US 3579632 A
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United States Patent Office 3,579,632 Patented May 18, 1971 3,579,632 HAIR AND SCALP TREATMENT WITH A PRINCIPALLY SODIUM CHLORIDE THICK VISCOUS AQUEOUS SLURRY Victor G. Sonnen, Broad Brook Road, Hazardville, Conn. 06036 No Drawing. Filed Aug. 2, 1965, Ser. No. 476,640 Int. Cl. A61k 7/06 U.S. Cl. 424-70 14 Claims ABSTRACT OF THE DISCLOSURE A hair conditioner composition, useful in reducing the drying time of the hair after washing and causing the hair to become more manageable, and also having dandruff alleviating properties, is provided comprising 30-76 parts by weight of a salt of at least 60% NaCl having a particle size preferably in the range of 0.00025 to 0.00125 inch and 70-24 parts by weight of water. The composition may also include thickening agents, a fatty alcohol, detergent, lanolinic material, perfume and dye.
The present invention relates to a hair conditioner and, more particularly, to an agent which provides more manageable hair.
It is an object of the present invention to provide a chemical treatment of the hair and scalp which will tend to alleviate the symptoms of seborrheic dermatitis of the scalp, commonly called dandruff.
It is a further object of the present invention to provide a hair rinse which may be used after the hair has been cleaned with conventional soap, shampoo, or detergent.
It is a still further object of the present invention to provide a treatment of the hair which will cause the hair to become more manageable than would normally be the case immediately after Washing and drying the hair.
It is still another object of the present invention to provide a hair conditioner agent which will shorten the drying time of the hair after the hair has been cleaned and rinsed with conventional shampoos.
The use of this hair conditioner is of great importance in any beauty salon in that it provides a saving of a considerable amount of time which is normally wasted drying the hair with heated ventilated air.
The following specific examples of formulations in accordance with this invention are illustrative only and should not be construed as limiting the scope of the invention.
These objects of the present invention are provided by treating the hair with the following formulation:
Parts by weight Salt (at least 60% NaCl) having a particle size less than 0.005 inch 30-76 Water 70-24 Thickening agent -20 Fatty alcohol 00.2 Detergent 0-3 Lanolin or derivative 0-2 Trace of perfume. Trace of dye.
At room temperature the above mixture forms a thick viscous slurry containing about 26 parts by weight of the salt as a saturated solution with the remainder in the form of fine particles suspended therein.
It has been discovered that a brief treatment of the hair and scalp with the very concentrated salt slurry irnproves the condition of the hair and scalp. It is not presently known whether the concentrated salt acts as an antiseptic or whether the concentrated electrolyte conditioner extracts water and Water soluble impurities from the hair and scalp; the exact mechanism may be a combination of the above or something else. At any rate, ap plicant does not wish to be limited by these theories but offers them as a possible explanation of the phenomena observed.
The use of the concentrated salt slurry on unwashed dry hair and scalp is feasible and will accomplish similar results to those described above. In most instances, however, it is more convenient to wash the hair before using the electrolyte hair conditioner. Use of the slurry described herein will be effective even on wet hair because the finely divided salt particles apparently dissolve readily and quickly thereby rendering the Water in the hair into a very concentrated of saturated salt solution.
One of the essential features of the present invention resides in the use of finely divided salt particles. The use of large salt particles is not satisfactory although the exact reason for this is not known. It may be that the smaller particles in the slurry are able to reach the scalp and all portions of the hair more easily than larger particles. In addition, the finely divided salt particles dissolve readily in water, thereby providing the concentrated salt solution required to condition the hair and scalp. Another advantage of the finely divided salt described lies in storage stability, The finely divided salt is far less prone to undesirable settling out of a thickened salt solution than is unground salt.
Generally it has been found that a particle dimension of 0.00025 to 0.00125 inch is optimum for the purposes of the present invention, although a particle size as coarse as 0.005 inch can be utilized. Many of the particles are odd shaped; reference is to the average distance across the particle in its smallest direction, it being understood that, on the average, the largest dimension will also be less than 0.005 inch.
Generally, ballmilling has been found effective for the purpose of comminuting salt particles to provide the particles useful in the present invention. Sandmills and other grinding machines may be utilized; also the salt may be procured in a finely divided state.
Thickener is preferably used with the salt and Water. Finely ground dry salt can be added to a thickened water solution with agitation of the Water, or the thickener may be stirred in last. In some instances, coarse salt crystals, thickener and water may be ground together.
Many thickening agents retard the grinding operation, although both organic and inorganic thickeners can be employed successfully. Hydroxyethyl and carboxymethyl substituted cellulosics are preferable thickening agents. Zero to 2% high molecular weight carboxymethyl cellulose, 0.65 to 0.85 carboxyl per cellulose unit, is particularly effective. Carboxylated polymers such as polyacrylic acid; polymethacrylic acid; maleicvinyl methyl ether copolymer; simple amides such as polyacrylamide, polyvinyl pyrrolidone; and seed and exuded natural gums such as guar seed and gum tragacanth (astragulus extrudate) are useful. Colloidal inorganic thickeners such as colloidal alumina; and Cab-O-Sil (0.05 micron silica) have also been found to be satisfactory thickeners. Adjuvant materials such as ethylene oxide adducts of nonyl phenol assist the thickening action of the silica.
Certain other thickening materials have been found to be unsatisfactory, the high salt concentration tending to destroy the thickening action. Polyvinyl alcohol, polyethylene oxide, and methyl cellulose were found to be unsatisfactory, salt-incompatible, thickening agents. The amount of thickening agent utilized depends on the nature of the agent, the molecular Weight of organic thickening agent (or particle size and adjuvant for inorganic agents), and size and concentration of salt particles as shown in the table. The range of thickening agent utilized in the table was 1.2 to 24% of the water content. While the thickening agent is not required at the maximum salt content of 76% (Example 19), it is generally preferred. Although the #6 spindle rpm. Brookfield (Brookfield Engineering Laboratories, Stoughton, Mass.) viscosity is only 8,000 centipoise with 76% salt and no thickening agent, the packing of the salt crystals is such that a water layer does not rise to the surface. With lesser quantities of salt than 76%, a salt Water layer separates unless a thickening agent is present and the slurry must then be mixed prior to use. Generally a 10 rpm. Brookfield viscosity of 15,000 cp. is the minimum required to retard or prevent separation of a salt water layer. Too high a viscosity, i.e., greater than 75,000 cp. (centipoise), is undesirable because the preparation becomes difiicult to rinse out of the hair. Generally the preferred viscosity is 25,000 to 45,000 cp. (Brookfield, l0 r.p.m.).
The table which follows gives the results of a number of examples of thickening agents utilized with 120 parts of NaCl and 100 parts of water after tumbling for hours in a jar mill:
Polyacrylamide 100 has a viscosity in centipoises at C. of 2% concentration of -50.
PVP K90 has an average molecular weight of 360,000.
Elvanol -42 had a viscosity in cps. of a 4% aqueous solution at 20 C. of 35-45. The mole percent hydrolysis on a dry basis is 87.2-89.2. The pH is 5.0-7.0, volatiles are 5% max. and ash is 0.75% max. (calculated as Na O).
CMC 4HP has a viscosity at 1% concentration of 1300- 2200 centipoises at 25 C. and a range of substitution of 0.38 to 0.48.
To prevent a hard crust from forming at the air interface, if the formulation is left for more than 1 hour without a closure or cap, it has been found advisable to include approximately 0.03% of a fatty alcohol such as cetyl or lauryl alcohol in the formulation. The fatty alcohol CH (CH OH retards water evaporation, hence crust formation. Generally a range of 0.01 to 0.3% is preferable. The fatty alcohol is not necessary for aerosol packaging.
For some purposes, such as softening the hair, it may be desirable to include a lanolin or lanolin derivative in TABLE [Thickening agents with 120 parts NaCl and 100 parts water-after tumbling 15 hours] Parts by Viscosity 01)., weight in #6 spindle 100 parts 10 rpm.
of water Thickening agent Brooklioltl Settling Comment Example:
1 1.2 Hercules (.M( 7 II 1* high M.W. car- 43,100 No hoxyinetliyl Cellulose of (1.65-0.85 (11 00011 per cellulose unit. I 11.4 WSR 301 Union Carbide) plmllS- 1 300 Yes Salts out of solved high M.W. polyethylene oxide. solution. 3. 3 Ml-tlioeel 4000 (Dow) 11](dlSS0lVltl 2, 800 Yes Do.
high M.W. rnvtliylulutl cellulose. 7. 0 Bayrnal (Du Pout) colloidal aluminum 21. 000 \"XYSI 8.0 (nli-O-Sil ltlS-fi (Cabot) 0.05 micron 13,000 b'light s1 lea. 2.5 Natrosol 250 HR (Hercules) hydroxy- 83,200 No No grinding.
othylatedcoilnlosio. 7 15.0 K-704 (Goodrich) polyacrylic acid. 13, 000 Yes Do. 8 11.0 Polyacrylamide100(Cyanamid) poly- 21, 600 V. Si.
at-rylamide. 9 M. 0 PEP K90 (GAE) polyvinyl pyrroli- 185,000 Yes No grinding.
one. 1.0 Type A high M.W. gelatin Thin Yes 15. 0 Elvanol 50-42 (Du Pout) DlTdlSSOlVOd Gels -88? hydrolyzed polyvinyl alcohol. 3.0 Gum tragacanth XXX SA (Stein 37,600 No Hall) galactomannau polysnccharido. 4. 0 CMC 4 H}? (Hercules) High M.W. 25, 500 Trace..-
cat-boxyrnetliyl cellulose, 0.38-0.48 (11 C 0 0 H per cellulose unit.
Appearance: white or off-white granules Softening point: C.- C.
Brittle temp.: 50 C.
Ash content, max. (calculated as CaO): 2.0 weight percent.
Methocel 4000 indicates that the viscosity of 2% solution at 20 C. is 4000 centipoises.
Natrosol 250 HR has a viscosity at 25 C. of 1% concentration of 1500-2500. The H indicates high molecular weight. The R indicates that it has a fast dispersion. Its properties are as follows:
Ash content, percent (Calculated as Na S0 4.0 max. Bulk density, g./ml.: 0.55-0.75
Color: white to light tan pH in solution: 6.5-8.5
K-704 has a Brookfield viscosity in centipoises at 78 F. of 4% concentration of 15; at 8% concentration of and at 12% concentration of 600.
the formulation. Generally a level of about 1% lanolin is desirable, although a range of 0.3 to 3% is useful.
If foaming and spreading action is desired, a detergent, or surface active agent such as a sulfated fatty alcohol (e.g., lauryl alcohol sulfate, decyl alcohol sulfate), a sulfated alkylphenol-ethylene oxide (e.g. ethoxylated nonyl phenol sulfate), amphoteric detergents (e.g., N-laurylmyristyl-B-aminopropionic acid; disodium N-lauryl l5- imino-dipropionate), or an alkanol amide (e.g., lauryl diethanolamide) may be added to the formulation, preferably 0.5 to 3% of the entire formulation. For cosmetic purposes, perfume and dye may be added as required.
The salt utilized in the present invention is principally sodium chloride; however, relatively non-toxic mixtures of 60% sodium chloride with up to 40% other salts, such as KC], MgCl may be employed. Sea salt (96% NaCl) for example, is suitable despite the high content of magnesium, calcium, and the presence of a wide variety of metals.
EXAMPLE 14 180 grams of sodium chloride, (table salt crystals) grams of water 1.8 grams Hercules (Hercules Powder (30., Wilmington, Del.) 7 HP CMC, (carboxymethyl cellulose 0.65 to 0.85-COOH per cellulose unit. A 1.2% solution of the polymer in water at 25 C. possesses a viscosity of 4,500 cp. at 10 r.p.m. Brookfield).
The above ingredients were charged into a one liter capacity jar mill half filled with approximately 4 inch fiintstones and tumbled 15 hours at 45 r.p.m. The resulting slurry was then drained free of the stones. A Brookfield viscosimeter fitted with a #6 spindle was immersed in the slurry. At 10 r.p.m. the viscosity was found to be 43,000 cp. Microscopic examination revealed crystals of salt ranging from 0.00025 to 0.00125 inch. Average crystal size was approximately 0.0005 inch. The thick viscous slurry did not settle on standing one month. When applied to freshly washed hair and permitted to remain in contact with the hair and scalp for two to five minutes before rinsing out the salt with fresh water, the formulation was found to have effected the following changes in the condition of the hair and scalp of several patients:
(1) The hair was more easily dried than usual. The drying time was reduced by about 50%.
(2) The hair was much more manageable than is normally freshly washed hair; i.e., it can be combed and held in place without application of an oil or grease hair tonic.
EXAMPLE 15 A formulation similar to Example 14 was tumbled for varying times in the jar mill:
hours Comment 1 to unground salt crystals.
2 Approximately /2 particles unground. 3 Approximately /3 particles unground. 5 Particle sizes range substantially from 0.00025 to 0.0025 inch.
7 Do. 15 Particle range substantially 0.00025 to 0.00125 inch.
This example shows that for the apparatus of Example 14 it is necessary to grind for at least 5 hours to obtain satisfactory particle size.
EXAMPLE 16 180 grams finely divided salt (0.0005 to 0.0025 inch crystals) was stirred into a solution of 1.8 Hercules 7 HP CMC in 150 grams of water. The resultant slurry viscosity (Brookfield #6 spindle) was R.p.m.: Op. 15,800 20 11,200 50 7,000
Final particle size of the salt ranged from 0.00025 to 0.0025 inch. The formulation did not settle on standing.
EXAMPLE 17 NaCl 180 Water 150 Cab-O-Sil MS-S [(Cabot)-0.05 micron silica] 12 The ingredients were mixed and were ballmilled hours.
Resultant viscosity at r.p.m. Cp. l0 13,000
Some settling occurred on standing. General Aniline and Film Igepal (IO-630 (2.4 grams-nonyl phenol ethylene oxide detergent) was stirred into the slurry. The slurry became very thick and no settling on storage was noted.
Viscosity at r.p.m. Cp. (approx) 10 40,000 20 33,600 50 13,000
6 EXAMPLE 18 The formulation:
Salt 180 Water 150 CMC 7 HP 1.8 Cetyl alcohol 0.1
The mixture was ballmilled for 15 hours. The formulation was very resistant to surface encrustation if permitted to stand without a cover.
EXAMPLE 19 Salt 240 Water The mixture was ballmilled 15 hours. The slurry was drained from the stones and permitted to stand for two days. A small quantity of salt water separated and was removed. The remaining slurry did not settle on standing and was found to consist of 76% salt.
Viscosity at r.p.m. Cp. 10 8,200 20 3,500 50 1,560
EXAMPLE 20 The formulation of Example 14 was prepared and 3.3 grams Ethoxylan (Malmstrom Chemical Co., Newark, N.J., ethoxylated water soluble lanolin which is a water and alcohol soluble emollient material having skin softening characterisics. It has the following characteristics) Color: Yellow Odor: Faint, pleasant Acid value (USP): 1.2 max.
Saponification value (USP modified): 12-20 Hydroxyl value (A.O.C.S. Cd. 13-60): 25-55 Iodine value (USP Hanus): 7-12 was stirred into 330 gm .of the Example 14 formulation. Hair treated with this formulation was softer and more pliant than when the formulation of Example 14 was used without the lanolin.
The ingredients were ballmilled 15 hours. Then 7.0 gm. Deriphat C General Mills (50% solution of N-laurylmyristyl-fi-amino-propionic acid in water) was mixed in.
Viscosity at r.p.m. Cp. l0 31,000 20 20,000
This formulation lathers readily when rubbed into wet hair. The formulation leaves the hair relatively free of snarls and excessive entanglement after rinsing and drying the hair.
It will be obvious to those skilled in the art that various changes may be made without departing from the spirit of the invention and therefore the invention is not limited to what is described in the specification, but only as indicated in the appended claims.
What is claimed is:
1. A composition for the treatment of hair and scalp to condition the hair and to alleviate the symptoms of seborrheic dermatitis of the scalp comprising a thick slurry consisting essentially of:
(a) 30-76 parts by Weight of at least one salt consist ing essentially of NaCl present in a minimum quantity of 60% by weight of the total salt content, and any remaining salts being selected from the group consisting of chlorides, potassium, magnesium and calcium, and having a particle size less than 0.005 inch;
(b) 70-24 parts by weight of water, and
(c) a salt-compatible thickening agent in an amount up to 20 parts by weight, said slurry having a viscosity of 15,000-75,000 cp. at 10 r.p.m. Brookfield.
2. A composition according to claim 1 further comprising (d) 0.001 to 0.3% of a fatty alcohol;
(e) 0.5 to 3% of a surface active agent, and
(f) 0.3 to 3% of an emollient selected from the group consisting of lanolin and ethoxylated lanolin, the percentages all being based on the entire formulation.
3. A composition in accordance with claim 2 wherein the particle size of said salt lies between 0.00025 and 0.00125 inch.
4. A composition in accordance with claim 2 wherein the viscosity of said slurry lies between 25,000 and 45,000 cp. at 10 r.p.m. Brookfield.
5. A composition in accordance with claim 2 wherein said fatty alcohol is of the formula CH (CH 01-1.
6. A composition in accordance with claim 5 wherein said fatty alcohol is selected from the group consisting of cetyl alcohol and lauryl alcohol.
7. A composition in accordance with claim 2 wherein said surface active agent is N-lauryl-rnyristyl-fl-aminopropionic acid.
8. A composition according to claim 1 wherein said thickening agent is up to 2 parts by weight of carboxymethyl cellulose having a viscosity of a 1.2% solution in water at 25 C. of 4500 cp. and having 0.65-0.85 carboxyl groups per cellulose unit to provide a resulting slurry viscosity of between 25,000 and 45,000 cp. at r.p.m. Brookfield and said salt has a particle size of between 0.00025 and 0.00125 inch.
9. A method of treating hair and scalp to condition the hair and to alleviate the symptoms of seborrheic dermatitis of the scalp comprising applying an effective amount of a slurry of (a) 30-76 parts by weight of at least one salt consisting essentially of NaCl present in a minimum quantity of 60% by weight of the total satlt content, and any remaining salts being selected from the group consisting of chlorides, potassium, magnesium and calcium, and having a particle size less than 0.005 inch; and
(b) 70-24 parts by weight of water, said slurry having a viscosity of 900075,000 cp. at 10 r.p.m. Brookfield, to the hair and scalp for a period of at least 2 minutes followed by rinsing the hair and scalp with water.
10. A method in accordance with claim 9 wherein said slurry further includes (c) suflicient salt-compatible thickening agent to provide a slurry viscosity of 15,000-75,000 cp. at 10 r.p.m. Brookfield.
11. A method according to claim 9 wherein said slurry contains 76% of said salt content.
12. A method according to claim 10 wherein said thickening agent is up to 2 parts by Weight of carboxymethyl cellulose having a viscosity of a 1.2% solution in Water at 25 C. of 4500 Cp. and having 0.65-0.85 carboxyl groups per cellulose unit to provide a resulting slurry viscosity of between 25,000 and 45,000 cp. at 10 r.p.m. Brookfield and said salt has a particle size of between 0.00025 and 0.00125 inch.
13. A composition for the treatment of hair and scalp to condition the hair and to alleviate the symptoms of seborrheic dermatitis of the scalp comprising a thick slurry consisting essentially of:
(a) 200 grams of salt consisting essentially of NaCl present in a minimum quantity of 60% by weight of the total salt content, and any remaining salt being selected from the group consisting of chlorides of potassium, magnesium and calcium, and having a particle size less than 0.005 inch;
(b) grams of water;
(0) 2.3 grams of carboxymethyl cellulose having a viscosity of a 1.2% solution in water at 25 C. of 4500 cp. and having 0.65-0.85 carboxyl groups per cellulose unit; and
(d) 7 grams of a 50% aqueous solution of N-laurylmyristyl-fi-aminopropionic acid; said slurry having a viscosity of 31,000 cp. at 10 r.p.m. Brookfield.
14. A method of treating hair and scalp to condition the hair and to alleviate the symptoms of seborrheic determatitis of the scalp comprising applying thereto an effective amount of a slurry of:
(a) 200 grams of salt consisting essentially of NaCl present in a minimum quantity of 60% by Weight of the total salt content, and any remaining salt being selected from the group consisting of chlorides of potassium, magnesium and calcium, and having a particle size less than 0.005 inch;
(b) 150 grams of water;
(0) 2.3 grams of carboxymethyl cellulose having a viscosity of a 1.2% solution in water at 25 C. of 4500 cp. and having 0.65-0.85 carboxyl groups per cellu lose unit; and
(d) 7 grams of a 50% aqueous solution of N-laurylmyristyl-fl-aminopropionic acid; said slurry having a viscosity of 3l,000 cp. at 10 r.p.m. Brookfield.
References Cited UNITED STATES PATENTS 42,311 4/1364 Rose l6787 2,773,834 12/1956 Henkin 167-87X 3,071,514 1/1963 Phillips et al. l6787 3,090,727 5/ 1963 Carter l6787 3,329,595 7/1967 Barbato et al 204128X 3,137,624 6/1964 Foley 424153 FOREIGN PATENTS 809,689 3/1959 Great Britain l6787 701,273 1/1931 France l6787 1,030,513 5/1958 Germany l6787 1,040,750 10/1958 Germany l6787 OTHER REFERENCES Nature, vol. 169, April 1952, pp. 662-663. Mapstone, Journal of the Society of Cosmetic Chemists, vol. 12, No. 4, May 1961, pp. 239-243.
ALBERT T. MEYERS, Primary Examiner V. C. CLARKE, Assistant Examiner U.S. Cl. X.R.