color and of medium weight was treated in a washwheel as follows. The treating solution consisted of 3 liters do of solution made up from 10.5 g. NaOI-I (3.5 g. p. l.) and 6.6 g. of 100 volume H202 solution (2.2 g. p. 1.). This solution had a pH of about 11.5. The rug was treated for minutes at a temperature of 60 F. The rug was then rinsed for 5 minutes in water at 90 F., following which it was treated for 10 minutes in a solution containing 2 cc. per liter formic acid. The rug was removed from the solution and dried at 140 F.,

after which it possessed a'high degree of sheen, unchanged color, and good pile characteristics.

Example II A rug sample having a green color, but otherv wise similar to that used in the preceding example was treated for 60 minutes at '75 F. in a solution made up from 3.5 g. p. 1. NaOH and 2.9 g. p. l. 100 volume H202. The pH of this solution was 12.3. After rinsing, souring and drying, the rug possessed a very good sheen, unchanged color and 60 good pile.

Example III A similar green rug was treated for 60 minutes at 75 F. in a solution made up from 3.5 g. p. 1.

. NazOz. Th pH of the resulting solution was 12.3.

A rug sample having a green color was treated.

Example V A solution formed by dissolving 3.6 grams of sodium perborate per liter of water was found to have a pH 01 10.2. When used according to the treatment described in Example 11, an excellent sheen was obtained on a sand-colored rug.

color and good. pile characteristics. Increasing Example VI We dissolved 11.3 grams of sodium perborate per liter of water (2.5 grams per liter of the peroxygen group) and adjusted the pH of portions of this solution by the addition of acetic acid. sheening was obtained with the portions of the solution having initial pH values of 9.5, 9.0, 8.5 and 8.0, but no sheening took place with a portion of the solution having an initial pH of 7.0. A sample of rug similar to that in Example V was used for treatment with each portion of the "solution, and each sample of rug was treated at 75 F. for 60 minutes.

Example VII We found that sheening of a sand-colored rug was obtained with solutions made up from 2.8

.grams per liter of'100-volume hydrogen peroxide (0.77 gram per liter of the peroxygen group) and having initial pH values of 10.0 and 11.0 obtained by the addition of sodium hydroxide. Treatment was carried out at 75 F. for a period of 1 hour witheach solution.

, Example VIII A solution made up from 8 grams per liter of V 100-volume hydrogen peroxide was adjusted to a pH of 8.0 with sodium hydroxide and was bullered by a NazHiPOi-KHzPOr mixture. This buifered solution provided a good sheen to a sample of sand-colored rug during a 1 hour treatment at 75 F. A similar solution'having the same peroxide concentration and similar initial pH but not buffered was used for the treatment of another sample of the same rug. The pilot the 'unbuffered solution decreased to about 4 to 5 by the end of the treatment period and resulted in less eflective sheening than the buffered solution.

Example IX A Wilton rug having a green color and of medium weight placed in a treating solution in a washwheel, the solution consisting of 3 liters of aqueous solution made up from 3.5 g; p. l. NaOH,

' 2.9 g. p. l. of 100 volume H202 solution, and 0.25

g. p. 1. sodium dodecyl bcnzenesulfonate. The

pH of this solution approximated 12.0. The treatment was continued for minutes at a temperature'of F. l The rugwas then rinsed for 5 minutes in water at F., following which it was treated for 10 minutes in a solution containing 2 cc. per liter of formic acid. The mg was removed from the solution and dried at 140 A rug sample similar to that used in Example IX was treated in the same way with a solution made up from 3.5 g. p. l. NaOH, 2.9 g. p. l. of

volume H202 solution, and 0.125 g. p. l. of sodium; lauryl sulfate, the pH of the solution being about 12.3. After rinsing, souring and drying, the rug possessed a high degree of sheen, unchanged the detergent composition to 0.25 g. p. l. gave identical results, but detergent concentrations upward or about 0.5 g. p. l. were somewhat less desirable thoughefl'ective. v

This application isa continuation-in-part of our applications Serial Nos. 310,574 and 310,576, .both filed on December 22, 1939.

We claim: 1. The method of sheening the pile of wool rugs which comprises subjecting the pile to'treatment in an aqueous solution containing hydroxyl 2. The method of sheening the pile of wool rugs which comprises subjecting the pile to treat ment in an aqueous solution containing hydroxyl ions and a peroxygen compound, the concentration of the said compound in the solution being equivalent to not less than about 0.55 nor more than about 2.2 grams of the peroxygen group, O2--, per liter and the pHof the solution being between about 10.. and 12.5.

3. The method of sheening the pile of wool ru s which comprises subjecting the pile to treat-; ment in an aqueous solution containing hydroxyl ions and a peroxygen compound, the concentration of said compound in the solution being equivalent to approximately 2.2 grams of the peroxygen group, O2, per literand the pH of the solution being between about 7.5 and 13.

4. The method of sheening the pile of wool rugs which comprises subjecting the pile to treatment in an aqueous solution of ,an alkali metal hydroxide and hydrogen peroxide, the concentration of the hydrogen peroxide gin the solution being equivalent to not less than about 0.14 nor more thanabout 2.8 grams of the peroxygen group, --O2.-, per liter and the pH of the solution being between about 7.5 and 13.

5. The method of sheening the pile of woolrugs which comprises subjecting the pil to treatment in an aqueous solution or sodium hydroxide and hydrogen peroxide, the concentration of the hydrogen peroxide in the solution being equivalent to not less than about 0.14 nor more than about 2.8 grams of the peroxygen group, -02, per liter and the pH of the solution being between about 7.5 and 13.

6. The method of sheening the pile of wool rugs which comprises subjecting the pile to treatment in an aqueous solution of an alkali metal peroxide, the concentration of the said peroxide in the solution being equivalent to not less than about 0.14 nor more than about 2.8 grams of the peroxygen group, -O2-, per liter and the pH of the solution being between about 7.5 and 13.

7. The method of sheening the pile of wool rugs which comprises subjecting the pile to treatment in an aqueous solution of sodium perborate, the concentration of the sodium perborate in the solution being equivalent to not less than about 0.14 nor more than about 2.8 grams of the perox' ygen group O2-, per liter and the pH of the solution being between about 7.5 and 13.

8. The method of sheening the pile of wood rugs which comprises subjecting the pile to treatment in an aqueous solution containing hydroxyl ions and a peroxygen compound, the concentration of said compound in the solution being eq val nt to not less than about 0.14 nor more than about 2.8 grains of the peroxygen group, -Oa, per liter and the pH of the solution being between about LB-and 13, the solution further containing a bufier material adapted to maintain a pHfof the solution within said pH range during treatment of'the pile.

9. The method of sheening the pile of wool rugs which comprises subjecting the pile to treatment in an aqueous solution containing hydroxyl ions and a peroxygen compound, the concentra-- tion of said compound in the solution being 1 equivalent to not less than about 0.14 nor more than about 2.8 grams of the peroxygen group, --Oz-, per liter and the pH of the solution being between about and 12.5.

10. The method of sheening the pile of wool ment in an aqueous solution containing hydroxyl ions, 2. peroxygen compound and a synthetic organic water-soluble detergent selected from the class consisting of higher organic sulfates, sulfonates and quaternary ammonium compounds ire of fatty acid ester substituents, the concentration of the'said peroxygen compound in the solution being equivalent to not less than about 0.14 nor more than about 2.8 grams of the peroxygen group, -'02, per liter, the pH being be tween about 7.5 and 13, and thedetergent concentration being between about 0.1 and 1.0 gram per liter.

11. The method of sheenin the pile of wool rugs which comprises subjecting the pile to treatment in an aqueous solution containing hydroxyl ions, a peroxygen compound and a synthetic organic water-soluble'detergent selected from the class consisting of higher organic sulfates, su1.-

. lent to not less than aboutolt nor more than ment in an aqueous solution of sodium hydroxrugs which comprises subjecting the pile to treatide, hydrogen peroxide and sodium lauryl sulfate,

the concentration of the hydrogen peroxide in the solution being equivalent to approximately 0.75 gram of the peroxygen group, -O2l-, per liter, the pH of the solution approximating 12.3 and the sodium lauryl sulfate concentration being between about 0.1 and 1.0-gram per liter.

14. The method of sheening the pile of wool rugs which comprises subjecting the pile to treatment in an aqueous solution of sodium hydrox. ide, hydrogen peroxide and a sulfonate of an alkylated benzene free of fatty acid ester substituents, the concentration of the hydrogen perox ide in the solution being equivalent to approxi' mately 0.75 gram of the peroxygen group, -O2- tration of said peroxygen compound in the solution being equivalent to not less than about 0.55

nor more than about 2.2 grams of the peroxygen 'ment in an aqueous solution of sodium hydroxide,

hydrogen peroxide and a synthetic organic water soluble detergent selected from the class consist ing of higher organic sulfates, sulfonates and quaternary ammonium compounds free of fatty acid ester substituents, the concentration of the and 1.0 gram per liter.

hydrogen peroxide in the solution being equiva-i.

per liter, the pH of the solution approximating 12.3 and the benzene sulfonate concentration be-.

ing between about 0.1 and 1.0 gram per liter.

15. The method or sheenin the pile of wool rugs which comprises subjecting the pile to treatment in an aqueous solution of sodium peroxide and a synthetic organic water-soluble detergent selected from the class consisting of higher or.- ganic sulfates, sulfonates and quaternary ammonium compounds free of fatty acid ester substituents, the concentration of said peroxide in the solution being equivalent to not less than about 0.14 nor more than about 2.8 grams of the peroxv y en group, O2, per liter, the pH of the solution being between about 7.5 and 13 and the detergent concentration being between about 0.1 and 1.0 gram per liter.

16. The method of sheening the'pile of wool rugs which comprises subjecting the pile to treatment in an aqueous solution containing hydroxyl ions, 9. peroxygen compound and sodium 'oleyl sulfate, the concentration of the said compound in the solution being equivalent to not less than about 0.14 nor more than about 2.8 grams of the peroxygen group, O2-, per liter, the pH being between about 7.5 and 13 and the sodium oleyl sulfate concentration being between about 0.1

JAMES DOUGLAS 'MACMAHON. LORENZO n. TAYLOR.