CN111329805A - Preparation method of novel natural madder graphene hair dye - Google Patents
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Abstract
The invention discloses a formula and a preparation technology of a madder-graphene-chitosan combined natural plant hair dye, and relates to the technical field of natural plant hair dyeing. The method comprises the following steps: harmless dye preparation, technical requirements, high hair dye adsorption rate and high-efficiency preparation process. The formula and preparation technology of the natural plant hair dye combined with graphene and chitosan according to the claims are characterized in that: 1) the ultrasonic-assisted extraction of the alizarin extracting solution in the madder plant as the basic color of the coloring agent solves the problem that the chemical hair dye contains aniline derivatives to cause human body damage; 2) reducing graphene oxide by using ascorbic acid, wherein the reduced graphene and chitosan interact to enhance the adhesion capability of the reduced graphene and the chitosan; 3) preparing a preparation method of the graphene-chitosan gel; 4) on the basis of reference and citation of similar standards, a natural plant hair dye formula combining graphene and chitosan and a preparation technology are formulated through combination of experimental tests and ingredient updating, and the blank of the project is filled.
Description
Technical Field
The invention relates to the technical field of natural plant type hair dyeing, in particular to a formula and a preparation technology of a novel natural madder graphene hair dye.
Background
In recent years, various types of hair dyes are available on the market, wherein the oxidative hair dyes have the advantages of good dyeing effect, long retention time, wide color tone range and the like, so that the hair dyes have more than 80% of market share in Europe, America and China, and are mainstream products in the current market. But the aniline derivatives have certain toxicity and sensitization as the main raw materials, are very easy to be absorbed by skin and hair to cause serious adverse reactions, such as local extreme itching and red swelling, can cause cancer in serious cases, and even cause poisoning and death. Therefore, the hair dye is always above the wave tip of the wind head. While pursuing individuality, the hair dyes are concerned. Therefore, there is an urgent need for a truly non-toxic, non-harmful, natural hair dye.
At present, the related patents of the natural plant type hair dyes in China are as follows:
the invention relates to a graphene modified hair dye, which comprises a hair dye and a color developing agent, wherein the hair dye comprises a graphene modified hair dye and a color developing agent, wherein the graphene modified hair dye is prepared from a graphene technology limited company of south China patent (application number) 201711395380.3 (invention name) and a graphene technology limited company of south China (applicant) (contact address) 226400 northside of Jiangsu province, south China city, such as east county, economic development area, Jialing Jianlu (abstract); the hair dye comprises the following components in percentage by mass; 5.0-15.0 parts of graphene modified gallic acid, 10.0-15.0 parts of an auxiliary agent, 15.0-25.0 parts of a cosolvent, 50.0-60.0 parts of distilled water and 50.0-60.0 parts of distilled water. And through gallic acid after the graphite alkene is modified, also can have the graphite alkene microchip on the dyeing molecule that dyeing agent that is connected with the graphite alkene microchip and color developing agent reaction generated, the graphite alkene of suitable particle size is the graphite alkene microchip, and the card that the graphite alkene microchip of suitable particle size can be firm is in the hair flake, is difficult for droing from the hair, prolongs the dyeing effect.
The invention relates to a natural plant hair dye < applicant > application number >201710163553.2< invention name > Chinese patent < application number > and < invention name > Xiaoshijiyuan < contact address >050000 Yuhua area of stone house city in Hebei province and Yuhua area sports south street century Jiatai mansion C seat 1033 < abstract > belonging to the field of hair dye, and providing a natural plant hair dye, which mainly comprises the following components: the hair dye adopts pure natural non-toxic plants as main raw materials of the hair dye, is rich in natural nutrient components, has the advantages of no irritation, no allergy and the like, is not easy to fade after being colored, and has the effects of nourishing and protecting hair after being used for a long time. The invention is suitable for dyeing hair.
The invention discloses a Chinese patent < application No. > 201610609576.7 < invention name > a paste natural plant hair dye < applicant > Changzhou Meisheng biomaterial limited company < contact address >213164 building A1001< abstract > of Chun Su province Changzhou city, Wu enter district science and education city, Increation Port 1, belonging to the field of hair dyes, and providing a paste natural plant hair dye, which mainly comprises the following components: the ointment is prepared from Indigofera tinctoria, henna, bacopa monnieri, madder, acacia, emblic leafflower fruit, catechu, coffee tree, eclipta alba, a penetrating agent, an absorbent, a thickening agent and deionized water. The hair dye adopts pure natural non-toxic plants as main raw materials, is rich in natural nutrients, has no irritation and allergy, and has effects of nourishing and caring hair after long-term use.
Research reports that toxic components in the original hair dye are replaced by graphene oxide, so that a safer hair dye is obtained. The invention develops a novel natural nontoxic hair dye on the basis of the characteristics, and the novel natural graphene madder plant hair dye which is safe, nontoxic, non-allergic and non-irritant is prepared by utilizing the performances of high surface area, flexibility, electric conductivity, heat conductivity, antibiosis and the like of graphene and matching with a madder natural plant extraction dye solution.
Disclosure of Invention
The invention extracts alizarin in madder plants as basic color of a coloring agent by ultrasonic wave assistance. The graphene oxide is reduced by using ascorbic acid to obtain the graphene with high surface area and high flexibility, the graphene can strongly interact with chitosan through hydrogen bonds, and the chitosan is further strongly combined with keratin on the hair surface through amino and hydroxyl groups of the chitosan and is attached to the hair surface to form a smooth coating. Meanwhile, due to the characteristic of amphipathy of the graphene oxide, the alizarin can be well attached to the surface of the hair, and the gel formed by the chitosan and the ascorbic acid can enhance the attachment capability of the gel, so that the hair dyeing effect is achieved. Thereby preparing a safe and nontoxic novel natural madder graphene hair dye.
The method extracts the alizarin in the madder by ultrasonic waves, and utilizes the ultrasonic waves to generate strong vibration, high acceleration, strong cavitation effect, thermal effect, stirring effect and the like to destroy cells of plants, so that a solvent can permeate into the cells, and the leaching and extraction of effective components in the cells are accelerated.
The graphene oxide is subjected to partial reduction treatment by ascorbic acid to obtain a reduced graphene sheet, which has a large transverse dimension, generally several microns or tens of microns, has high flexibility, and does not penetrate through dermis. The graphene oxide has amphipathy, and can be well attached to the surface of hair to form a smooth and continuous coating similar to a coating. The graphene oxide and the reduced graphene can strongly interact with the chitosan through hydrogen bonds, so that the dispersibility of the graphene is improved, the chitosan is strongly combined with keratin on the surface of hair through amino and hydroxyl of the chitosan, and the chitosan is used as a dispersing agent to form a gel with ascorbic acid, so that the adhesion capability of the chitosan is improved.
Mixing the extracted alizarin, the reduced graphene and the chitosan gel according to different proportions to obtain a series of hair dyes with different colors, and uniformly coating the hair dyes on hair to achieve the effect of dyeing the hair.
The hair dye prepared from the madder extract and the chitosan gel has obvious effect and is not easy to fade, and the madder extract and the chitosan gel can be well attached to the surface of hair.
The hair dye prepared from the graphene and the chitosan gel has an obvious effect and is not easy to fade, and the result shows that the graphene has a strong adhesion effect while playing a color development effect.
The hair dye prepared from the madder extract and the graphene-chitosan gel according to different proportions has the effect after hair dyeing, and the madder graphene hair dye is based on brown and gray. When the amount of the madder root extract is more than the amount of the madder root extract, the color is brown. When the dosage of the graphene-chitosan gel is more, the color is grayish green. The overall color appeared to have a distinct color system gradient.
The color fastness test shows that the color of the whole detergent after being washed for the first time by the washing liquid is not changed greatly, and the color becomes light after being washed for ten times by continuous rubbing, but the original color can not be faded, so that two obvious brown and gray systems can be maintained. The hair dye has strong color fastness and washing fastness after dyeing, and the color can be kept for a long time.
Therefore, the novel natural madder graphene hair dye prepared by the experiment can be positioned into a semi-permanent natural, safe and nontoxic hair dye. The hair-whitening mask is suitable for congenital defect teenager hair-whitening, middle-aged and elderly people hair-whitening, European and American people and the like, and has extremely high research and development values and popularization values.
Description of the optimal raw material ratio:
1. extraction of alizarin
Accurately weighing 30.0 g of sieved madder, adding 300 mL of 70% ethanol solution, performing ultrasonic treatment at 40 ℃ for 20 min, and filtering to obtain filtrate for later use.
2. Preparation of reduced graphene
Accurately measuring 50mL of 10mg/mL graphene oxide solution into a 250 mL round-bottom flask, then accurately measuring 50mL of 50 mg/mL ascorbic acid solution, stirring and heating at 90 ℃ for 1 hour, centrifuging at 10000r/min for 5 min, and washing with deionized water for 3 times to obtain a black product reduced graphene.
Preparation of Chitosan gel
Accurately weighing 300 mL of 2.5 mg/mL ascorbic acid solution into a 500 mL beaker, then accurately weighing 0.75 g of chitosan, and uniformly stirring the weighed chitosan and ascorbic acid solution in a water bath at 60 ℃ to obtain chitosan gel.
4. Preparation of graphene-chitosan gel
Measuring 200mL of chitosan gel, adding the reduced graphene prepared in 6.2, and uniformly mixing to obtain the graphene-chitosan gel.
5. Arrangement of other reagents
Preparation of 70% ethanol solution: weighing 3-4 parts of ethanol in a volumetric flask, and adding deionized water to a certain volume.
Preparation of 5 mg/mL graphene oxide: weighing a proper amount of graphene oxide in a beaker, adding a small amount of deionized water to dissolve the graphene oxide, and then fixing the volume.
Preparation of 50 mg/mL ascorbic acid solution: weighing a proper amount of ascorbic acid in a beaker, adding a small amount of deionized water to dissolve the ascorbic acid, and then fixing the volume.
Preparation of 2.5 mg/mL ascorbic acid solution: weighing a proper amount of ascorbic acid in a beaker, adding a small amount of deionized water to dissolve the ascorbic acid, and fixing the volume.
The preparation of the washing liquid comprises the steps of weighing 2.5 g of sodium dodecyl benzene sulfonate into a 250 ml beaker, adding 250 ml of distilled water, heating to 60 ℃ in a water bath, completely dissolving and cooling, slowly transferring into a 500 ml volumetric flask, washing the beaker with deionized water for three times, transferring into the volumetric flask, and carrying out constant volume to obtain 5.0 mg/ml of washing liquid.
Technical scheme
1. Extracting alizarin: accurately weighing 30.0 g of sieved madder, adding 300 mL of 70% ethanol solution, performing ultrasonic treatment at 40 ℃ for 20 min, and filtering to obtain filtrate for later use.
2. Preparing reduced graphene: accurately measuring 50mL of 10mg/mL graphene oxide solution into a 250 mL round-bottom flask, then accurately measuring 50mL of 50 mg/mL ascorbic acid solution, stirring and heating at 90 ℃ for 1 hour, centrifuging at 10000r/min for 5 min, and washing with deionized water for 3 times to obtain a black product reduced graphene.
3. Preparation of chitosan gel: accurately weighing 300 mL of 2.5 mg/mL ascorbic acid solution into a 500 mL beaker, then accurately weighing 0.75 g of chitosan, and uniformly stirring the weighed chitosan and ascorbic acid solution in a water bath at 60 ℃ to obtain chitosan gel.
4. Preparing graphene-chitosan gel: measuring 200mL of chitosan gel, adding the reduced graphene prepared in 6.2, and uniformly mixing to obtain the graphene-chitosan gel.
Mixing the madder root extract and the graphene-chitosan gel to obtain hair dyes in different proportions:
hair dye style 1 ratio of madder extract to graphene-chitosan gel 5:1
Hair dye style 2 ratio of madder extract to graphene-chitosan gel 4:1
Hair dye style 3 ratio of madder extract to graphene-chitosan gel 3:1
Hair dye style 4 proportion of madder extract to graphene-chitosan gel 2:1
Hair dye style 5 Rubia cordifolia extract and graphene-chitosan gel in a ratio of 1:1
Hair dye style 6 the proportion of madder extract to graphene-chitosan gel is 1:2
Hair dye style 7 the proportion of madder extract to graphene-chitosan gel is 1:3
Hair dye style 8 the proportion of madder extract to graphene-chitosan gel is 1:4
Hair dye style 9 madder extract and graphene-chitosan gel in a ratio of 1:5
The proportions of the madder extract and the graphene-chitosan gel are different, the colors are different, the proportions of the madder extract in samples 1 to 4 are more, and the color gradually changes from dark brown to ash; the sample 5 is prepared by mixing the madder root extract and the graphene-chitosan gel in a ratio of 1:1, and the color is ochre lime; the graphene-chitosan gel ratio of samples 6 to 9 is more, and the color gradually changes from green brown to grey green.
Description of the drawings:
fig. 1 shows different colors (black and white images show different gray scales) of the madder extract and the graphene-chitosan gel in different proportions.
Detailed Description
The method comprises the following steps: the hair was rinsed and then wiped dry (retaining some water).
Step two: the hair dye is smeared on hair, and the hair is wrapped by a hot towel for 30-40 minutes or wrapped by a preservative film and uniformly blown by a blower for about fifteen minutes.
Step three: the hair is washed with warm water.
Step four: after hair dyeing, the hair conditioner and the anti-hair loss film are matched according to the self requirement in the daily hair washing process, so that the hair dyeing lasting effect is better.
The experiment creatively extracts the alizarin extracting solution in the madder plant as the basic color of the coloring agent through ultrasonic wave assistance. The graphene oxide is reduced by using ascorbic acid to obtain the graphene with high surface area and high flexibility, the graphene can strongly interact with chitosan through hydrogen bonds, and the chitosan is further strongly combined with keratin on the hair surface through amino and hydroxyl groups of the chitosan and is attached to the hair surface to form a smooth coating. Meanwhile, due to the characteristic of amphipathy of the graphene oxide, the alizarin can be well attached to the surface of the hair, and the gel formed by the chitosan and the ascorbic acid can enhance the attachment capability of the gel, so that the hair dyeing effect is achieved. Thereby preparing a safe and nontoxic novel natural madder graphene hair dye. And testing the related performances such as color fastness and the like.
International patent application No. PCT/CN2016/074428 discloses a hair-darkening dyeing composition, which employs one or more of chitin, chitosan, gelatin, silicone oil and resin as a hair dye, but the adsorption rate of chitin, chitosan and gelatin to protein fibers such as hair is low, so the invention needs to overcome this deficiency. The preparation of the novel natural madder graphene hair dye well utilizes the graphene and the chitosan to solve the problem.
Chinese patent application No. 201711395380.3 discloses a graphene modified hair dye, which is prepared by dispersing graphene in an aqueous solution, adding gallic acid, and stirring at 50-80 deg.C for 6-8 hr; in the hair dyeing process, the dyeing agent A is required to be kept for 30-40 minutes firstly, and then the color developing agent B is required to be kept for 30-40 minutes, so that the problems of resource waste, difficulty in acceptance of enterprises and common people and the like can be caused in the aspects of industrial preparation and use. The novel natural madder graphene hair dye is prepared by stirring reduced graphene for about one hour at high temperature, mixing the reduced graphene with prepared chitosan to prepare graphene for coagulation, and further mixing the graphene with an madder extracting solution obtained by ultrasonic waves and the like to prepare the hair dye; the using time of the hair dye is shortened by half, the problem of long time consumption in preparation and use of the hair dye is well solved, and the hair dye is easier to accept by people and put into production and use.
The main material used for preparing the medicine is madder which is distributed in northeast, northwest and northwest China, Sichuan China, Tibet China and the like. Is usually in sparsely, forest borders, shrubs or grasslands, is distributed in the regions of korea, japan and russia far east, has abundant resources, and is a plant dye with a long history. On the industrial level, the cost of the raw material is low. From the aspect of putting into the market for use, the hair dye is easier to be accepted by common people compared with other products which are expensive and have the same hair dyeing effect.
Most of hair dyes, which are composed of chemically synthesized pigments, are harmful to hair itself, and if they are inadvertently stuck to the scalp, they cause problems such as loss of hair or increase of dandruff, and in severe cases, they are also allergic. Some poor hair dyes also have a harsh taste. In life, a plurality of customers can reflect the problems that the scalp feels scorching and stabbing when dyeing hair, the hair dyeing experience is poor and the like, and the novel natural madder graphene hair dye well solves the problem. Due to the fusion of the madder root, the novel natural madder graphene hair dye can not stimulate the scalp when in use to cause the phenomena of dandruff increase and stabbing pain after hair dyeing, and also has the effects of detoxifying, enhancing hair color and warm color, relieving pain and itching, treating skin diseases, diminishing inflammation and sterilizing and the like.
The safe and nontoxic hair dye with different colors is prepared by combining graphene-chitosan and taking alizarin in natural madder as a basic color. The product can prevent hair from being split, dried, broken and damaged while achieving the hair dyeing effect, and can adsorb scalp grease, sterilize and diminish inflammation, thereby achieving the effects of protecting scalp and hair and generating stabbing pain feeling of scalp when hair is dyed less. The madder, a Chinese herbal medicine component contained in the product, is a long-history plant dye which has the functions of stopping bleeding, cooling blood, clearing heat, removing jaundice, relieving pain and itching, sterilizing and diminishing inflammation and is suitable for partial skin patients.
The experiment creatively extracts the alizarin extracting solution in the madder plant as the basic color of the coloring agent through ultrasonic wave assistance. The graphene oxide is reduced by using ascorbic acid to obtain the graphene with high surface area and high flexibility, the graphene can strongly interact with chitosan through hydrogen bonds, and the chitosan is further strongly combined with keratin on the hair surface through amino and hydroxyl groups of the chitosan and is attached to the hair surface to form a smooth coating. Meanwhile, due to the characteristic of amphipathy of the graphene oxide, the alizarin can be well attached to the surface of the hair, and the gel formed by the chitosan and the ascorbic acid can enhance the attachment capability of the gel, so that the hair dyeing effect is achieved. Thereby preparing a safe and nontoxic novel natural madder graphene hair dye. And testing the related performances such as color fastness and the like.
International patent application No. PCT/CN2016/074428 discloses a hair-darkening dyeing composition, which employs one or more of chitin, chitosan, gelatin, silicone oil and resin as a hair dye, but the adsorption rate of chitin, chitosan and gelatin to protein fibers such as hair is low, so the invention needs to overcome this deficiency. The preparation of the novel natural madder graphene hair dye well utilizes the graphene and the chitosan to solve the problem.
Chinese patent application No. 201711395380.3 discloses a graphene modified hair dye, which is prepared by dispersing graphene in an aqueous solution, adding gallic acid, and stirring at 50-80 deg.C for 6-8 hr; in the hair dyeing process, the dyeing agent A is required to be kept for 30-40 minutes firstly, and then the color developing agent B is required to be kept for 30-40 minutes, so that the problems of resource waste, difficulty in acceptance of enterprises and common people and the like can be caused in the aspects of industrial preparation and use. The novel natural madder graphene hair dye is prepared by stirring reduced graphene for about one hour at high temperature, mixing the reduced graphene with prepared chitosan to prepare graphene for coagulation, and further mixing the graphene with an madder extracting solution obtained by ultrasonic waves and the like to prepare the hair dye; the using time of the hair dye is shortened by half, the problem of long time consumption in preparation and use of the hair dye is well solved, and the hair dye is easier to accept by people and put into production and use.
The main material used for preparing the medicine is madder which is distributed in northeast, northwest and northwest China, Sichuan China, Tibet China and the like. Is usually in sparsely, forest borders, shrubs or grasslands, is distributed in the regions of korea, japan and russia far east, has abundant resources, and is a plant dye with a long history. On the industrial level, the cost of the raw material is low. From the aspect of putting into the market for use, the hair dye is easier to be accepted by common people compared with other products which are expensive and have the same hair dyeing effect.
Most of hair dyes, which are composed of chemically synthesized pigments, are harmful to hair itself, and if they are inadvertently stuck to the scalp, they cause problems such as loss of hair or increase of dandruff, and in severe cases, they are also allergic. Some poor hair dyes also have a harsh taste. In life, a plurality of customers can reflect the problems that the scalp feels scorching and stabbing when dyeing hair, the hair dyeing experience is poor and the like, and the novel natural madder graphene hair dye well solves the problem. Due to the fusion of the madder root, the novel natural madder graphene hair dye can not stimulate the scalp when in use to cause the phenomena of dandruff increase and stabbing pain after hair dyeing, and also has the effects of detoxifying, enhancing hair color and warm color, relieving pain and itching, treating skin diseases, diminishing inflammation and sterilizing and the like.
Claims (3)
1. A preparation technology of natural hair dye can obtain a series of colors according to different proportions, and comprises the following contents:
mixing the madder root extract and the graphene-chitosan gel to obtain hair dyes in different proportions:
hair dye style 1: the ratio of the madder extract to the graphene-chitosan gel is 5: 1;
hair dye style 2: the ratio of the madder extract to the graphene-chitosan gel is 4: 1;
hair dye style 3: the ratio of the madder extract to the graphene-chitosan gel is 3: 1;
hair dye style 4: the ratio of the madder extract to the graphene-chitosan gel is 2: 1;
hair dye style 5: the ratio of the madder extract to the graphene-chitosan gel is 1: 1;
hair dye style 6: the ratio of the madder extract to the graphene-chitosan gel is 1: 2;
hair dye style 7: the ratio of the madder extract to the graphene-chitosan gel is 1: 3;
hair dye style 8: the ratio of the madder extract to the graphene-chitosan gel is 1: 4;
hair dye style 9: the ratio of the madder root extract to the graphene-chitosan gel is 1: 5.
2. The method according to claim 1, wherein 30.0 g of the sieved Rubia cordifolia is accurately weighed, 300 mL of 70% ethanol solution is added, the mixture is sonicated at 40 ℃ for 20 min, and the filtrate is obtained after filtration for further use.
3. The method of preparing reduced graphene-chitosan according to claim 1, wherein: 1) accurately measuring 50mL of 10mg/mL graphene oxide solution into a 250 mL round-bottom flask, then accurately measuring 50mL of 50 mg/mL ascorbic acid solution, stirring and heating at 90 ℃ for 1 hour, centrifuging for 5 min at the rotating speed of 10000r/min, and washing for 3 times by deionized water to obtain a black product reduced graphene; 2) accurately weighing 300 mL of 2.5 mg/mL ascorbic acid solution into a 500 mL beaker, then accurately weighing 0.75 g of chitosan, and uniformly stirring the weighed chitosan and ascorbic acid solution in a water bath at 60 ℃ to obtain chitosan gel; 3) preparing graphene-chitosan gel: measuring 200mL of chitosan gel, adding the reduced graphene prepared in the step 1), and uniformly mixing to obtain the graphene-chitosan gel.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112933000A (en) * | 2021-03-18 | 2021-06-11 | 电子科技大学中山学院 | Antibacterial nail polish and preparation method thereof |
| KR102338053B1 (en) | 2021-07-16 | 2021-12-13 | 한국콜마주식회사 | Hair coloring leave-on cosmetics containing graphene oxide |
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