Patent US3960476A successfully refreshed from Google Patents.
US3960476A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Lyophilized and spray dried dyes
Assignee: Individual
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Filing: 1974-04-15
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Granted: 1976-06-01
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Expires: 1994-04-15
Abstract
Abstract A process for producing a dye in powder form involves reacting an oxidation agent with an oxidation base in an aqueous alkaline preferably ammoniacal medium having a pH ranging from 8 to 13 at a temperature and during a period of time allowing at least a partial oxidation, preferably between 15°-30°C for a period of about 5 minutes to 30 hours and lyophilizing or spray-drying the resulting reaction product. The resulting dye can be used to color keratinic fibers, especially human hair.This is a continuation of application Ser. No. 120,353 filed March 2, 1971 now abandoned.
Inventors
- 👤 Giuliana Ghilardi
- 👤 Pierre Bore
- 👤 Jean-Francois Grollier
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-02 15:31
CPC Classifications
C; C09; C09B; C09B67/00; C09B67/0001; C09B67/0003; A; A61; A61K; A61K8/00; A61K8/02; A61K8/18; A61K8/30; A61K8/40; A61K8/41; A61K8/413; A61Q; A61Q5/00; A61Q5/10; C09B53/00; C09B53/02
Claims Analysis
Total Claims: 19
Claim 1
Independent Claim
148 words
A process for producing a lyophilized dyestuff comprising reacting with a molar excess of hydrogen peroxide an oxidation base in an aqueous alkaline solution open to ambient atmosphere and having a pH ranging from 8 to 13 at a temperature between about 15°-30°C for a period of about 5 minutes to 30 hours and lyophilizing said raction mixture, said oxidation base being selected from the group consisting of paratoluylene diamine, paraphenylene diamine, N,N-dimethyl paraphenylene diamine, chloroparaphenylene diamine, 2-methoxy-5-methyl paraphenylene diamine, 2,6-dimethyl-3methoxy paraphenylene diamine, tetramethyl paraphenylene diamine, 2-methoxy paraphenylene diamine, para aminophenol, 2,6-dimethyl para aminophenol, 2,4-diamino anisole, 2-methyl para aminophenol, the hydrochlorides thereof, and mixtures thereof, wherein lyophilizing said reaction mixture comprises freezing said reaction mixture at a temperature of about -200°C to -60°C and subliming said frozen mixture at a temperature of about -50°C to -30°C at a pressure of about 0.01 mm Hg to 0.1 mm Hg.
Claim 2
Dependent Claim
148 words
A process for producing a lyophilized dyestuff comprising reacting with a molar excess of hydrogen peroxide an oxidation base in an aqueous alkaline solution open to ambient atmosphere and having a pH ranging from 8 to 13 at a temperature between about 15°-30°C for a period of about 5 minutes to 30 hours and lyophilizing said raction mixture, said oxidation base being selected from the group consisting of paratoluylene diamine, paraphenylene diamine, N,N-dimethyl paraphenylene diamine, chloroparaphenylene diamine, 2-methoxy-5-methyl paraphenylene diamine, 2,6-dimethyl-3methoxy paraphenylene diamine, tetramethyl paraphenylene diamine, 2-methoxy paraphenylene diamine, para aminophenol, 2,6-dimethyl para aminophenol, 2,4-diamino anisole, 2-methyl para aminophenol, the hydrochlorides thereof, and mixtures thereof, wherein lyophilizing said reaction mixture comprises freezing said reaction mixture at a temperature of about -200°C to -60°C and subliming said frozen mixture at a temperature of about -50°C to -30°C at a pressure of about 0.01 mm Hg to 0.1 mm Hg.
Claim 3
Dependent Claim
34 words
The process of claim 1 which also includes desorbing the lyophilized reaction product at a temperature ranging between 15°-60°C at a pressure of about 0.01 mm Hg to eliminate therefrom any residual moisture content.
Claim 4
Dependent Claim
15 words
The process of claim 1 wherein said aqueous alkaline solution is an aqueous ammoniacal solution.
Claim 5
Dependent Claim
66 words
The process of claim 1 wherein said oxidation base and said hydrogen peroxide are reacted in the presence of a coupler selected from the group consisting of metaphenylene diamine, 2,4-diamino toluene, metal aminophenol, 6-methyl-3-aminophenol, N-methyl meta aminophenol, 4-methoxy-3-aminophenol, resorcin, α-naphthol, 3-methoxy-4-aminophenol and the sulfate, hydrochloride and hydrobromide thereof, the molar ratio of said coupling agent to said oxidation base before oxidation being between 0:1 and 10:1.
Claim 6
Dependent Claim
23 words
The process of claim 4 wherein the molar ratio of said coupler to said oxidation base before oxidation is between 0:1 and 2:1.
Claim 7
Dependent Claim
123 words
The process of claim 1 wherein said hydrogen peroxide and said oxidation base are reacted in the presence of a filler selected from the group consisting of hydrolysis products of proteins, alanine, glycine, glutamic acid, cystine, polyvinyl pyrrolidone having a molecular weight ranging between 40,000 to 360,000, a copolymer of polyvinyl pyrrolidone and vinyl acetate having a molecular weight ranging between 40,000 to 160,000 wherein the weight ratio of polyvinyl pyrrolidone to vinyl acetate is 70%:30% to 30%:70% and a copolymer of crotonic acid and vinyl acetate having a molecular weight of 40,000 to 200,000 wherein the weight ratio of crotonic acid to vinyl acetate is 90%:10%, said filler being present in amounts of 1-20 percent by weight of the total reaction mixture.
Claim 8
Dependent Claim
14 words
A dye in powder form made in accordance with the process of claim 1.
Claim 9
Dependent Claim
135 words
A process for producing a spray-dried dye comprising reacting an oxidation base with a molar excess of hydrogen peroxide in an aqueous alkaline solution open to ambient atmosphere and having a pH ranging from 8 to 13 at a temperature between about 15°-30°C for a period of about 5 minutes to 30 hours and spray drying said reaction mixture, said oxidation base being selected from the group consisting of paratoluylene diamine, paraphenylene diamine, N,N-dimethyl paraphenylene diamine, chloroparaphenylene diamine, 2-methoxy5-methyl paraphenylene diamine, 2,6-dimethyl-3-methoxy paraphenylene diamine, tetramethyl paraphenylene diamine, 2-methoxy paraphenylene diamine, para aminophenol, 2,6-dimethyl para aminophenol, 2,4-diamino anisole, 2-methyl para aminophenol, the hydrochlorides thereof, and mixtures thereof, wherein spray drying said reaction mixture comprises introducing said reaction mixture into a current of air having an inlet temperature between 80°-350°C and an outlet temperature between about 50°-200°C.
Claim 10
Dependent Claim
135 words
A process for producing a spray-dried dye comprising reacting an oxidation base with a molar excess of hydrogen peroxide in an aqueous alkaline solution open to ambient atmosphere and having a pH ranging from 8 to 13 at a temperature between about 15°-30°C for a period of about 5 minutes to 30 hours and spray drying said reaction mixture, said oxidation base being selected from the group consisting of paratoluylene diamine, paraphenylene diamine, N,N-dimethyl paraphenylene diamine, chloroparaphenylene diamine, 2-methoxy5-methyl paraphenylene diamine, 2,6-dimethyl-3-methoxy paraphenylene diamine, tetramethyl paraphenylene diamine, 2-methoxy paraphenylene diamine, para aminophenol, 2,6-dimethyl para aminophenol, 2,4-diamino anisole, 2-methyl para aminophenol, the hydrochlorides thereof, and mixtures thereof, wherein spray drying said reaction mixture comprises introducing said reaction mixture into a current of air having an inlet temperature between 80°-350°C and an outlet temperature between about 50°-200°C.
Claim 11
Dependent Claim
21 words
The process of claim 8 wherein the inlet air temperature ranges between 150°-300°C and the outlet air temperature ranges between 80°-130°C.
Claim 12
Dependent Claim
21 words
The process of claim 8 wherein the inlet air temperature is about 300°C and the outlet air temperature is about 100°C.
Claim 13
Dependent Claim
15 words
The process of claim 8 wherein said aqueous alkaline solution is an aqueous ammoniacal solution.
Claim 14
Dependent Claim
61 words
The process of claim 8 wherein said hydrogen peroxide and said oxidation base are reacted in the presence of a coupler selected from the group coonsisting of metaphenylene diamine, 2,4-diamino toluene, meta aminophenol, 4-methoxy-3aminophenol, resorcin, α-naphthol, 3-methoxy-4-aminophenol and the sulfate, hydrochloride and hydrobromide thereof, the molar ratio of said coupler to said oxidation base before oxidation being between 0:1 to 10:1.
Claim 15
Dependent Claim
23 words
The process of claim 12 wherein the molar ratio of said coupler to said oxidation base before oxidation is between 0:1 and 2:1.
Claim 16
Dependent Claim
123 words
The process of claim 8 wherein said hydrogen peroxide and said oxidation base are reacted in the presence of a filler selected from the group consisting of hydrolysis products of proteins, alanine, glycine, glutamic acid, cystine, polyvinyl pyrrolidone having a molecular weight ranging between 40,000 to 360,000, a copolymer of polyvinyl pyrrolidone and vinyl acetate having a molecular weight ranging between 40,000 to 160,000 wherein the weight ratio of polyvinyl pyrrolidone to vinyl acetate is 70%:30% to 30%:70% and a copolymer of crotonic acid and vinyl acetate having a molecular weight of 50,000 to 200,000 wherein the weight ratio of crotonic acid to vinyl acetate is 90%:10%, said filler being present in amounts of 1-20 percent by weight of the total reaction mixture.
Claim 17
Dependent Claim
14 words
A dye in powder form made in accordance with the process of claim 8.
Claim 18
Dependent Claim
71 words
A two component pack which comprises, as the first component, a dye made in accordance with the process of claim 1 and as the second component a cosmetic carrier for said dye, said carrier comprising a member selected from the group consisting of water, lower alkanol selected from the group consisting of ethanol and isopropanol and an aqueous solution of said lower alkanol containing 1-96 weight percent of said lower alkanol.
Claim 19
Dependent Claim
71 words
A two component pack which comprises, as the first component a dye made in accordance with the process of claim 8 and as the second component a cosmetic carrier for said dye, said carrier comprising a member selected from the group consisting of water, lower alkanol selected from the group consisting of ethanol and isopropanol and an aqueous solution of said lower alkanol containing 1-96 weight percent of said lower alkanol.
References Cited (Backward Citations)
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1979-06-01 | 1979-12-01 | 1980-06-01 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1983-06-01 | 1983-12-01 | 1984-06-01 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1987-06-01 | 1987-12-01 | 1988-06-01 | $7700.00 | Window Closed / Lapsed |