AU6093073A - Hair setting process - Google Patents

Description

1.25 1.4 1.6

MICROCOPY RESOLUTION TEST CHART OFSTANDARDS-1963 BUREAU NATIONAL

-I

7h' "THE I ROCTER GAMvBLE COMPANY

IC I of"- 301 East Sixth Street, Cincinnati, Ohio 45202 United States of America

hecreby\ applv for tile grant of a Patent for an invention entitled liii HAI{ SETTING PR(1CES3S"

oitch is described in the accompanying (c specification. complete

(N'ot e: The following paragraph applies on ly to Con venztion applications)

Ulhi. application is a Convent ion application based on the basic application(s) for a patent or simila r protection identified by number, country, and filing date as follows: 294053 United States of Amorica 2nd October, 1972 I ~C II

,\ddrcsv, for Service: 131-IILLIPS ORMONDE AND FITZPATRICK Patent antI Trade Mark Attorneys 37-41 Queen Street Mvelbourne, Australia

Dated (g 2nd October, 1973

()PHILLIPS, 0RIMONDE FITZPATRICK CNot il Attorneys for THE PRO Y"ER GAYI3LB COMPAN~Y ac~

PS, ORMONDE AND FITZPATRICK Patent and Trade Mark Attorneys Melbourne, Australia

COMMON)IALI'II OF AUSTRALIA I'atcritts .4(

I)I~LARAIONFOR A PAI'EN't APPL-ICAION T INSi 11 (1 (iNS

III s'llort of thlc W Convention applicntion made by The 'Procter Gamble Company 2 7

I I hereintifrr cAtte 'apptllicant(s)") for a paitent Wc for an I III I inveit ion entlitled d

HAIR SETTING PROCESS

lMIKKI Dean Pickering Fite 'cc IC. <CIr.; II Vice President of The Procter Gamble Company, of 301 EaIst Sixth Street;, Cincinnati, Ohio, hI United States of America, dIo mol cmCif\ md-, sincerely dleclare as follows:

of tilc apl~licant(s). I :tnmi,",-Yrr authorized to mnake this dleclaraition on bchlt'i

AI

EUGENE ZEFFREN JERRY TURNER 145 Fleming Road 5275 Southgate Blvd. Wyoming, Ohio 45215 Fairfield, Ohio 45014 United States of United States of America, AC America +-,are thle actial inventor(s) the appllicant(s) thie invention and the facts up~on whiichi vra:re enititledl to Imike thleapl)lica-tion are aisfollo0ws: AnP-iCalnt is the assigrtee of the invention from the actiial inventors-

(AN'ulc: 1'o(oi'rrtlp/ts .3 antd 4 rapply only/ to Contention altplic'rifiotts) 3 IVhe basic alpptica"tion(4 fnr Iantent or simlilatr p~rotection on wichl the appIflication is baIsed I II is,e idecntified by country, filing date, and basic applicant(s) ats follows:

Uniited States Serial No. 294,053 filed 2 October 1972; by Eugene Zeffren and Jerry Turner in United States of America

4. 1 bil~l ajpllicotion(,4 referredl to ill patragraph) 3 hecreof wvns/wofo- the first appllication(-g) nimaIc iit ~i nf tile inlvent i~ C'onvyention cot it ry itt respecct t Ieubject Of tile a1pl Cat ionl. Utt

C 'I 5' C

(SIC Declarcc ,It (kt Cincinnati, O~hio, U.S.A. Dted~ (1) November 8, 1973 '0 t110THE PROCTER-.. GAMBLE COMPANY

Dean Pickering/Fit(- Comiimissiotner of PItcnits 1to:'ilte IVice President,

11111.L11S ORMONDE FITZPArTRICK amidl i'rade Motrk At tarneiys Paitenmt Melbourne, Atmstralia

COMMONIVEALT11 OF3 AusTri bIA

Patents Act

COMPLETE SPECIFICATION (ORIGINAL)

Clalss In G4ris,

Application Number: Cqol I Odged: tO1

Comnplete Specification Lodgcd: 4 te -17-5

Published: kr k,

RcLited Art: I r~' 'i k7

APPLICANT'S RI3F.:P&G C;Lse 1907 1111ci ot ApplicatfsJ TfE IROCTER GAI"BLE COMPANY

NLI.\dLC'(C") of Applican 301 Bast Sixth Street, Cincinnati, Ohio 45202, United States of America

m Ins%'nor(s): Eugene Zeffren and Jerry Turner

:OltIklrc, tar Ser\ ic PHI LLIPS, ORNIONDE~ ITIZPATRICK Patent aind Trade MIark Attorneys 37-411 Queen Street Mfelbourne, Aj~ra, 3000 the invenition nuitted: A mu C omplc! e Speciiationl for

0(OC7 1973 "ll'iIR SETT114G lil0'JES3"'

Ih toIh is a fullIdeceription ,I -iement of this in~ ettioni, ineludiktg the best methovd (if pelt rmiing itktO\ n ito applicant(s): v

p DJoc I

I- HAIR SETIING PROCESS

Eugene Zeffren and Jerry Turner

BACKGROUND OF THE INVENTION

This invention relates to a process for deforming

hair. More particularly, the invention discloses processes

and compositions for curlingor straightening human hair employ-

ing monopersulfate oxidizing agents which do not substantially

bleach melanin when employed under the conditions herein-

after disclosed.

Both hot and cold hair curling processes involve

various heat or chemical treatments, or combinations

thereof, to disrupt the keratin structure of the hair.

Following this initial disruption, the hair is subjected

to longitudinal stresses, for example, by winding on a

mandrel, following which the keratin structure is sub-

stantially reestablished with the hair in the curled

configuration. Curling processes employing heat and

caustic solutions are known as "hot" processes,

whereas those employing chemical compounds such as the thioglycolates are known us "cold" processes.

Cold processes have come into general acceptance inasmuch

as they can be utilized by relatively inexperienced

operators in home permanents.

It is recognized in the art that hair which has been exten-

sively bleached, subjected to oxidative conditions where-

by the melanin is substantially destroyed, is relatively easy

to curl or set in a more-or-less permanent configuration

by simply moistening the hair and subjecting it to a

longitudinal stress. Presumably, common hair bleaches

disrupt chemical bonds in keratin fibers with a net effect

similar to that when hair is contacted with a thioglycolate

cold waving solution. Hair in which the

keratin molecules are oxidatively disrupted is thereby rendered

deformable and the hair can then either be curled or straightened,

as desircd. Of course, hair treated with the common hair

bleaches, a basic solution of hydrogen peroxide, is a.

not only more susceptible to curling but also has a different

color due to the action of the bleach on the melanin color

bodies in the hair. For this reason oxidative hair bleaches are not generally considered to be acceptable for curling

hair inasmuch as the user must thereafter tint or dye the

treated hair to reestablish the original hair color. It has now been discovered that a certain class of

oxidizing agents, the monopersulfates, can be applied to

hair to oxidize the chemical bonds in keratin, thereby

rendering the hair deformable without substantial bleaching _f the natural hair color. It is surprising that the monopersulfates are capable of disrupting the keratin fibers without attendant bleaching, inasmuch as these compounds are well-known as bleaches for syntnetic fibers.

Presumably, the kinds of stains which can be bleached from

fabrics and fibers are sufficiently different from the

melanin coloration of the hair that the monopersulfates, while

capable of bleaching such stains, have no substantial effect on

melanin. In any event, it has now been found that monopersulfates

can be applied to hair to cause sufficient disruption of the

keratin fibers to allow the deformation of the hair by applying

a longitudinal stress thereto, but without changing the natural

hair color.

The use of per-salts, including persulfates and monoper-

sulfates in the neutralizing solution of hair waving compositions

is known in the art; see, for example, U.S. Patent 3,583,408 and

ELCHEM 1384 Catalog, DuPont. When employed as neutralizers, such

per-salts are commonly used in the acid pH range following the

thioglycolate treatment to reestablish the sulfur-sulfur bonds in

the keratin fiber, whereas by the present process it has been

discovered that monopersulfates can be employed to disrupt keratir

bonds. U.S. Patent 3,679,347 teaches the use of monopersulfates in

hair dyeing processes, but does not suggest their use for

deforming hair in the manner of this invention.

The concurrently filed application of J. A. Anderson,

entitled "Hair Setting Process", Serial No. filed

P&G Attorney's Docket No.1908 discloses hair curling

processes employing monoporsulfates and certain chelating agents.

It is an object of the present invention to provide a method for deforming keratin fibers, especially human hair, by means of monopersulfate oxidizing agents without substantial hair bleaching.

It is a further object herein to provide a method for

curling hair b- means of monopersulfate oxidants. These and

other objects are obtained herein as will be seen by the

following disclosure.

SUMMARY OF THE INVENTION The instant invention encompasses a process for deforming

hair comprising contacting said hair with an effective amount, i.e.,

an amount sufficient to thoroughly wet the hair, of an aqueous

solution comprising from about 1% to about 20% by weight of an oxidant

of the foimula MHSO 5 wherein M is an alkali metal cation, the pH

of said treatment solution being in the range from about 5 to about

11. The hair is treated with the solution of the MHSO 5 oxidant for

a period from about 1 to about 30 minutes, following which the

oxidant is removed by a water rinse or shampoo; the moist, treated a

hair is subjected to a longitudinal stress to achieve any desired a

configuration. For example, the wet hair can be w;ound on a mandrel

9p. and allowed to dry on the mandrel, thereby achieving a curled effect.

Alternatively, the wet hair can be fashioned into a straight configu-

ration and allowed to dry, thereby resulting in hair straightening. S In an alternate mode, the hair can be subjected to a longitudinal

S stress during treatment with the oxidant, rinsed, and allowed to dry in the stressed configuration. Again, curling or straightening,

Sas desired, is thereby obtained. DETAILED DESCRIPTION OF THE INVENTION The oxidizing agents used in the present process are water-

soluble monopersulfate salts of the formula MISO 5 wherein M is an

alkali metal cation, lithium, sodium, potassium, rubidium or cesium. The nature of the alkali metal cation is of no import to the present invention inasmuch as all such salts are water- soluble and it is the monopersulfate anion which is the active oxidizing species in solution. However, the monopersulfate salts wherein M is potassium are available from E. I. DuPont de Nemours Co. under the trade name OXONE and are preferred herein because of this commercial availability. The other alkali metal monopersulfate salts can be prepared, for example, by ion exchange reactions with the potassium salt or by neutralization of the corresponding acid with the appropriate alkali metal hydroxide.

The foregoing monopersulfate salts are employed in the

present process as aqueous solutions containing from about 1% to

about 20%, preferably 2% to about 10%, by weight of said mono-

persulfate salt. The piH of the aqucous monopersulfate

solutions used herein is adjusted to within the range from

about 5 to about 11. Solution pH's greater than 11 can be

S. used; however, such high pH's are unduly irritating to normal

skin and are preferably avoided. A solution pH of about 7.0-9.5

is preferred. Solution pH's within the desired range can be

established by dissolving the monopersulfate salt in water and

adding sufficient base, alkali metal hydroxide, ammonium

hydroxide, or organic base such as diethanolamine, triethanol-

amine and the like, to the solution until the desired pH within

the specified range is obtained. However, it has been dis-

covered that the pH of such solutions normally will change to

the acid range when applied to the hair. Accordingly,

it is preferred that a buffer be employed in the aqueous

solution of monopersulfate to keep the pll within the range of about 5 to about 11. Any of the common organic and inorganic buffer salt combinations capable of establishing a pH within this range are suitable for use in conjunction with the monopersulfate salts. Exemplary buffers suitable for use herein include, for example, the sodium hydroxide sodium borate; sodium hydrogen phosphate potassium dihydrogen phosphate; sodium borate hydrochloric acid; and phosphate buffers prepared in the manner fully described in

"Hawks Physiological Chemistry", Oser, Ed. 14, pps. 41-43, McGraw-Hill (1965).

As noted hereinabove, it is necessary that the mono-

persulfate salt in contact with the hair be maintained at a

pH in a range from about 5 to about 11 to provide the desired

hair deformation. While any of the common buffers suitable for use in this pH range can be employed for this purpose, it

has been discovered that carbonate-bicarbonate buffers are

most preferred herein. Presumably, carbonate-bicarbonate

buffer mixtures employed in conjunction with the alkali metal

monopersulfates serve both as a pH buffer and, in some

way, promote the softening of the hair or otherwise

allow the monopersulfate to interact with the keratin in

an optimal fashion. Irrespective of the actual mechanism, it

has been found that compositions employing the monopersulfate

salt dissolved in aqueous carbonate-bicarbonate buffers at a pH

in the range from 5 to 11, preferably 7.0-9.5, are preferred for use herein. Accordingly, aqueous solutions comprising from about to 20% by weight of the alkali metal monoperulat 1% to 'i 4 20% by weight of the alkali metal monopersuli'ata,

o•* preferably KHSO 5 from about 0.5% to about 10% by weight of sodium bicarbonate and from about 0.5% to about 10% by weight of sodium carbonate, the balance of said compositions comprising water, are preferred for use herein to deform hair. The total concentration of mixed carbonate-bicar- bonate buffer in such compositions is preferably from about to about 15% by weight.

Aqueous solutions of the monopersulfate salts used

herein decompose when stored for periods in excess of

about 24 hours. As noted hereinabove, it is necessary to the practice of this invention that the solutions contain

not less 'than 1% by weight of the MHSO salt. Of course, .5 5 highly concentrated solutions of MHSO 5 salts can be pre-

pared which can be stored for several weeks or months

without decomposing below the 1% limit. However, this

is economically wasteful and it is preferable to use

freshly prepared MHSO 5 solutions herein. In the present

connotation, a "freshly prepared" solution is an aqueous

solution of the moropersulfate salt which is prepared within

2 6. about 1/2 hour prior to application to the hair. **The monopersulfate solutions herein can contain

additional components which serve to aid in their appli-

cation to hair. For example, various gelling agents such

as silica gel, high molecular weight polyoxyethylenes,

carboxymethylcellulose, veegum, and the like can be used in such solutions as thickeners for the convenience of the user. Various surfactants, for example the alkylbenzene sulf; and sulfonates and nonionic surfactants, such as polyoxyethylene condensates of alkyl phenols, as well as sodium and potassium soaps, can be present in the compo- sitions improve rinseability thereof, thereby aiding in removal from the hair once the treatment is complete.

Various perfumes, emollients, conditioning aids such as

silicone derivatives and the like can be present in

the compositions to provide pleasing cosmetic and

aesthetic aspects thereto. It is to be understood that

all manner of such nonionic, anionic'and amphoteric

auxiliary materials commonly used to enhance the cosmetic

aspect of hair curling compositions can be employed in the present compositions provided that such selected materials are

stable coriipatible with the monopersulfates at the intended

S pH use range herein. However, hydrocarbyl quaternary ammonium

salts material.s Lommonly employed in hair softening

compositions interfere with the action of the monopersulfates

2 on hair and, hence, are preferably avoided in e*e the compositions and processes herein. The instant process of deforming hair, i.e.,

curli. or straightening, can be carried out over a 0 temperature range of from about 0°F. to about 150 F.

26 Of course, use of the higher temperatures within the range, for example, by means of a hair dryer or electrically heated hair curler, will increase the rate of curling. Use of colder temperatures within the range will reduce the rate. 'Curling process-. are generally 0 carried out at a room temperature of from about 65 F.

to about 90 0 and this temperature range is preferred

in the instant process.

In the process of curling hair by applying a

solution of a monopersulfate salt, a longitudinal

stress is applied to the hair to achieve

deformation and the desired hair set. The hair to be

curled is wound on a mandrel and held in place during the

curling operation. The types of mandrels used for this

purpose are those well known in the art, including the

spiral rod and the Croquignole curler. When the spiral

rod mandrel is employed, the hair on the head is divided

into multiple sections, usually four to about eight. The

sections are then subdivided into smaller squares, ca. 1

in. x 1 in. Starting at the proximal end, the hai.. in

each block is then wound on the mandrel in the shape of a helix. The distal ends are held by a string, or clip,

or other holding device.

When the Croquignole curler is employed to curl

hair, the process is somewhat different. The hair on the

25: head is sectioned into blocks rang.ng in size from about 1/2

to 1 inch 2 to 3 inches, depending on the final hair style a envisioned. The hair in each block is then combed and the d.stal ends are placed centrally on the mandrel, which is then wound and secured in place by means of a rubber band or other clipping device. In both the spiral rod and Croquignole techniques, end papers can be used to facilitate collecting the distal ends.

In still a third technique, which results in the

formation of relatively large, loose curls, the hair is

wound in a generally circular configuration without special winding devices and set into place by means of hair

pins or clips. These so-called pin curls have a very large diameter and result in a very loose set. By proper selection

of the means whereby the longitudinal stress is applied to the

hair, curls of varying degrees of tightness can be achieved. Spiral winding results in the formation of relatively tight

curls; Croquignole winding yields somewhat looser curls;

de ~while pin curls are usually quite loose.

rIn one method of curling hair by means of a solution of a

a"onopersulfate salt, the hair is first wound as described above,

depending on the type of curl desired. The winding can be done with

Sdry hair, moistened hair or hair moistened with the solution

of monopersulfate salt. Preferably, the hair is shampooed, rinsed and towel dried prior to winding. After winding, the hair is thoroughly saturated with the monopersulfate solution. Additional monopersulfate solution can be applied from time-

to-time during the curling step to keep the hair thoroughly saturated.

The solution is allowed to remain in place from about 1 minute 3( dipcunding on the strength of the moi crsulfate solution and the degree of curl tightness desired. The treatment time will also depend to a certain extent on the coarseness of the hair, coarser hair requiring longer times within the range noted to achieve a curl. Likewise, longer times within the range are usually required when children's hair is being curled by this process. If hair has been rendered porous by peroxide bleaching or by sun or weather damage, a shorter time in the range is sufficient to impart the desired curl. The time necessary to achieve a curl can be determined by the user prior to application to the head by means of a test curl. Generally, coarse, thick hair will require a curling time of about 30 minutes when a 2% solution of the monopersulfate salt is employed.

Damaged hair will require from about 1 to about 10 minutes to achieve a curl when a 2% monopersulfate solution is employed;

children's hair will require from about 20 to about 30 minutes

to achieve a curl under the same conditions. For most

purposes, it is preferable that the solution of monopersulfate B remain in contact with the hair for a period of time from

about 5 minutes to about 15 minutes. In a preferred process herein, the hair to be curled

is contacted with an aqueous solution of the mqnopersulfate oxidant under the conditions of pH, time and temperature as noted hereinabove, while said hair remains in its natural

configuration. Following treatment with the monopersulfate

oxidant solution, the solution is removed from contact with

the hair by a water rinse or by shampooing. The hair is then moistened with water and subjected to a longitudinal stress, by winding on a mandrel if the hair is to be curled, or by brushing if the hair is to be straightened. The hair is then allowed to dry while in the stressed configuration.

It is to be recognized that this procedure is suitable for re-

setting or re-curling hair which has been deformed by the reaction

of a solution of the monopersulfate salt in the manner of

this invention. That is to say, hair which has had its keratin

structure disrupted by the monopersulfate salt can be re-curled, re-straightened or otherwise deformed, as desired, by simply

moistening the hair, again subjecting it to the appropriate

longitudinal stress, and allowing it to dry.

Hair can be straightened in the manner of this invention

by contacting said hair with an aqueous solution of an alkali metal monopersulfate salt under the same conditions of pH,

time and temperature as those used in the waving processes

disclosed above. For example, the hair can be wound in a

Croquignole winding using curlers havino a diameter of from about

2 1/2 inches to about 3 1/2 inches and allowed to dry. Hair

2 rolled on rollers of such large diameter will fall into a

substantially straight configuration upon final brushing. In an

alternate straightening procedure the hair is treated with the

monopersulfate solution and then the wet hair is brushed into a

straight configuration. The hair is then simply allowed to dry

in the straightened configuration. The foregoing processes are preferably carried out by contacting the hair with a freshly-prepared aqueous solution

comprising from about 1% to about 20% by weight of KIHSO,. from about 0.5% to about 10% by weight of sodium bicarbonate, and from about 0.5% to about 10% by weight of sodium carbonate, for a period of time from about 1 minute to about 30 minutes; rinsing the hair with water to remove substantially all of the KHSO 5 and subjecting the moist hair to a longi- tudinal stress to achieve the desired configuration and (4) allowing said hair to dry in the stressed configuration. Hair treated in this manner can be remoistened with water and reset several times and a good set can be achieved each time by simply subjecting it to a longitudinal stress.

An important advantage of the instant process is that

hair treated with the monopersulfate solution can be re-set

several times by simply rewetting the hair, subjecting it to

a stress, and allowing it to dry. In this manner, hair can be

re-styled as desired by the user. However, it has been found

that polyvalent metal ions, presumably calcium and magnesium

ions dissolved in ordinary tap water, may have a cumulative adverse

effect on the setting properties of hair which has been treated

with the monopersulfate solution. That is to say, hair treated

in thiq fashion eventually absorbs sufficient calcium and/or

magnesium ion that it is no longer as capable of being set by

simple treatment with water. When this occurs, the hair must

again be treated with an aqueous solution of a monopersulfate

salt to restore its deformable characteristics. For this reason,

it is desirable herein that the water used in any of the process

steps, the water used in the solutions of monopersulfate,

the water used to moisten the hair prior to se'ting, and the

water used to remove the monopersulfate from the hair, be sub-

stantially free from polyvalent metal ions. Acccrdingly, it is desirable that deionized water be employed in the compositions and processes herein. By so doing, hair treated with the mono- persulfate salt is capable of being set and reset up to about or more times without the need for additional treatments with the monopersulfate solution.

The following examples illustrate the hair deforming

proce-s of this invention but are not intended to be limiting

thereof.

EXAMPLE I

Hair switches, ca. 2 0.2 g. per switch,were soaked in

a freshly prepared aqueous solution consisting of 4% by weight

OXONE (commercil material comprising 41.5% KHSO 5 the balance

being equal proportions of K2SO 4 and KHSO 4 and 5% by weight

to'al carbonate buffer, comprising a mixture of 0.1% by weight

sodium carbonate and 4.9% by weight sodium bicarbonate. The

pH of the solution was 8.0. Soaking was carried out for minutes at room temperature 0 (ca. 72 F).

Immediately following treatment with the foregoing

buffered OXONE solution, the hair was shampooed with a commercial shampoo composition containing anionic surfactants and thoroag'hly

Srin with water. The treated hair, which had a silky-slick

feel, was wound in a Croquignole fashion on a mandrel (commercial hair curler; diameter ca. 1/4 The hair in the wound con-

figuration was allowed to dry at room temperature over a period

of about e hours. Following this, the hair was removed from the mandrel. The natural hair color was not substantially

changed by this treatment.

The curled hair switch obtained in the foregoing itanner

was tested for set retention of the curl measured by curl

1oss) as follows. The curl was suspended a closed robmiber containing a saturated solution of ammonium chloride, which provided a constant relative humidity of about 0S%. The distance the curl unwound after having been in the closed chamber for a two hour period was then measured and the percentage curl loss was computed by the following equation: loss of curl length of curl drop (inches in 2 hours)X 100 length of hair switch (inches)

Control switches set with various commercial setting gels and

setting liquids, as well as with ordinary tap water,were used

as controls in the test to measure the relative effect of the monopersulfate treatment. Test results are set forth in Table

1, below. Table 1 Loss Hair Treatment of Curl

4% OXONE 5% carbonate buffer 12 Control A1 57

Control B2 63

Tap Water Set 1 Commercial, non-thioglycolate hair setting gel

2 Commercial, non-thioglycolate hair setting liquid 2 The foregoing data clearly demonstrate that hair which

has been oxidized by the monopersulfate solution will accept

and retain a curl imparted thereto by a longitudinal stress to

o a far greater extent than does ui'oxidized hair ;et with water S** or with representative, commercial, non-thioglycolate hair setting preparations.

In the focegoing procedure treatment times with the

monopersulfate solution of 1,5,10 and 15 minutes are employed, respectively. In each instance the curl retention of hair treated

with the potassium monopersulfate solution is substantially

15 I greater than that of hair curled for an equivalent time with water or with the commercial, non-thioglycolate setting gel or setting lotion.

Hair curled in the foregoing manner is shampooed,

rinsed in tap water and re-set to achieve a new hair style.

This treatment is repeated about 7 times, after which the

setting properties of the hair are partially lost.

The foregoing procedure is modified by using deionized

water to prepare the solution of OXONE and in the water rinse.

Hair thus treated can be re-wetted with deionized water and

re-curled 10 times without substantial loss of its setting

properties. EXAMPLE II

Hair on a human test subject is cleansed with a

commercially available shampoo containing anionic surfactants

and thoroughly rinsed with water. The hair on the head is

sectioned into blocks having an average area of about 3 in.

:by means of a styling comb. Distal ends of the hair are

collected in tissue end papers and wound in Croquignole fashion

around commercial 3/8 in. curlers and affixed in place at the

head with rubber coated spring clips.

The curled hair on the subject's head is then thoroughly e

saturated with a freshly prepared solution comprising 5% by

weight KISO5 5% by weight sodium bicarbonate, 0.8% by weight

sodium carbonate, 4% by weight carboxymethylcellulose thickener,

the balance of said composition comprisinc water. The pH of the

composition is about 8.4. The curled hair saturated with the

monopersulfate composition is allowed to remain in place for about 5 minutes. Following this time, each curl is again saturated with an additional quantity of the fresh monoper- sulfate solution and the hair is allowed to remain in place in the curlers for an additional 15 minutes. Following this second 15 minute period, the hair is removed from the curlers and thoroughly rinsed with water. The hair is then towel dried.

Hair treated in the foregoing manner is found to have

a substantial curl and improved body properties over hair set

in similar fashion using ordinary tap water or a commercial,

non-thioglycolate setting gel. The natural hair color is not

affected.

In the above process, the potassium monopersulfate is

replaced by an equivalent amount of lithium monopersulfate,

sodium monopersulfate, rubidium monopersulfate and cesium mono-

persulfate, respectively, and equivalent hair curling results are secured.

The foregoing curling process is carried out using

solutions of potassium monopersulfate at pH's of 7, 9, 10 and 11, respectively; at each pH the hair is found to be substantially deformed and curled by the process.

EXAMPLE III

A hair straightening pomade is prepared as follows.

To an aqueous gel comprising 5.5 parts by weight sodium car-

bonate, 5 parts by weight sodium carboxymethylcellulose,

3 parts by weight magnesium aluminum silicate (veegum; binder)

and 100 parts by weight water are added 25 rarts by weight

OXONE. The OXONE is blended into the ge.atinous mixture by

hand to yield a thick pomade.

The freshly prepared pomade paste prepared in the

foregoing manner .s applied to water-wet, naturally curly

hair and rubbed in with the fingers for about 5 minutes.

Following this, the hair coated with the pomade is brushed

until a substantially straight configuration is achieved. The

thickness of the pomade helps maintain this longitudinally

stressed configuration. Following the brushing operation,

the hair in its straightened configuration is coated with

additional, fresh monopersulfate pomade which is then allowed

to remain on the hair for a period of about 30 minutes.

Following the second treatment with pomade, the hair is

rinsed and thoroughly shampooed. Thereafter, the wet hair is

brushed into a substantially straight configuration and allowed

to dry. After drying, the hair retains the straight con-

figuration. The natural color of the hair is not affected by

this treatment.

In a modification of the above procedure, the hair

coated with the monopersulfate pomade and in the substantially btraight brushed configuration is heated to a temperature of

about 150°F. As the pomade dries it is replaced by additional

pomade, from time to time. Following about 10 minutes of the heat treatment, the hair is rinsed in water, shampooed, brushed

into a substantially straight configuration and dried with an

electric dryer at about 150 0 F. This treatment is particularly

useful in straightening extremely coarse, curly hair in a

relatively short period of time without modifying the natural

hair color.

As noted hereinabove, the monopersulfate hair deforming

compositions of this invention are preferably applied to clean

hair. That is to say, hair which has had its coating of

dirt and excess lipids removed by shampooing is more sus-

ceptible to oxidation by the monopersulfate solution and

improved treatments are thereby secured. In a preferred

embodiment of this invention, the shampoo and monopersulfate

solution are applied to hair concurrently. Accordingly,

shampoo compositions containing the monopersulfate

oxidizing agentand having a pH from about 5 to about 11 can be

prepared and applied to the hair to cleanse and oxidize said

hair simultaneously. Following treatment with the mono-

persulfate-containing shampoo, the hair is rinsed with water

and the wet hair subjected to a longitudinal stress in the

manner hereinabove described and allowed to dry. Hair treated

in this manner is found to maintain its set even under con-

ditions of high humidity.

As noted hereinabove, compounds of the formula

MHSO 5 decompose relatively quickly on contact with water.

In contrast, the dry monopersulfates are stable indefinitely.

In order to provide the user of the shampoo compositions

herein with a fresh solution of monopersulfate salt, it is

necessary to package the shampoo and dry monopersulfate

S" separately. In this way, the user can mix the ingredients

just prior to application to the hair. Accordingly, the

present invention encompasses hair deforming compositions in kit form, the kit comprising a separately packaged, aqueous shampoo composition and a separately packaged portion of a monopersulfate salt of the formula MHSO 5 wherein M is as defined above. The kit can contain sufficient shampoo and monopersulfate to provide multiple treatments, or can provide sufficient material for a single treatment. A kit suitable for single treatment use comprises from about 1.0 oz. to about 7.0 oz. of a separately packaged, water-based shampoo of the type hereinafter disclosed and from about 0.01 oz.

to about 1.5 oz., preferably about 0.02 oz. to about 0.5 oz.,

of a separately packaged monopersulfate salt of the type

disclosed herein. Kits of the foregoing size provide a

sufficient volume of material for thorough saturation of the

hair. Larger kits which are integral multiples of the

single-use kits can be provided. With such multiple-use

kits, it is convenient to provide a single, large volume of

shampoo and incremental packets of monopersulfate salt.

For use, an aliquot of shampoo is admixed with a single, pre-

measured package of the monopersulfate.

The kits herein are used by simply admixing the dry

monopersulfate and the aqueous shampoo and agitating the

mixture until the monopersulfate dissolves. The resulting

solution is then applied to the hair, preferably hair which has been pre-moistened with water, in the manner disclosed

above.

The shampoo compositions employed in the kits herein comprise water and a surfactant. The

f :t .!rs jnf importt: nt ingro iicnt in any shampoo composition, and the choice of surfactant for use in conjunction with the monopersulfate salts in the hair deforming kits herein is critical inasmuch as the cationic alkyl ammonium surfactants commonly employed in hair care compositions known in the art are not suitable for use in the shampoo compositions of this invention. As noted above, such positively charged materials apparently inter- act with the oxidized hair and interfere with its deformation.

Accordingly, such cationic materials are preferably avoided

in the shampoos herein. Other than the foregoing limitation,

all manner of the well-known non-cationic, anionic,

nonionic and amphoteric surfactants can be used in the

shampoo-in hair setting composition herein.

Anionic surfactants such as the well-known, water-

soluble salts of alkylbenzene sulfates and sulfonates wherein the alkyl group contains from about 10 to about 18 carbon

atoms are useful in the shampoo compositions herein. Like-

wise, the water-soluble salts of fatty acids containing from e

about 10 to about 20 carbon atoms, soap, are suitable ee*

for use in monopersulfate shampoo compositions. Nonionic

S: surfactants, such as the alkylated polyoxyethylenes, are

useful in the shampoo compositions herein. Alkyl glycerol ether

sulfates and sulfonates wherein the alkyl group contains from

about 9 to about 21 carbon atoms are an especially preferred

class of surfactants for use in the monopersulfate shampoo compositions. Amphoteric surfactants, such as the N-alkyl-

sarcosinates having an alkyl group containing 9 to 20 carbon r atoms are also useful herein. It is to be understood that the water-soluble salts of the foregoing anionic detergents, especially the alkali metal salts, are all useful as the surfactant component of the shampoo compositions herein.

Any of the foregoing types of surfactants are well

known in the art and are commercially available. Especially

preferred as the surfactant component of the monopersulfate

shampoo compositions herein are the sodium alkyl glycerol ether sulfates, wherein the alkyl group contains from about to about 18 carbon atoms; the sodium alkyl sulfates, wherein

the alkyl group contains from about 10 to about 18 carbon

atoms; sodium N-laurylsarcosinate, and mixtures thereof.

Shampoo compositions employed in the kits herein

comprise from about 1% to about 20% by weight of a member selected from the group consisting of anionic, nonionic, and

amphoteric curfactants, the balance of said compositions

comprising water and minor portions of non-cationic cosmetic

ingredients including anionic thickeners, perfumes, and the

like, said shampoos having a pH within the range from about C 5 to about 11, preferably from about 7 to about 9.5. As

in the case of the curling and straightening compositions

above, the shampoo compositions preferably contain from about 1% to about 20% by weight of a buffer capable of

maintaining the pH within the selected basic range. Any of

.26. the pH buffer systems disclosed for use in the curling compo-

sitions herein are also suitable in the shampoos. The

Scnhonn te-bjcarbona.ite buffer system is especially preferred in the shampoos herein. Accordingly, preferred shampoo compositions herein contain, as an additional component, from about 0.5% to about 10% by weight of sodium carbonate.

and from about 0.5% to about 10% by weight of sodium bicar-

bonate, the total mixed carbonate-bicarbonate present in

the composition being within the range of from about 1% to

about 20% by weight of the total composition. The shampoo base

is admixed with the monopersulfate salt to give freshly prepared shampoo-in composition for deforming hair containing

at least about preferably 2% to 10%, by weight of

the water-soluble monopersulfate salt. The following examples are intended to illustrate

hair styling kitv comprising a shampoo and a monopersulfate

salt and their use in deforming hair but are not intended to

be limiting thereof. EXAMPLE IV

Component 1 Amount

OXONE 0.12 oz.

Component 2

2 Shampoo* 4.0 oz.

S* Shampoo formulation comprising Sodium Alkyl Glycerol Ether Sulfate (Alkyl mixed C1 2 -C 1.8%.by weight; Sodium Carbonate, 1.1% by weigh; Socium Bicarbonate, 5.3% by weight; Veegum, 2.8% by weight; Perfume, 0.65% by weight; Water, balance.

The full packet of OXONE is admixed with the full

bottle of shampoo and agitated until all the OXONE dissolves. The pH of the composition is ca. 9.

The pH-I of the composition is ca. 9. *B

The freshly prepared OXONE-shampoo composition of

Example IV is used to curl hair as follows. The hair to be

curled is first moistened with water and then all of the

shampoo composition is applied to the hair and worked in

until a lather forms. The composition is then allowed to

remain in contact with the hair for 5 minutes, after

which the hair is thoroughly rinsed with water and lightly

towel dried. The moist hair is then wound in Croquignole

manner using 1/4 in. mandrels and affixed in place at the

scalp line. The hair is then allowed to dry at room

temperature. After drying, the rollers are removed and the resulting hair is found to have a curl which is

not readily removed under conditions of high relative

humidity. The natural hair color is not affected by this

treatment.

So In the above composition, the packet of OXONE is

S replaced by 0.10 oz. packets of LiHSO 5 NaHSO 5 RbHSO 5 and

S. CsHSO 5 respectively, and equivalent hair curling results are

secured.

SQ. In the above kit, the carbonate-bicarbonate buffer

system in the shampoo component is replaced by an equivalent amount of a sodium phosphate-sodium hydrogen phosphate buffer.

The resulting shampoo composition has superior lipid removal

properties. Hair treated with this shampoo in the foregoing

manner maintains a curl even under conditions of high relative

humidity. In the above kit, the shampoo is prepared using deionized

water. In addition, a 6 oz. bottle of deionized water is

included in the kit. The deionized water is used to rinse the

shampoo from the hair prior to setting.

24 I

EXAMPLE V

Component 1 Amount

OXONE 0.45 oz.

Component 2 Shampoo* 3.0 oz. SShampoo formulation comprising Sodium Alkyl Sulfate (alkyl mixed C1 2 C1 6 1.0% by weight; Potassium Alkyl Glycerol Ether Sulfate (alkyl mixed C 1 2 C1 8 1% by weight; Sodium Carbonate, 1.1% by weight; Sodium Bicarbonate, 8% by weight; Sodium Carboxy- methylcellulose, 3% by weight; Glycerol, 3% by weight; Perfume, 0.5% by weight; Water, balance.

The full packet of OXONE is admixed with the full

bottle of shampoo and agitated until all the OXONE dissolves.

The pH of the composition is ca.

The freshly prepared OXONE-shampoo composition of

Example V is used to straighten hair as follows. The hair

to be straightened is first moistened with tap water and

all of the shampoo composition is applied to the hair and worked in until a lather forms. The composition

is then allowed to remain in contact with the hair for

approximately 30 minutes, after which the hair is thoroughly

rinsed with water and lightly towel dried. The moist hair

is then combed into a substantially straight configuration and affixed in place with clips. The hair is then dried

using a standard forced air dryer at a temperature of about

120 0 F. After drying, the clips are removed and the hair is

in the substantially straight configuration. The.straightened

hair does not curl or kink under conditions of high relative humidity. The natural color of the hair is not substantially affected by this treatment.

In the above composition, the shampoo formulation is

modified by replacing the sodium alkyl sulfate with an equivalent

amount of sodium alkyl benzene sulfate (alkyl 13.8 carbon

atoms, avg.), sodium N-lauryl sarcosinate, sodium alkyl-

glycerol sulfate (alkyl C1 0 C1 8 and sodium coconut soap,

respectively, and equivalent results are secured. The foregoing examples illustrate the hair deforming

kits of the instant invention comprising a separately packaged, water-based, non-cationic shampoo and a separately packaged portion of a water-soluble monopersulfate oxidant, said portion being

sufficient to provide a concentration of oxidant in the shampoo

of at least about preferably about 1% to about 20% by

weight. It is to be recognized that such compositions can contain other ingredients such as tints, emollients, hair

control agents and the like, so long as such additional ingredients are not: cationic in nature.

Claims (1)

1. The claims defining the invention are as follows

   1. A process for deforming hair comprising: (1) contacting said hair with an aqueous solution comprising from

   about 1% to about 20% by weight of an oxidant of the formula

   MHSO 5 wherein M is an alkali metal cation, at a pH of from

   about 5 to about 11; subjecting the moist, treated hair

   to a longitudinal stress; and thereafter drying the hair

   in the stressed configuration.

   2. A process according to Claim 1 wherein the oxidant

   is KHSO 5

   3. A process according to Claim 1 wherein the oxidant

   is OXONE

   4. A process according to Claim 1 carried out at a

   pH in the range of 7.0 to

   A process according to Claim 1 wherein the solution

   of oxidant remains in contact with the hair for a period from

   about 1 minute to about 30 minutes.

   6. A process according to Claim 1 wherein the solution of oxidant contains a carbonate-bicarbonate buffer.

   7. A process according to Claim 1 wherein the moist, treated hair is wound on a mandrel and dried, whereby the hair i url'd.

   8. A process according to Claim I wherein the moist,

   treated hair is fashioned into a substantially

   straight configuration and dried, whereby the hair is

   straightened.

   9. A process according to Claim 1 wherein the hair

   is contacted with an aqueous solution comprising from about

   3% to about 15% by weight of KHSO 5, from about 0.5% to about

   by weight of sodium bicarbonate, from about 0.5% to

   about 10% by weight of sodium carbonate, for a period of

   from about from 5 minutes to about 30 minutes, rinsed,

   subjected to a longitudinal stress and dried in the stressed

   configuration.

   A process for deforming hair comprising the steps of:

   contacting hair with an aqueous solution comprising from about

   1% to about 20% by weight of oxidant of the formula MHSO 5 wherein

   M is an alkali metal cation, at a pH of from about 5 to about

   11 for a period of time from about 1 minute to about

   minutes; rinsing the oxidant solution from the hair

   ,with water; subjecting the moistened hair from step (2)

   to a longitudinal stress; and drying the hair while in the

   stressed configuration.

   11. A process according to Claim 10 wherein the stress

   is applied by winding the hair on a mandrel.

   12. A process according to Claim 10 wherein the stress

   is applied by winding the hair in pin curls,

   13. A process according to Claim 10 wherein the oxidant

   is KHSO 5

   14. A process according to Claim 10 wherein the oxidant is OXONE

   A process according to Claim 10 which is carried

   out at a pH in the range of 7.0 to

   16. A process according to Claim 10 wherein the

   solution of oxidant remains in contact with the hair for a

   period of from about 5 minutes to about 30 minutes.

   17. A process according to Claim 10 wherein the

   solution of oxidant contains carbonate-bicarbonate buffer.

   18. A process according to Claim 10 wherein the water

   used to rinse the oxidant from the hair is deionized water.

   19. A hair deforming composition in kit form comprising:

   a separately packaged, water-based shampoo; and, a separately packaged portion of an oxidant of the formula

   MHSO 5 M wherein M is an alkali metal cation, said portion being sufficien to proiride a concentration of oxidant in the

   shampoo of at least about 1% by weight.

   29 I

   I

   A kit according to Claim 19 which is designed for

   single use comprising: from about 1.0 oz. to about

   oz. of a separately packaged, water-based shampoo; and,

   from about 0.01 oz. to about 1.5 oz. of the oxidant.

   21. A kit according to Claim 19 wherein the oxidant

   is OXONE

   22. A kit according to Claim 19 wherein the shampoo

   contains a carbonate-bicarbonate buffer at a pH of from

   to about

   23. A shampoo composition, comprising:

   from about 1% to about 20% by weight of a non-

   cationic surfactant;

   from about 1% to about 20% by weight of a basic buffer salt;

   from about 2% to about 10% by weight of a water-

   soluble monopersulfate salt; and

   the balance of said composition comprising water.

   r S

   S" DATED 2nd October, 1973

   1::ILLo, ORONDE FITZPATRICK, Attorneys for TIEj iCOTER G.A.BLE COMPANY

   *Owl i

   30 I