CN108403580A - A kind of natural plant pigment hair dye and preparation method thereof and preparation method thereof - Google Patents
A kind of natural plant pigment hair dye and preparation method thereof and preparation method thereof Download PDFInfo
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- CN108403580A CN108403580A CN201810274662.6A CN201810274662A CN108403580A CN 108403580 A CN108403580 A CN 108403580A CN 201810274662 A CN201810274662 A CN 201810274662A CN 108403580 A CN108403580 A CN 108403580A
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- 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
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/35—Ketones, e.g. benzophenone
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- 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
- A61K8/463—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing sulfur containing sulfuric acid derivatives, e.g. sodium lauryl sulfate
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- 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
- A61K8/64—Proteins; Peptides; Derivatives or degradation products thereof
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- 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
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/73—Polysaccharides
- A61K8/731—Cellulose; Quaternized cellulose derivatives
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- 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
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/98—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution of animal origin
- A61K8/981—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution of animal origin of mammals or bird
- A61K8/982—Reproductive organs; Embryos, Eggs
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- 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
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/98—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution of animal origin
- A61K8/981—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution of animal origin of mammals or bird
- A61K8/986—Milk; Derivatives thereof, e.g. butter
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- 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
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/42—Colour properties
- A61K2800/43—Pigments; Dyes
- A61K2800/432—Direct dyes
- A61K2800/4324—Direct dyes in preparations for permanently dyeing the hair
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/59—Mixtures
- A61K2800/592—Mixtures of compounds complementing their respective functions
- A61K2800/5922—At least two compounds being classified in the same subclass of A61K8/18
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Abstract
The present invention relates to a kind of natural plant pigment hair dyes and preparation method thereof, belong to technical field of fine.Sulfydryl is connected on the higher natural plant pigment dyestuff of safety by the present invention becomes reactive dye, when hair dyeing, disulfide bond in hair is opened, sulfydryl in sulfydryl and hair in reactive dye forms disulfide bond and links together, achieve the purpose that permanent stain, it is acted synergistically simultaneously using rabbit hair keratin and soybean protein, protein molecular is set to fold, it is embedded in hydrophobic grouping and the sulfydryl exposure of active site of protein, enhance bio-adhesive performance, promote absorption of the hydrophobic film of hair epicuticula to nutriment, and form film on hair surface, hair is formed and is protected；The present invention is a kind of nontoxic, non-carcinogenesis vegetalitas hair dye, has good hair dyeing effect, and washing fastness, light fastness are good.
Description
Technical field
The present invention relates to a kind of natural plant pigment hair dyes and preparation method thereof, belong to technical field of fine.
Background technology
Hair dye is long as a kind of hair cosmetic applicating history, has formed many systems till now by long-run development
Row, by the popular welcome of consumer.The type of hair dye is various, can be from ingredient, dosage form, form, hair dyeing principle and timeliness
Property etc. many aspects classify.Ancient times, people were once had hair dyed with plant extracts, since p-phenylenediamine, to oxidations such as toluenediamines
After application is in hair dye, synthesizes organic hair dye and develop rapidly, developed so far including oxidation dye, acidity
The various products such as dyestuff, disperse dyes, direct dyes, metal dye.Oxidation dye is since its hair dyeing effect is good, the duration
Advantage long, more than tone type becomes current most widely used hair dyes.
While global hair dye market is developed very fast, having hair dye, there is also the problems of many sternnesses, most of
The problems such as there are toxicity, sensitization, carcinogenicities, damage hair healthy, and coloring effect is poor, easy oxidation discoloration.Due to certain tools
There is the raw material of certain toxicity that safer substance there is no to substitute at present, therefore is still being widely used.P-phenylenediamine is exactly wherein
An example at present for the product of hair dyeing, there is no more preferably raw material to replace although it is more toxic, domestic at present
It is in the great majority in the product of outer hair dyeing or with phenyl amines hair dye, there is very big market.As people are to makeup
The safety issue of product is more and more paid close attention to, and it is extremely urgent to develop the hair dye that a kind of fastness to washing is high, safety is good.
Invention content
The technical problems to be solved by the invention：For existing hair dye, there are toxicity, damage hair healthy, coloring effect
The problem of difference, easy oxidation discoloration, provides a kind of natural plant pigment hair dye and preparation method thereof.
In order to solve the above technical problems, the technical solution adopted by the present invention is：
A kind of natural plant pigment hair dye, including color developing agent and mordant, described color developing agent weight of material part are：0.8~1.2
The modified curcumin of part, 0.15~0.20 part of lauryl sodium sulfate, 5~10 portions of nutrient solutions, 10~15 parts of rabbit hair keratin solutions,
Described mordant weight of material part is：0.5~0.8 part of green vitriol, 1.5~2.0 parts of sodium carboxymethylcelluloses, 0.15~0.20 part ten
8~12 parts of deionized waters are added in sodium dialkyl sulfate.
The modified curcumin is that curcumin is dissolved in dimethylformamide, is mixed instead with thioacetic acid, niter cake
2~3h is answered, vulcanized sodium, ethanol solution, 1~2h of insulation reaction are added, filtration washing drying is made.
The mass ratio of the curcumin and dimethylformamide is 1：15~1：50.
The dosage of the thioacetic acid is 10~30 times of curcumin quality, and the niter cake dosage is curcumin quality
0.6~2.4 times.
The amount of sodium sulfide is 4~10 times of curcumin quality, and the mass fraction of the ethanol solution is 95%, dosage
It is 25~80 times of curcumin quality.
The hybrid reaction temperature is 120~130 DEG C, and the insulation reaction temperature is 120~130 DEG C.
The nutrient solution is by 150~200 parts by weight egg white, 100~120 parts by weight of soybean albumen powders, 200~300 weight
Part milk composition.
The rabbit hair keratin solution be the rabbit hair be dissolved in mass fraction be in 2% sodium hydroxide solution be made.
The mass ratio of the rabbit hair and sodium hydroxide solution is 1：5~1：20.
A kind of preparation method of the natural plant pigment hair dye, the specific steps are：
（1）Curcumin is dissolved in dimethylformamide, with thioacetic acid, niter cake 2~3h of hybrid reaction, must be reacted
Liquid；
（2）Vulcanized sodium, ethanol solution, 1~2h of insulation reaction are added into reaction solution, filtration washing drying obtains modified curcumin；
（3）Egg white, soyabean protein powder are taken, is added in milk and is uniformly mixed, obtain nutrient solution；
（4）It takes the rabbit hair to be dissolved in sodium hydroxide solution, obtains rabbit hair keratin solution；
（5）Modified curcumin, lauryl sodium sulfate, nutrient solution, rabbit hair keratin solution are uniformly mixed, color developing agent is obtained；
（6）By green vitriol, sodium carboxymethylcellulose, lauryl sodium sulfate, mixing in deionized water is added, obtains mordant.
Compared with other methods, advantageous effects are the present invention：
（1）Sulfydryl is connected on the higher natural plant pigment dyestuff of safety by the present invention becomes reactive dye, when hair dyeing, hair
In disulfide bond open, the sulfydryl in sulfydryl and hair in reactive dye forms disulfide bond and links together, and reaches permanent dye
The purpose of color, while having the characteristics that good skin-friendly, nontoxicity and adsorptivity using rabbit hair keratin, it is assisted with soybean protein
Same-action makes protein molecular fold, and hydrophobic grouping and the sulfydryl exposure of active site of protein is embedded in, to enhance dredging for albumen
Water reciprocation enhances the hydrophobic effect and electrostatic interaction of the amino acid residue and hair albumen on albumen, increases albumen
On cysteine residues and hair in glycoprotein mercapto formed disulfide bond, enhance bio-adhesive performance, promote hair
Absorption of the hydrophobic film of epicuticula to nutriment, and film is formed on hair surface, hair is formed and is protected, is gone forward side by side
One step fixes reactive dye and enters in hair the molecule that chelating forms bigger, after the scale of hairline is closed, no longer goes out, is formed
Permanent hairdye；
（2）The present invention is a kind of nontoxic, non-carcinogenesis vegetalitas hair dye, have good hair dyeing effect, and washing fastness,
Light fastness is good.
Specific implementation mode
1~2g curcumins are taken, are added in 30~50g dimethylformamides, 10~15min is stirred with 300~400r/min,
20~30g thioacetic acid, 1.2~2.4g niter cakes are added, and is heated to 120~130 DEG C, insulated and stirred reacts 2~3h,
Reaction solution is obtained, 8~10g vulcanized sodium is added into reaction solution, 50~80g mass fractions are 95% ethanol solution, at 120~130 DEG C
1~2h of lower insulation reaction, is filtered after being cooled to room temperature, and filter residue is washed with deionized 3~5 times, then the filter residue after washing is set
In vacuum drying chamber, is dried to constant weight at 105~110 DEG C, obtain modified curcumin, take 150~200g egg white, 100~
120g soyabean protein powders are added in 200~300mL milk, stir 20~30min with 300~400r/min, obtain nutrient solution, take 1
~2kg the rabbit hairs are washed with deionized clean and are fitted into baking oven, dry 2~3h at 50~55 DEG C, then are transferred to crushing
Broken section of 1~5mm is crushed in machine, 10~20kg mass fractions, which are added, in broken section of the rabbit hair is in 2% sodium hydroxide solution, 80~
3~5h is reacted under 85 DEG C of waters bath with thermostatic control, filters to get filtrate, obtains rabbit hair keratin solution, and 0.8~1.2g is taken to be modified curcumin,
0.15~0.20g lauryl sodium sulfate, 5~10g nutrient solutions, 10~15g rabbit hair keratin solutions, with 200~300r/min
20~30min is stirred, color developing agent is obtained, takes 0.5~0.8g green vitriols, 1.5~2.0g sodium carboxymethylcelluloses, 0.15~0.20g ten
Sodium dialkyl sulfate is added in 8~12mL deionized waters, stirs 20~30min with 300~400r/min, obtains mordant.
1g curcumins are taken, are added in 30g dimethylformamides, 10min is stirred with 300r/min, adds 20g sulfydryl second
Acid, 1.2g niter cakes, and 120 DEG C are heated to, insulated and stirred reacts 2h, obtains reaction solution, and 8g vulcanized sodium is added into reaction solution,
50g mass fractions are 95% ethanol solution, and the insulation reaction 1h at 120 DEG C is filtered after being cooled to room temperature, is washed with deionized
Filter residue 3 times, then the filter residue after washing is placed in vacuum drying chamber, it is dried to constant weight at 105 DEG C, obtains modified curcumin, take
150g egg white, 100g soyabean protein powders are added in 200mL milk, stir 20min with 300r/min, obtain nutrient solution, take 1kg rabbits
Hair is washed with deionized clean and is fitted into baking oven, the dry 2h at 50 DEG C, then is transferred in pulverizer that be crushed to 1mm broken
Broken section of addition 10kg mass fraction of the rabbit hair is to react 3h in 2% sodium hydroxide solution under 80 DEG C of waters bath with thermostatic control, filter by section
Filtrate obtains rabbit hair keratin solution, and 0.8g is taken to be modified curcumin, 0.15g lauryl sodium sulfate, 5g nutrient solutions, 10g rabbit hairs angle
Protein solution stirs 20min with 200r/min, obtains color developing agent, take 0.5g green vitriols, 1.5g sodium carboxymethylcelluloses, 0.15g 12
Sodium alkyl sulfate is added in 8mL deionized waters, stirs 20min with 300r/min, obtains mordant.
1.5g curcumins are taken, are added in 40g dimethylformamides, 13min is stirred with 350r/min, adds 25g sulfydryls
Acetic acid, 1.8g niter cakes, and 125 DEG C are heated to, insulated and stirred reacts 2.5h, obtains reaction solution, and 9g sulphur is added into reaction solution
Change sodium, 65g mass fractions are 95% ethanol solution, and the insulation reaction 1h at 125 DEG C filters after being cooled to room temperature, uses deionized water
It washs filter residue 4 times, then the filter residue after washing is placed in vacuum drying chamber, dried to constant weight at 107 DEG C, obtain modified turmeric
Element, takes 175g egg white, 110g soyabean protein powders to be added in 250mL milk, stirs 25min with 350/min, obtains nutrient solution, take
The 1kg rabbit hairs are washed with deionized clean and are fitted into baking oven, the dry 2h at 53 DEG C, then are transferred in pulverizer and are crushed to
Broken section of addition 15kg mass fraction of the rabbit hair is to react 4h under 83 DEG C of waters bath with thermostatic control in 2% sodium hydroxide solution by broken section of 3mm,
It filters to get filtrate, obtains rabbit hair keratin solution, 1.0g is taken to be modified curcumin, 0.17g lauryl sodium sulfate, 7g nutrient solutions, 13g
Rabbit hair keratin solution stirs 25min with 250r/min, obtains color developing agent, take 0.65g green vitriols, 1.75g sodium carboxymethylcelluloses,
0.17g lauryl sodium sulfate is added in 10mL deionized waters, stirs 25min with 350r/min, obtains mordant.
2g curcumins are taken, are added in 50g dimethylformamides, 15min is stirred with 400r/min, adds 30g sulfydryl second
Acid, 2.4g niter cakes, and 130 DEG C are heated to, insulated and stirred reacts 3h, obtains reaction solution, and 10g vulcanizations are added into reaction solution
Sodium, 80g mass fractions are 95% ethanol solution, and the insulation reaction 2h at 130 DEG C is filtered after being cooled to room temperature, is washed with deionized water
It washs filter residue 5 times, then the filter residue after washing is placed in vacuum drying chamber, dried to constant weight at 110 DEG C, obtain modified curcumin,
It takes 200g egg white, 120g soyabean protein powders to be added in 300mL milk, 30min is stirred with 400r/min, nutrient solution is obtained, takes 2kg
The rabbit hair is washed with deionized clean and is fitted into baking oven, the dry 3h at 55 DEG C, then is transferred in pulverizer and is crushed to 5mm
Broken section, 20kg mass fractions are added as in 2% sodium hydroxide solution, 5h is reacted under 85 DEG C of waters bath with thermostatic control for broken section in the rabbit hair, are filtered
Filtrate is obtained, rabbit hair keratin solution is obtained, 1.2g is taken to be modified curcumin, 0.20g lauryl sodium sulfate, 10g nutrient solutions, 15g rabbits
Feather keratin solution stirs 30min with 300r/min, obtains color developing agent, take 0.8g green vitriols, 2.0g sodium carboxymethylcelluloses, 0.20g
Lauryl sodium sulfate is added in 12mL deionized waters, stirs 30min with 400r/min, obtains mordant.
The hair dye of a kind of natural plant pigment hair dye and the production of Guangzhou company prepared by the present invention is detected,
Specific testing result such as following table table 1：
1 natural plant pigment hair dye performance characterization of table
The natural plant pigment hair dye that as shown in Table 1 prepared by the present invention, washing fastness is good, colour-fast after solarization, light fastness
Good, the hair color contaminated is natural, glossy, and dyeing time is short.
Claims (10)
1. a kind of natural plant pigment hair dye, including color developing agent and mordant, which is characterized in that the color developing agent weight of material
Part it is：0.8~1.2 part of modified curcumin, 0.15~0.20 part of lauryl sodium sulfate, 5~10 portions of nutrient solutions, 10~15 portions of rabbits
Feather keratin solution, described mordant weight of material part are：0.5~0.8 part of green vitriol, 1.5~2.0 parts of sodium carboxymethylcelluloses,
8~12 parts of deionized waters are added in 0.15~0.20 part of lauryl sodium sulfate.
2. a kind of natural plant pigment hair dye as described in claim 1, which is characterized in that the modified curcumin is turmeric
Element is dissolved in dimethylformamide, and with thioacetic acid, niter cake 2~3h of hybrid reaction, it is molten to add vulcanized sodium, ethyl alcohol
Liquid, 1~2h of insulation reaction, filtration washing drying are made.
3. a kind of natural plant pigment hair dye as claimed in claim 2, which is characterized in that the curcumin and dimethyl methyl
The mass ratio of amide is 1：15~1：50.
4. a kind of natural plant pigment hair dye as claimed in claim 2, which is characterized in that the dosage of the thioacetic acid is
10~30 times of curcumin quality, the niter cake dosage are 0.6~2.4 times of curcumin quality.
5. a kind of natural plant pigment hair dye as claimed in claim 2, which is characterized in that the amount of sodium sulfide is turmeric
The mass fraction of 4~10 times of quality amount, the ethanol solution is 95%, and dosage is 25~80 times of curcumin quality.
6. a kind of natural plant pigment hair dye as claimed in claim 2, which is characterized in that the hybrid reaction temperature is
120~130 DEG C, the insulation reaction temperature is 120~130 DEG C.
7. a kind of natural plant pigment hair dye as described in claim 1, which is characterized in that the nutrient solution is by 150~200
Parts by weight egg white, 100~120 parts by weight of soybean albumen powders, 200~300 parts by weight milk composition.
8. a kind of natural plant pigment hair dye as described in claim 1, which is characterized in that the rabbit hair keratin solution is
It is to be made in 2% sodium hydroxide solution that the rabbit hair, which is dissolved in mass fraction,.
9. a kind of natural plant pigment hair dye as claimed in claim 8, which is characterized in that the rabbit hair and sodium hydroxide are molten
The mass ratio of liquid is 1：5~1：20.
10. a kind of preparation method of natural plant pigment hair dye as claimed in any one of claims 1 to 9 wherein, feature exist
In, the specific steps are：
（1）Curcumin is dissolved in dimethylformamide, with thioacetic acid, niter cake 2~3h of hybrid reaction, must be reacted
Liquid；
（2）Vulcanized sodium, ethanol solution, 1~2h of insulation reaction are added into reaction solution, filtration washing drying obtains modified curcumin；
（3）Egg white, soyabean protein powder are taken, is added in milk and is uniformly mixed, obtain nutrient solution；
（4）It takes the rabbit hair to be dissolved in sodium hydroxide solution, obtains rabbit hair keratin solution；
（5）Modified curcumin, lauryl sodium sulfate, nutrient solution, rabbit hair keratin solution are uniformly mixed, color developing agent is obtained；
（6）By green vitriol, sodium carboxymethylcellulose, lauryl sodium sulfate, mixing in deionized water is added, obtains mordant.
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| CN201810274662.6A CN108403580A (en) | 2018-03-30 | 2018-03-30 | A kind of natural plant pigment hair dye and preparation method thereof and preparation method thereof |
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| CN201810274662.6A CN108403580A (en) | 2018-03-30 | 2018-03-30 | A kind of natural plant pigment hair dye and preparation method thereof and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020026161A1 (en) * | 2018-07-31 | 2020-02-06 | Wool Research Organisation Of New Zealand Incorporated | Keratin compositions |
| CN112336643A (en) * | 2020-10-10 | 2021-02-09 | 中芯生物科技(浙江)有限公司 | Application of fibroin as carrier of hair dye and hair dyeing method |
| CN112411203A (en) * | 2020-10-13 | 2021-02-26 | 武汉纺织大学 | Red Lyocell fabric prepared by dyeing with plant dye hippeastrum and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020026161A1 (en) * | 2018-07-31 | 2020-02-06 | Wool Research Organisation Of New Zealand Incorporated | Keratin compositions |
| CN112969448A (en) * | 2018-07-31 | 2021-06-15 | 新西兰羊毛研究组织 | Keratin composition |
| CN112336643A (en) * | 2020-10-10 | 2021-02-09 | 中芯生物科技(浙江)有限公司 | Application of fibroin as carrier of hair dye and hair dyeing method |
| CN112336643B (en) * | 2020-10-10 | 2022-07-19 | 中芯生物科技(浙江)有限公司 | Application of fibroin as carrier of hair dye and hair dyeing method |
| CN112411203A (en) * | 2020-10-13 | 2021-02-26 | 武汉纺织大学 | Red Lyocell fabric prepared by dyeing with plant dye hippeastrum and preparation method thereof |
| CN112411203B (en) * | 2020-10-13 | 2022-11-29 | 武汉纺织大学 | Red Lyocell fabric prepared by dyeing with plant dye hippeastrum and preparation method thereof |
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