US2692238A - Wash and rinse composition for whitening and brightening nylon - Google Patents

Description

Patented Oct. 19, 1954 game WASH AND RINSE COMPOSITION FOR WHITENING AND BRIGHTENING NYLON Palmer G. Hendrix, Hickory, N. 6., assignor, by mesne assignments, to Pro-Nyl Chemicals, Inc., Salisbury, N. 0., a corporation of North Carolina No Drawing. Application March 9, 1954, Serial No. 415,149

17 Claims.

This invention relates to a new textile whitening and brightening wash and rinse composition and is more particularly concerned with a new whitening and brightening Wash and rinse composition especially adapted for household use in the washing and rinsing of nylon textile goods, such as stockings and clothing of all inds, as well as many other manufactured nylon textile goods found in the home.

The undesirable yellowish cast and dull appearance developed in white as well as dyed nylon fabrics over a period of time has been a bane of the housewifes existence. The yellowish or off-white tint is aggravated by continued exposure to light, weathering and continued laundering. Securing and simple bleaching are not effective to whiten and brighten nylon.

In recent years, workers in the art have developed so-called optical bleaching and bright ening agents to solve this problem. Actually, these known optical brighteners are not bleaching agents in the true sense of the word because their use is predicated on the fact that they are fluorescent and capable of emitting blue light. Therefore, instead of employing a blue coloring material to absorb yellow light, which is in fact created by blue light being absorbed on the fabric, these new optical brighteners effectively destroy the yellowing elfect by emitting the "lost blue light.

As far as is presently known all of the compositions on the open market today employing optical brighteners of the foregoing character are compounded with a soap or other detergent. However, when these brighteners are combined with a soap or detergent, and this can be demonstrated and proven by test data, they have very little effect on nylon. For some unknown reason, when the brightener has heretofore been compounded with a soap or detergent, it has had very little if any affinity for the nylon cloth and will not remain on the cloth.

One method of utilizing optical brighteners for nylon is disclosed in my prior patent No.

2,619,470, wherein a rinse composition is disclosed utilizing a particular brightener so treated as to have an aflinity for nylon. I later discovered additional means and methods of utilizing optical brighteners in a rinse composition which methods and means are fully disclosed in my co-pending application Serial Number 321,939 for Improved Textile Whitening and Brightening Rinse Composition, filed November 21, 1952.

It is therefore the primary object of this invention to provide a composition utilizing any one of several optical brighteners combined with a soap or synthetic detergent in such a manner as to cause the brightener to adhere to nylon fabric.

It is another object of this invention to utilize optical brighteners other than the brightener disclosed in my prior patent and prior application, and to form a composition of such brighteners Or any one of them which may be used as a rinse or which may be combined with a soap or synthetic detergent and wherein the brighteners will be caused to adhere to nylon fabrics.

It is still another object of the invention to provide a concentrated whitening and brightening rinse and Wash composition for household use which has extremely good brightening and whitening effect on nylon fabrics, whether they be dyed or undyed.

In my prior patent No. 2,619,470, it was disclosed that a particular brightener 3,7-dianisoylamido dibenzothiophenesulfone 2,8 sulfonic acid (or its sodium salt) could be combined with at least 20% tertiary butyl alcohol for an eifective nylon rinse composition and that this brightener could also be rendered effective for nylon by use of other alcohols, though with certain limitations as to shelf life.

In my said co-pending application, Serial Number 321,939, it was disclosed that by the use of sulphuric acid, these other alcohols could be utilized with good results. In said prior composition it was necessary to use at least 20% alcohol to achieve desire results.

It has now been discovered, in accordance with the present invention, that by adding a soap or detergent to the composition of my prior patent and co-pending application, a much smaller amount of alcohol may be used with the desired results.

Heretofore the use of optical brighteners with soap or detergents has not been effective but by employing alcohols as herein provided, the brighteners may be combined with a soap or a detergent with excellent results when used in the wash.

It has been further discovered that additional optical brighteners may be used in a rinse or wash composition in lieu of 01' in addition to said 1 3.7-dianisoylamido dibenzothiophenesulfone-2,8- sulfonic acid. These additional brighteners are selected from the generic class of amino cumarins embraced within the formula:

mercially .as .fBlancophor A. W. ,by General Dyestuff Corporation, and p. dimethyl amino- ,3- methyl cumarin, sold commercially as Calcofiuor White R. W. by American Cyanamid Company. These additional brighteners may be used as set forth in said patent and said application .as .an effective rinse composition and by the addition of a soap or detergent any one of said brighteners or a combination of the same may be used as an efiective nylon laundering or Wash composition in the manner more fully disclosed herein.

The present invention is predicated, in part, therefore, on the provision of a concentrated whitening and brightening rinse containing four ingredients: (1) Any one of the foregoing organic optical brighteners or a combination thereof found vastly superior for use in rinsing nylon suspended in (2) an aqueous medium containing at least 20% of a simple .monohydric alcohol, (with the exception of tertiary butyl alcohol where acid is necessary), (3), a mineral acid, such as sulphuric acid, hydrochloric acid or phosphoric acid, preferably of 66% strength, to .render the suspension stable, and (4) a small amount of hydroscopic agent, such as polyhydric alcohol. As a wash composition it has the additional ingredient of (5) a soap or synthetic detergent. The optical brighteners, the particular suspending medium, and the acid are essential. Here again, as pointed out in my said co-pending application, the sulphuric acid is not necessary when employing tertiary butyl alcohol. Sulphuric acid is necessary only with the other lower alcohols. The hygroscopic agent is optional but desirable.

In the concentrated rinse composition of the present invention the simple .monohydrio alcohol may be methyl alcohol, ethyl alcohol, propyl .alcohol, isopropyl alcohol, butyl alcohol, tertiary butyl alcohol, or isobutyl alcohol, or any .mixture thereof, it being pointed out again that the monohydric alcoho1 content of the concentrated rinse being at least of the total in the concentrated rinse so that a good suspension may be obtained in the ultimate dilute rinse. When employed as a wash composition by the addithe building up of static electricity in the rinsed and dried nylon goods.

The following specific rinse compositions are given by way of illustration:

Example 1 1 ozs. of p. di methyl amino beta methyl cumarm 3 lbs. of tertiary butyl alcohol 1 ozs. of glycerine balance Water to give a total of 8 lbs.

Example 2 1 /2 ozs. of p. diethyl amino cumarin 3 lbs. of tertiary butyl alcohol 1% ozs. 0f glycerine balance water to give a total of 8 lbs.

Example 3 1 ozs. of sulphuric acid 1 /2.ozs. of water 4 1. ms. of ,p. di methyl-amino beta .methyl cu- 'm'arin All mixed together to form a paste. Then 3 lbs. of ethyl alcohol and 1 ozs. of glycerine are added, plus a balance of Water to give a total of 8.1bs.

Example 4 A composition is compounded in the same manner and with the same ingredients in the same amounts of Example 3 except that hydrochloric acid is substituted for sulphuric acid.

Example 5 amounts of example 3 except that isopropyl alcohol is substituted for ethyl alcohol.

Example 7 1 ozs. of sulphuric acid 1. ozs. of water 1 ozs. of p. diethyl amino cumarin All mixed together to form a paste. Then 3 lbs. of ethyl alcohol and 1 ozs. of glycerine are added, plus a balance of water to give a total of 8 lbs.

As indicated above, any of the various abovedisclosed monohydric and polyhydric alcohols could be substituted for the ethyl alcohol and glycerine, respectively, in the foregoing formulas No. 3 and No. 7. Also, the amount of ethyl alcohol could be reduced to about 2 lbs, but not much further, because the 'monohydric alcohol content must be at least 20% of the concentrated rinse suspension. The monohydric alcohol content could be higher, say 40 to.50'% but this would be undesirable from an economic standpoint.

The amount of optical brightener in the concentrated rinse composition can be varied between 0.1% and 6.0%, although best results are obtained when employing 0.5% to 1.5%.

If desired, a plurality of optical brighteners may be combined in any of the foregoing formulas to give a total of 1 /2 ozs. of brightener in each formula. Also, one of the other optical brighteners disclosed herein may be combined with 3,7- dianisoylamido dibenzothiophenesulfone-2,8 sulfonic acid, or any of said brighteners may be combined or intermixed. The total amount of brighteners can vary between 0.1% and 6.0% as above stated. The 'brighteners disclosed are substantial equivalents insofar as their affinity to nylon is concerned. However, they have varied characteristics with respect to other fabrics. For this reason, it is frequently desirable to combine one or more of the brighteners as stated, although they may be used independently (according to this invention) with excellent results on nylon or nylon garments.

The amount-of sulphuric acid or other mineral acid in the concentrated rinse is generally the same as the amount of optical brightener, but then it may be varied down to 50% of the amount of brightener used. In any instance, however, the amount of water used to make the basic paste should be the same as the amount of acid.

The amount of polyhydric alcohol in the con centrated rinse-composition, when it is employed therein, can be varied between 1.5% and 4.25%.

The foregoing compositions when diluted to the extent necessary for the final rinse, as pointed out hereinafter, are not in any way dangerous or deleterious to the nylon treated in said dilute rinse. However, in some instances, the concentrated rinses of the invention may, because of the presence of sulphuric acid, affect nylon goods deleteriously. Therefore, should a housewife, by mistake, use the concentrated rinse in full strength, there is a possibility, as stated, that the nylon goods may be damaged. In order to obviate this, the composition of the present invention may have added thereto a small amount of household ammonia, in an amount about twice that of the sulphuric acid employed. The addition of ammonia to the composition acts as a buifer so that the concentrated rinse, even when employed in full strength, will not be harmful to nylon goods. The resulting solution is then used in the rinse water just as any of the compositions of the invention.

Another specific example, therefore, would be exactly in accordance with the Examples 3, 4, 5, 6 and 7 above except that three ounces of household ammonia are added to the final eight pound solution.

In use, nylon garments are washed in the usual manner and are then rinsed in a dilute rinse solution containing two tablespoons full of the foregoing formula to each gallon of water. Adequate brightening and whitening effect is obtained in about four or five minutes rinsing time.

It will be found that the suspended solid particles of the optical brightener or brighteners employed will be deposited upon the nylon goods during the rinsing operation and that, after drying, will be held firm by the nylon goods even after repeated washings.

The foregoing compositions may be utilized as washing or laundering compositions by the addition of a soap or synthetic detergent thereto according to this invention.

The following specific wash compositions are given by way of illustration:

Example 8 1 ozs. of 3,7-dianisoylamido dibenzothiophene-sulfone-2,8-su1fonic acid is dissolved in 1 lb. tertiary butyl alcohol, and then added to 5 lbs. 6 /2 ozs. water and intermixed therewith.

Then add 1 lbs. of sodium lauryl sulfate to ive a total of 8 lbs.

Example 9 1 /2 ozs. of p. diethyl amino beta methyl cumarin is dissolved in 1 lb. tertiary butyl alcohol, and then added to 5 lbs. 6 ozs. of water and intermixed therewith. Then add 1% lbs. of sodium isopropyl naphthalene sulfonate to give a total of 8 lbs.

Example 10 1 /2 ozs. of p. diethyl amino cumarin is dissolved in 1 lb. tertiary butyl alcohol, and then added to 5 lbs. 6 ozs. of water and intermixed therewith.

Then add 1 lbs. of sodium dodeeyl benzene sulfonate to give a total of 8 lbs.

Example 11 A composition is compounded in the same manner and with the same ingredients in the same amounts of Example 10 except that potassium oleate is substituted for sodium dodecyl benzene sulfonate.

As indicated above, any of the various abovedisclosed monohydric alcohols could be substituted for the tertiary butyl alcohol in the foregoing formulas 8, 9, 10 and 11 by the addition of sulfuric acid in the manner disclosed in said copending application.

The following specific compositions are given by way of illustration:

Example 12 1% ozs. of sulphuric acid 1 ozs. of water 1 1 ozs. of p. dimethyl amino beta methyl cumari All mixed together to form a paste. Then 1 lb. of ethyl a cohol and 5 lbs., 3 ozs. of water are added and intermixed. Then add 1%; lbs. of sodium salt of 7-ethyl 2 methyl undecanol-4 sulfate to give a total of 8 lbs.

Example 13 A composition is compounded in the same manner and with the same ingredients in the same amounts of Example 12 except that sodium lauryl sulfate is substituted for the sodium salt of 7- ethyl 2 methyl undecanol-4 sulfate.

Example 14 A composition is compounded in the same manner and with the same ingredients in the same amounts of Example 12 except that potassium stearate is substituted for the sodium salt of 7- ethyl 2 methyl undecanol-4 sulfate.

Example 15 A composition is compounded in the same manner and with the same ingredients in the same amounts of Example 12 except that methyl alcohol is substituted for ethyl alcohol.

Example 16 A composition is compounded in the same manner and with the same ingredients in the same amounts of Example 12 except that isopropyl alcohol is substituted for ethyl alcohol and sodium lauryl sulfate is substituted for the sodium salt of 7-ethy1 2 methyl undecanol-4 sulfate.

Example 17 A composition is compounded in the same manner and with the same ingredients in the same amounts of Example 12 except that methyl alcohol is substituted for ethyl alcohol and hydrochloric acid is substituted for sulphuric acid Example 18 A composition is compounded in the same manner and with the same ingredients in the same amounts of Example 12 except that isopropyl alcohol is substituted for ethyl alcohol and sodium isopropyl naphthalene sulfonate is substituted for sodium salt of 7-ethyl 2 methyl undecanol-4 sulfate.

Example 1.9

A composition is compounded in the same manner and with the same ingredients in the same amounts of Example 12 except that isopropyl a1- cohol is substituted for ethyl alcohol and sodium dodecyl benzene sulfonate is substituted for sodium salt of 'l-ethyl 2 methyl undecanol-4 sulfate.

1 /2 ounces 3,7-dianisoylamido dibenzo-thiophenesu1fone-2,8-sulfonic acid or 1 ounces of p. diethyl amino cumarin may be substituted for the p. dimethyl amino beta methyl cumarin in the foregoing formula of Examples 12 through 19.

In any of the foregoing examples wherein sulplated.

P il? assi n;h dro hl ric; sidz si siel t sais a b e sed ls whsto a h s a a ia d. aims a -am u t q irerc ntase o nsrfiq s scl sq er -Wei ht In any of the foregoing formulas-8; through 19,; angyr fi Q P 93M 2???" ynthet c dgf 'F may be substituted for the detergent given. Forexample, any ordinary low titer soap in liquid form, and synthetic detergents such as sulfated fatty aclohols, sodium alkyl aryl sulfonates and the like may be employed.

An 'QQnYen iQ a oap n. liqu f m m y be s dt u h s ot ss um c ea s. sodium eats, oeesium s ra nd. o ium teatai l Qrfmi .2 1 3 3 A159 tem ated 11 29 9 2 o s repar d sim 'sa fy ns ocoa: nut oil-with caustic soda o'r caustic potash. Commercial liquid soaps such as Badger Liquid Soap, Colgate Concentrated Liquid Soap, Big Six, Hi-Jel d' bxs ou may o sed.-

Sodium salts of sulfated fatty v alcohols may also be employed as. detergents. As used. com-1 mercially this type of detergent is usuallya mine. ture of the sodiu nsalts of sulfated fattyalcohols. made by reducing the mixed, fatty acids of cocoanut oil, palm kernel: oil or ofcottonseed oil and of fish. or sperm oils. Sometimes natural waxes such as. spermaceti, Wool fat and beeswax are.

sulfated directly. The. mixture of the sulfated alcohols. which goes by the commercial name lauryl alcoholf consists, of about 15% mixed Cs and C10 (octyl and decyl) alcohols, 40% 012' (lauryl or dodecyl) alcohol, 30% C14 (myristyl or tetradecyl) alcohol and 15% mixed; C1 and Q18 are contemplated, such as. sodiurnlaurylsulfate sodium octyl sulfate, sodium decyl sulfate, sodium dodecyl sulfate, sodium myristyl sulfate, sodium tetradecyl sulfate, sodium cetyl sulfate, sodium stearyl sulfate and sOdium oleyl sulfate.

ypica of t e o in ssv of y thet er ent e: 991 9 G rd io M d na Qrvu Au i i l. Map ofix. T lfsav n. sand pan Tere to Q ol p n. Cxclanoallmft Dr ne a dan and Lissapol.

Alkyl and alkyl aryl sulfonates may also be employed as detergents. The alkyl or alkane sulfcnates may be the sodium salts. of sulfonated higher fatty acids such as those found in cocoa-. nut oil, palm oil, olive oil, etc. This will give rise to sodium salts of sulfonated mixed higher fatty acids, although the sodium salts of sulfonated, preformed individual acids may be employed. Esters of sulpho fatty acids are also contem- (See Bertsch Patent No. 1,918,372.) Likewise amides of the foregoing, such as sulfonated cocoanut oil fatty acid amide, may be used. '(See Bertsch Patent No. 1,918,373.)

The alkyl aryl sulfonates as. used commercially are one or more sodium salts of alkyl, (eithen short or long chain, usually. the latter) benzene or naphthalene sulfonic acids. The allsyl may be lower alkyl, such as methyl, ethyl, propyl, butyl and isopropyl, or it may be and usuallyis a'higher alkyl having from 8 to 18 carbon atoms, such as octyl, nonyl, decyl and lgeryl. 'Ijhese higher alkyls may be derived from the fatty acids of cocoanut oil, palm oil and olive oil, or from a hydrocarbon kerosene fraction contain: ing edomin nt .2. car on. atoms tov h l ul s ooifi a l ma be. ment oned. the s di m alt, of th acid. d ed from ousin henna with. os .or pa sd e .ii

over, in all= of: the.

- 8; raction his ot a ka at c lo de) f 5%. 5 iilm- $QPFQP L narzhthalsn ul x asm. i ly 39M 3 l lf fi l'fi od ....-.ksr n e i qs ta. a odium. do: deeylfbenzene sulfonate.

Q bera s n sa f gs es; hich. m w-ha y d- E Q b WHQ. l i' i le 9.3%? Q1. sur ac Active, nts? by s bw r gronyf (1949 nc ud d. i) he pre o e .33 5 92? re; 1139. a ac e c mmer i detergents; 419%. New 00ml, So a NfiAE s etvm r st l ttaw fs Xynomine may be, employed.

the: mount of dh sms; was ame s: a sefe a as a 9m ii t. t m g s i i ie- 1 as cb; as .0%..

The m u t o Soap e hs ei rs et s. o a nzo e fo olv fa osit a etraat be. as i tl r e $i Oneteaspoon'fullof the concentrate wash co n; position'should be used; witheachgallonofw 11. water and the fabrics are washed and rins usualmannen without the addition of soaps. or detergents or Whitening agents,

be used without harmful results but if more than 5 teaspoonsful per gallon is used, the articlebe ing washed may have anundesirable. bluish tinge.

This application is a continuation-in-part of; application Serial No. 343,813, filednpril 14, 105;), now abandoned. I

What is claimed is;

1. A concentrated; Whitening and brightening rinse composition for. nylon goods consisting essentially. of water having 0.1% to 6.0% of. an amino. cumarin suspended stably therein and containing t m ner l a ia Sa d a it being. of 66% strength and being present in an: amount of from 50% to of the amount of; the. amino cumarin, and; at least.20% of a simple mpnohydric alcohol from the. groupconsisti ofmethyl, ethyl, propyl, isopropyl, butyland so; butylalcohols, said amino cumarin. being; sel ected from the group consisting. of diethyl amino cumarin and p. dimethyl amino. ,B me thyl cumarin. l

2. A concentrated whitening and brightening rinse composition forv nylon goods consisting essentially of Water having 0.1% to. 6.0% of an amino cumarin suspended stably therein and containing 0.1% to 6% mineral acid, saidv acid being of; 66% strength and bei g present in an amount of from 50% to 100% of the amount ofthe amino cumarin, and at least 20% of methyl alcohol, said aminocumarin being selected from the group consisting of p. diethyl amino cumarin me am e fi-m thy Wi ona.

3. A concentrated whiteningand brightening rinse composition for. nylon goods consist essentially of water. having 0.1% to 6.0%. of an amino cumarin suspended stably thereln and containing 0.1% to 6% mineral acid, said acid being of 66% strength and being present in an amount of from 5.0% to 100% of the amount of the amino cumarin, and at least 20 of isopropyl alcohol, said amino cumarin being selected from the group consisting of p. diethyl amino curnarin and 'p. dimethyl amino B-methyl cumarin.

4. A concentrated Whitening and brightening rinse composition for. nylon goods consisting ss nt l a e hav 4% o. 60% o a amino. cumarin suspended stably. therein." onta ni to 6%. m n r sai an a ein o s r gt and. being r in amount of from 50% to 100% of'th e a ount the amino cumarin, and at least of isobutyl alcohol, said amino cumarin being selected from the group consisting of p. diethyl amino cumarin and p. dimethyl amino B-methyl cumarin.

5. A concentrated whitening and brightening rinse composition for nylon goods consisting essentially of water having 0.5% to 1.5% of an amino cumarin suspended stably therein and containing 0.5% to 1.5% mineral acid, said acid being of 66% strength and being present in an amount of from 50% to 100% of the amount of the amino cumarin, at least 20% of a simple monohydric alcohol from the group consisting of methyl, ethyl, propyl, isopropyl, butyl and isobutyl alcohols, and a small amount of a polyhydric alcohol, said amino cumarin being selected from the group consisting of p. diethyl amino cumarin and p. dimethyl amino c-methyl cumarin.

6. A concentrated whitening and brightening rinse composition for nylon goods consisting essentially of water having 0.5% to 1.5% of an amino cumarin suspended stably therein and containing 0.5% to 1.5% mineral acid, said acid being of 66% strength and being present in an amount of from 50% to 100% of the amount of the amino cumarin, at least 20% of a simple monohydric alcohol from the group consisting of methyl, ethyl, propyl, isopropyl, butyl and isobutyl alcohols, 1.5% to 4.25% glycerine and 1.0% to 3.0% household ammonia, said amino cumarin being selected from the group consisting of p. diethyl amino cumarin and p. dimethyl amino c-metnyl cumarin.

7. A concentrated whitening and brightening rinse composition for nylon goods having the following formula:

1 ozs. of an amino cumarin 1 ozs. sulphuric acid (66% strength) 3 lbs. of isopropyl alcohol 1 ozs. of glycerine Balance water to give a total of 8 lbs. said amino cumarin being selected from the group consisting of p. diethyl amino cumarin and p. dimethyl amino 6-methyl cumarin.

3. The composition of claim 1 in which the amino cumarin is p. diethyl amino cumarin.

9. The composition of claim 1 in which the 10 amino cumarin is p. dimethyl amino fi-methyl cumarin.

10. A concentrated whitening and brightening wash composition for nylon goods comprising Water containing 10% to 60% of an anionic dc tergent, 0.1% to 6% of an amino cumarin, 0.1% to 6% of a mineral acid, said acid being of 66% strength and being present in an amount of from to 100% of the amount of the amino cumarin, and at least 4% of a monohydric alcohol from the group consisting of methyl, ethyl, propyl, isopropyl, butyl and isobutyl alcohols, said amino cumarin being selected from the group consisting of p. diethyl amino cumarin and p. dimethyl amino B-methyl cumarin.

11. A concentrated whitening and brightening wash composition for nylon goods comprising water containing 10% to of a sodium salt of a sulfated fatty alcohol, 0.1% to 6.0% of a p. dimethyl amino p-methyl cumarin, 0.1% to 6.0% of a mineral acid, said acid being of 66% strength and being present in an amount of from 50% to of the amount of the amino cumarin, and at least 4% isopropyl alcohol.

12. The composition of claim 10 in which the detergent is a sodium salt of a sulfated fatty alcohol.

13. The composition of claim 10 in which the detergent is sodium isopropyl naphthalene sulfonate.

14. The composition of claim 10 in which the detergent is sodium dodecyl benzene sulfonate.

15. The composition of claim 10 in which the acid is sulphuric acid.

16. The composition of claim 10 in which the amino cumarin is p. diethyl amino cumarin.

17. The composition of claim 10 in which the amino cumarin is p. dimethyl amino ,B-methyl cumarin.

References Cited in the file of this patent UNITED STATES PATENTS Number Name Date 2,333,329 Miglarese Nov. 2, 1943 2,600,375 Ackermann June 17, 1952 2,619,470 Hendrix Nov. 25, 1952 2,643,197 Savidge June 23, 1953 2,654,713 Fleck Oct. 6, 1953

Claims (1)

1. A CONCENTRATED WHITENING AND BRIGHTENING RINSE COMPOSITION FOR NYLON GOODS CONSISTING ESSENTIALLY OF WATER HAVING 0.1% TO 6.0% OF AN AMINO CUMARIN SUSPENDED STABLY THEREIN AND CONTAINING 0.1% TO 6% MINERAL ACID, SAID ACID BEING OF 66% STRENGTH AND BEING PRESENTED IN AN AMOUNT OF FROM 50% TO 100% OF THE AMOUNT OF THE AMINO CUMARIN, AND AT LEAST 20% OF A SIMPLE MONOHYDRIC ALCOHOL FROM THE GROUP CONSISTING OF METHYL, ETHYL, PROPYL, ISOPROPYL, BUTYL AND ISOBUTYL ALCOHOLS, SAID AMINO CUMARIN BEING SELECTED FROM THE GROUP CONSISTING OF P. DIETHYL AMINO CUMARIN AND P. DIAMETHYL AMINO B-METHYL CUMARIN.