Classifications

• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
  • A61Q5/00—Preparations for care of the hair
  • A61Q5/10—Preparations for permanently dyeing the hair
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K8/00—Cosmetics or similar toiletry preparations
  • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
  • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
  • A61K8/46—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing sulfur
• • D—TEXTILES; PAPER
  • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
  • D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
  • D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
  • D06P3/02—Material containing basic nitrogen
  • D06P3/04—Material containing basic nitrogen containing amide groups
  • D06P3/30—Material containing basic nitrogen containing amide groups furs feathers, dead hair, furskins, pelts
• • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
  • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y10S8/00—Bleaching and dyeing; fluid treatment and chemical modification of textiles and fibers
  • Y10S8/916—Natural fiber dyeing
  • Y10S8/917—Wool or silk

Definitions

• a further object of the invention is to provide a method for permanently dyeing keratinous material, and' particula'rly humanhain-under suitable conditions withnon i toxic coal-tar dyes, in--such a manner that the color is' securely fixed in the dyed materialandcannot b removed by rubbing, washing or shampooingi-
• a still further object of the-invention is to providea method 1 for permanently dyeing human hair with nontoxic dyes in-a manner to permit permanenbwaving'bf' the dyed hair without change of the "color imparted -to the hair and without hair damage.
• a still further object of theinvention is to providefa method forpermanently dyeing human hair with entirely non-toxic and harmless dyes, which methodis ea'sy'and" safe 'in its application, satisfactory in its results; and does not require either a pre-treatrnent or an-after-treatment" ofthe hair; i p
• Still'a further object of the invention is to provide'a method of permanently dyeing human hair by means of the dyes which areknown as certified colors and Which heretofore have not been successfully used for this'pui pose; l
• Still anotherobject of the invention is to produce a preparation for the permanent dyeing of keratino'usmaterialg andparticularly' of human hair; which can be applied to-the"*hair in a simple manner and which pro prisesth'e desired coloringeasily andsafely andwithout undesirable or harmful side eflec'ts or after'effectsi
• a special object of the invention is to produce a preparation-forthe-permanent dyeing of keratinousmaterial, andparticularly of-human hair, which consists of two" separate solutions to be mixed immediatelybefore appli-' cation to thematerial to be' dyed, and which yields a mixture producing the desired coloring effect by'means" of-cer'tifiedcolors'in a reliable, safe'and permanent man-'
• Another specialobject of the invention is to produce" a preparationfor"the permanent dyeing of 'ker'atinous" materiaL particularly of human hair, which consists-of a dry, powdery mixture of several water-solublein gredients which, on
• the dyeing method according to my invention comprises the steps of treating the material to be dyed "with a freshly prepared neutral to mildly alkaline, aqueous solution containing a small percentage of a water-soluble mercapto compound and, as sole coloring agent, a dyestufi of the group consisting of the Ext. D & C, D & C and F D & C certified colors and mixtures thereof, washing the dyed material with an aqueous medium, and drying'it.
• certified colors could be used for the perm'anent' dyeing of keratinous matter only in strongly acid or" strong salt solutions, and at elevated temperatures.
• The'pr esent'invention is based on my discovery that the Ext. D & C, D & C and F D & C certified, non-toxic coal tar dyes are suitable for the permanent dyeing of keratinous material at moderate temperatures and in neutral or mildly alkaline solutions, if a relatively small percentage of water-soluble mercapto compounds is added to the dye solutions immediately before they are used.
• Myinvention makes it possible to dye human hair in a simple manner permanently with dye preparations containing" exclusively completely harmless and safe ingredientsand to produce natural, predictable color shades which arefast to rubbing, washing, shampooing and permanent waving.
• the substances migrating with the water or transported thereby become effectively trapped or imbedded in the hair substance and are not subject to removal by customary treatments, such as rubbing, toweling, washing, shampooing or permanent Waving; Microscopic examination has shown the hair fibers to be uniformly stained over the areas between the imbrications.
• dye solutions suitable for the dyeing of keratinous material according to my invention may contain preferably between about 0.033 and 6.2% by weight of the solution of such dyestuffs.
• the water-soluble mercapto compounds to be used in the dye solutions according to my invention are particularly the water-soluble mercapto compounds of the general type useful for hair waving and depilatory purposes. Suitable examples are thioglycolic and thiosalicylic acids in the form of their water-soluble salts, thioglycol, thioglycerol and thiophenol. At present, I prefer in most cases to use thioglycolic acid because it is readily available, has no intense objectionable odor, and is ordinarily entirely harmless in the concentrations in which it is used according to my invention, but I do not limit my invention either to this or to any other particular mercapto compound.
• the water-soluble mercapto compounds are present in my dye solutions in quantities equivalent with respect to S H group to about 0.1 to 6% by Weight of the solutions of thioglycatic acid.
• a mercapto compound content equivalent with respect to S H group to between about 1.2% and about 6% by weight of the solution of thioglycolic acid has been found to give most favorable results.
• the temperatures used in my dyeing processes may vary between about 50 and about 110 F. Temperatures of between about 60 and about 80 F. are preferred, particularly in the use of my invention for the permanent dyeing of human hair.
• the dye solutions according to my invention are applied to the keratinous material at a pH value between about 6.6 and about 11.3 and preferably at a pH value of between about 9 and 10.2.
• a pH value between about 6.6 and about 11.3 and preferably at a pH value of between about 9 and 10.2.
• I have successfully used concentrated aqueous ammonia, sodium hydroxide, sodium carbonate in the presence of ammonium chloride, ethylene diamine, and triethanolamine. Other alkalies could undoubtedly be employed.
• Useful effects in coloring hair are accomplished at temperatures of between about 60 F. and about 80 F. with relatively weak solutions of mercapto compounds and usually at mild alkalinities. I have found adequate, for example, up to about 4% by weight of the solution of thioglycolic acid at alkalinities corresponding to pH values of not more than about 10.5 during 15 to 25 minutes. Many of my successful hair dyeings, accomplished without evidence of any resultant hair damage have been performed with less than 2.6% by weight of the solution of thioglycolic acid in the form of its sodium salt, with excess of ammonia as free base at pH values of about 9 to 10 at a temperature of about 68 F. within about to minutes. This combination of conditions lies well within allowable extremes and may be adopted as normal.
• alkalinity should be adjusted to a lower pH value, for instance, 9.4 or less to preclude irreversible hair damage.
• a high temperature such as, for example, 110 F.
• a moderate concentration of mercapto compound for instance, in the range of up to about 2.5% by weight of the solution of thioglycolic acid, may require lowering of the pH value below 9.3 in order to preclude hair damage.
• very good hair coloration without any evidence of hair damage, may be effected with 2.5% by weight of the solution of thioglycolic acid acting upon hair at 110 F. during 15 minutes at a pH of 8.0. Decrease below normal of any of the three factors diminishes the risk of hair damage but weakens correspondingly the resultant coloration.
• coloring action is appreciably less than at 60 to F. for 1.4% by weight of the solution of thioglycolic acid at a pH of 9.4 acting during 20 minutes.
• coloring action is appreciably less than with 1.4% by weight of the solution of thioglycolic acid, other conditions remaining the same for both cases.
• coloring action is appreciably less than at a pH of 8.5 for 2.5% by weight of the solution of thioglycolic acid at 70 F. during 20 minutes.
• Minima for concentration of mercapto compound, pH, and temperature are not imposed like maxima, by the susceptibility of hair to damage, but are chosen when low values for one or more factors require considerable increase above normal in one or more of the remaining factors for good and intense coloring of the hair.
• the solutions have a pH value between 6.6 and 10.4 but not higher than 9.4 when the mercapto concentration is equivalent to at least 3% by weight of the solution of thioglycolic acid and not higher than 9.15 when the mercapto concentration is equivalent to at least 5.6% by weight of the solution of thioglycolic acid.
• the solution is applied to the hair at a temperature of between about 50 F. and F. but not less than 70 F. when both mercapto concentration and pH value approach their minimum values and not higher than 80 F. when both mercapto concentration and pH value approach their maximum values.
• Mild oxidizing agents such as hydrogen peroxide, and acids, such as acetic acid, may be used in these cases, which :are within thebroad scope of my inventiomfor after-treatment of the dyed hair.
• My invention also covers the new preparations for the permanent dyeing of keratinous material to be .used in...
• Such preparation maybe, for instance, a'
• Preparations which are intended for the dyeing of human hair contain preferably a quantity of: wateresoluble mercapto compound equivalent withrespect to SH' group toabout 1.2%"to6%-' by weight-of the solution-of' thioglycolic acid and have a pH value of "between*6.6 to 10.4 but not higher than 9.4 when the mercaptoconcentration is equivalentioat least 3%- by weight of the. solution of thioglycolic acid and not higher than:.9.15. when the mercapto. concentrationis equivalent to at least 5.6%..by weight of the solution of thioglycolicacid.
• a preparation of :the dyeing of keratinous .material,. and particularlyrof human hair may comprisea' of. the two solutions,; the total-quantity of solvent in both solutions and the relative proportionsof the solutions being such that the resulting mixture is neutral or mildly alkaline and contains a small percentage ofa watersoluble mercapto compound.
• a preparation for the dyeing of keratinous materiaLand particularly of human hair may be a substantially dry powder mixture comprising a dry, water-soluble solid mercapto compound, an ammonium salt, a dry, weakly alkaline, water-soluble salt of an alkali-metal, and,:'as:
• a dry, wateresolubledyestuff selected from the group consisting of. the Ext. D & .C,.D;& Cand.
• a dye solution which contains a small percentage of mercapto compound and is neutral or mildly alkaline.
• Example -I Firm textured, nearly colorless human hair was immersed for 15 minutes-at a temperature of F., with exclusion of air, in a solution carrying,0.920g.. of a dyestufi'mixture consisting of:
• Example [I Firm textured, nearly colorless human hair was satu- Y rated for 3 minutes in a solution containing 3.89 g. of a dyestuff mixture consisting of:
• the hair was in part merely rinsed and blotted, then dried, in part well-shampooed, then rinsed, blotted and dried.
• the rinsed hair retained a pale pink-violet coloration,- the shampooed hair a distinctly paler pink-violet coloration; Most of the pale color adhering' to the merely rinsed hair was located superficially and-was removable by shampooing. The hair .was not permanently dyed.
• the thioglycolic acid content amounted to 2.6% by weight of the solution, the dyestutf content to about 4% by weight of the solution.
• hair of the same character was similarly saturated for 3 minutes and then exposed wet for 15 minutes to the atmosphere under identical temperature conditions estimated on the average to be about 60 F.
• the hair was in part merely rinsed and blotted, then dried, in part well shampooed, then rinsed, blotted and dried.
• the merely rinsed hair retained a strong violet-brown coloration
• the shampooed hair likewise a strong violet-brown coloration, hardly distinguishable from that of the merely rinsed hair.
• the hair was substantially dyed.
• Example III A solution was prepared containing:
• This mixture was immediately applied at a temperature of 68 F. to uucolored human hair, conveniently by a brush.
• the wet hair was allowed to remain exposed to the atmosphere for 20 minutes at a temperature at which the wet solution was maintained substantially constant at 60 F. Thereafter, the dark excess of dye was rinsed from the hair with Warm water until the washings were substantially colorless.
• the hair was then gently toweled and finally dried with a warm air current. The hair retained a natural and pleasing dark auburn coloration. It was subsequently gently shampooed with only an insignificant change of hair coloration resulting from even the first shampooing.
• Example IV 0.800 g. D & C Black #1 (C. 1. 246) 0.600 g. D & C Orange #3 (C. I. 27)
• the mixture was immediately applied at a temperature of about 77 to uucolored hair conveniently by a brush.
• Thejwet hair was allowed to remain exposed to the atmosphere for 20 minutes at a temperature at which the evaporation of the water caused some cooling down of the solution.
• the average temperature of 20. minutes exposure time was estimated to be about 75 F.
• Example V A mixture was prepared of:
• Example V1 2.4 g D & c Black #1 c. I. 246) 1.7 g. D & 0 Orange #3 c. I. 27 21 g. Ext. D & c Red #13 c. I. 252
• Example VII 3 yes utlv ixtur aving the. amecomposition as in the preceding example were dissolved in a solvent containing:
• Example VIII 6.2 g. of -a dye mixture 1 having the; same. composition as in the preceding, two exampleswere dissolvedin a solvent; containing:
• A- solution was preparedqcarryingz 0.50 g. D & C Violet #1 (C. I. 697) 2.5 0 g. thioglycolic acid 1.1 g. sodium hydroxide 7.41 ml.” concentrated ammonia aqua q. s. water to make 100 mLpH' 10.4
• the average temperature of the solution was about 64 F. Thereafter, the hairwas well rinsed'and dried. It re-. tained apermanent pronounced bluecoloration;
• Example X A solution was prepared'carrying:
• the solution throughout the total exposure time of 23 minutes was estimated to be about 68 F
• the hair waswellrinsed and dried.
• the hair retained a pronounced blue .colora tion, slightly, duller-and a little more reddish than the.
• Example XI A solution was prepared carrying:
• the fresh solution was chilled to 50 F. and firm.
• Example XII A solut-ion was prepared, carrying 1.65 g. of adyestufif: mixture; having the same composition as in- Ex: ample XI; and
• Example XIII 1 A solution was prepared carrying 1.56 g. ofadyestulf mixture having the same-composition as in Example XII, and d 25.0 ml. propylene glycol 2.5 g. thioglycolic acid.
• Example XIV A solutionv was prepared containing:
• Example XV A mixture, in powder form, consisting of:
• Example XVI A solution was prepared carrying:
• the hair was rinsed and dried. It retained a reddish blond coloration.
• Example XIX A solution was prepared containing 1.65 g. of a dye mixture having the same composition as in Example XIX, and:
• Example XX A solution was prepared containing:
• the wool was incipiently, but weak- 1y, dyed, at ordinary temperatures with'the weakly alkaline mixture of dyestufis.
• Example XXI A solution was prepared carrying 0.300 g. D& Black #1 (c. 1.246 0.088 g. D'& 0 Brown #1 c. I. 234 0.113 g. Ext. 13a 0 Red #13 o. I. 252
• Example Example XXII Wool was treated with the solution and by the method described in Example XXI at 50 F. for 15 minutes. After subsequent rinsing and drying, the wool retained a pronounced permanent, medium gray coloration without any evident alteration of the texture or strength.
• Example XXIII Wool was treated with the solution and in the manner described in Example XXI at pH 8, and at a temperature of 110 F.', for 15 'minutes. After rinsing and drying,
• the wool retained abeautiful velvet black. It had been permanently dyed. No wool damage was evident. The dyed fabric remained soft and pliable.
• Example XXIV' Wool was dyed in the solution and by the process described inExample XXI at pH 6.6, and at a temperature of 110 F., for 15 -minutes. Afterrinsing and drying, the wool retained a permanent, very dark reddish brown coloration, noticeably lighter than the velvet black retained after the identical procedure with a corresponding solution at pH 8.0 as described in Example XXIII.
• a method forthe permanent dyeing of keratinousmaterial which comprises treating the material to be dyed with a freshly prepared aqueous solution containing a quantity of a water soluble mercapto compound oflow" toxicity equivalent .with. respect to, SH group to aboutture-between about 50 F. and 110 F;
• n&' c, D & .C and FD & c certified colors larld mixtures thereof the solution having a pI-I valu'e between 6.6 and 10.4 butnot higher than 9.4 when the mercapto'concentration is equivalent to at least 3 by weight .of the solution of thioglycolic acid and not higher than'f9,15 whenthe mercapto concentration is equivalent tofat least 5.6% byjweight of the solution of thioglycolic acid,'then washingthe dyed hair with an aqueous medium and drying the same.
• a method for the permanent dyeing. of human hair which comprises the steps of treating the hair to be dyed with afreshly'pjrepared aqueous solution of a quantityof a water-soluble mercapto compound of the group consisting of thioglycolic acid, thiosalicylic acid in the form, of its water-solublesalts, thioglycol, thioglycerol and thiophenol equivalent withrespect to SH group to about 1.2%
• a method for the permanent dyeing of human hair which consists of the steps of treating the hair to be dyed at a temperature of between about 50 F. and 110 F. with a freshly prepared aqueous solution of a quantity of a water-soluble mercapto compound of the group consisting of thioglycolic acid, thiosalicylic acid in the form of its water-soluble salts, thioglycol, thioglycerol and thiophenol equivalent with respect to SH group to about 1.2% to 4% by Weight of the solution of thioglycolic acid and containing, as sole coloring agent, about 0.033% to about 6.2% by weight of the solution of a dyestutf of the group consisting of the Ext.
• D & C, D & C and F D & C certified colors and mixtures thereof said solution having a pH value of between 6.6 and 10.4 but not higher than 9.4 when the mercapto concentration is equivalent to at least 3% by weight of the solution of thioglycolic acid, then Washing the dyed hair with an aqueous medium and drying the same.
• a method for the permanent dyeing of human hair which consists of the steps of treating the hair to be dyed at a temperature between about 50 F. and 110 F. with a freshly prepared aqueous solution of a quantity of a Water-soluble mercapto compound of the group consisting of thioglycolic acid, thiosalicylic acid in the form of its water-soluble salts, thioglycol, thioglycerol and thiophenol equivalent with respect to SH group to about 4% to 6% by weight of the solution of thioglycolic acid and containing, as sole coloring agent, about 0.033% to about 6.2% by weight of the solution of a dyestuff of the group consisting of the Ext, D & C, D & C and F D & C certified colors and mixtures thereof, said solution having a pH value between 6.6 and 9.4 but not higher than 9.15 when the mercapto concentration is equivalent to at least 5.6% by weight of the solution of thioglycolic acid, then treating the
• a water-soluble mercapto compound selected from the group consisting of thioglycolic acid, thiosalicylic acid in the form of its water-soluble salts, thioglycol, thioglycerol and thiophenol equivalent with respect to SH group to about 1.2% to 6% by Weight of the solution of thioglycolic acid and, as sole
• D & C, D & C and F D & C certified colors and mixtures thereof said solution having a pH value between 6.6 and 10.4 but not higher than 9.4 when the mercapto concentration is equivalent to at least 3% by Weight of the solution of thioglycolic acid and not higher than 9.15 when the mercapto concentration is equivalent to at least 5.6% by weight of the solution of thioglycolic acid.
• a preparation for the permanent dyeing of keratinous material in the form of a substantially dry powdered mixture comprising a dry water-soluble solid mercapto compound of low toxicity, an ammonium salt, a dry, weakly alkaline water-soluble salt of an alkali metal, and, as sole coloring agent, a dry dyestuff selected from the group consisting of the Ext.
• D & C, D & C and F D & C certified colors and mixtures thereof the several ingredients being present in such proportions that, on addition of the dry powdered mixture to a predetermined quantity of water, a dye solution is formed which contains about 0.033% to about 6.2% by weight of the solution of dyestutf and a quantity of mercapto compound equivalent with respect to SH group to about 0.1% to about 6% by weight of the solution of thioglycolic acid and which has a pH value of between about 6.6 and 11.3.
• a preparation for the permanent dyeing of human hair in the form of a substantially dry powdered mixture comprising a dry water-soluble salt of thioglycolic acid, an ammonium salt, a dry, weakly alkaline watersoluble salt of an alkali metal, and, as sole coloring agent, a dry dyestuff selected from the group consisting of the Ext. D & C, D & C and F D & C certified colors and mixtures thereof, the several ingredients being present in such proportions that, on addition of the dry powdered mixture to a predetermined quantity of water, a dye solution is formed containing about 0.033 to 6.2% b. w.
• a method for the permanent dyeing of keratinous material which comprises the steps of preparing separately an aqueous dye solution containing, as sole coloring agent, a dyestufi selected from the group consisting of the Ext. D & C, D & C and F D & C certified colors and mixtures thereof and a water solution of a Watersoluble mercapto compound, the respective pH values of the two solutions, the total quantity of solvent in both solutions, the relative proportions of the solutions, the concentration of mercapto compound in the mercapto solution and the concentration of dyestufi in the dye solution being such that a mixture of the two solutions contains about 0.033% to about 6.2% by weight of the solution of dyestuff and a quantity of mercapto compound equivalent with respect to SH group to about 0.1% to about 6% by weight of the solution of thioglycolic acid and has a pH value between about 6.6 and about 11.3, combining the two separate solutions to form such mixture, applying the freshly prepared mixture to the keratinous material to be
• a method for the permanent dyeing of human hair which comprises the steps of preparing separately an aqueous dye solution containing, as sole coloring agent, a dyestutf selected from the group consisting of the Ext. D & C, D & C and F D & C certified colors and mixtures thereof and a Water solution of a water-soluble mercapto compound of the group consisting of thioglycolic acid, thiosalicylic acid in the form of its watersoluble salts, thioglycol, thioglycerol and thiophenol, the respective pH values of the two solutions, the total quantity of solvent in both solutions, the relative proportions of the solutions, the concentration of mercapto compound in the mercapto solution and the concentration of dyestuff in the dye solution being such that a mixture of the two solutions contains about 0.033% to about 6.2% by weight of the solution of dyestutr and a quantity of mercapto compound equivalent with respect to SH group to about 1.2% to about 6% by weight of

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Citations (11)

• 1951
  • 1951-06-28 US US234156A patent/US2776668A/en not_active Expired - Lifetime
• 1956
  • 1956-12-27 FR FR1169087D patent/FR1169087A/fr not_active Expired
• 1957
  • 1957-01-04 CH CH350076D patent/CH350076A/fr unknown

Patent Citations (11)

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