CN110974752A

CN110974752A - Novel plant hair dye and preparation method thereof

Info

Publication number: CN110974752A
Application number: CN201911412262.8A
Authority: CN
Inventors: 岳双辰
Original assignee: Jiuzhou Yihua Shanghai Biotechnology Co Ltd
Current assignee: Jiuzhou Yihua Shanghai Biotechnology Co Ltd
Priority date: 2019-12-31
Filing date: 2019-12-31
Publication date: 2020-04-10

Abstract

The invention discloses a novel plant hair dye and a preparation method thereof, wherein a hydrogen peroxide rinsing process of the traditional hair dye is abandoned, and a polygonum multiflorum extract and black mulberry extract soaking process of Chinese herbal medicine components is adopted, so that the hair dyeing effect is further ensured, and secondary damage is not caused to hair quality; the invention abandons the traditional AB dosage form, adopts the 3 dosage forms, also carries out hair care and repair during hair dyeing, and protects the hair quality. The chitosan nano sol is not simply used as an additive, is made into a nano sol to be a supporting body, and can fill the defects generated by hair dyeing on the surface of the hair through the permeation absorption and the surface attachment and wrapping of the chitosan nano sol, and recover the softness and elasticity of the hair.

Description

Novel plant hair dye and preparation method thereof

Technical Field

The invention belongs to the technical field of hair dyes, and particularly relates to a novel plant hair dye and a preparation method thereof.

Background

Permanent hair dyes work by opening the hair scales on the surface of the hair by using chemicals, which cause the dye to penetrate into the hair in the form of an intermediate and then form a bond within the hair. The hair quality is affected by the damage to the hair cortex and cortex structure of the hair during the hair dyeing process, which is known as hair dyeing damage. In addition, sensitizing agents such as ammonia water and the like adopted in the hair dye can generate strong sensitizing effect on skin, so that skin allergy caused by hair dyeing is caused.

For the scalp, on the one hand, most of the dye intermediates used for permanent hair dyeing are amines or phenols, which may cause irritation to the scalp or, if the skin is easily irritated, may be irritated again by the irritation; on the other hand, as mentioned above, after the dye intermediate of the permanent hair dye enters into the hair, some chemical substances are also needed to promote polymerization, and a combined body with a large volume is formed, which easily causes skin irritation.

For hair, the dyeing process is completed by forming a macromolecular pigment through the polymerization of an oxidation dye in the hair, the internal composition structure of the hair can be inevitably damaged in the process, when the hair skin is damaged and becomes rough, even the hair scales are degraded, the structure of the hair skin is not complete and continuous, the water and nutrient substances in the hair cannot be kept not to be lost, and then the hair is easy to dry and branch, lose elasticity and is not flexible any more.

Because the chemical hair dye can damage the protein structure in the hair after dyeing the hair, the hair can be further damaged by perming after dyeing the hair, and even the medulla layer can be damaged, and the inner core of the hair can be damaged. The result is that not only the hair becomes dry and brittle due to the permanent wave, but also the permanent wave effect is greatly impaired, and the hair style cannot be maintained for a long time or even cannot be styled.

Disclosure of Invention

The invention provides a novel plant hair dye and a preparation method thereof, and solves the problems of hair quality damage, poor durability of plant hair dyeing components and difficult hair perming and shaping after hair dyeing caused by chemical hair dyeing in the conventional hair dye.

The technical scheme of the invention is as follows:

a novel plant hair dye comprises an agent A, an agent B and an agent C,

the agent A comprises: water, cetearyl alcohol, ceteareth-20, ammonia, thioglycolic acid;

the agent B comprises: water, chitosan, modified silicone oil, cetearyl alcohol, ceteareth-20, ferrous sulfate, methylparaben, propylparaben;

the agent C comprises: water, chitosan, cetearyl alcohol, ceteareth-20, gallic acid, maltodextrin, Polygoni Multiflori radix extract, maltodextrin, black mulberry fruit extract, tannic acid, methyl hydroxybenzoate, and propyl hydroxybenzoate.

Preferably, the preparation method of the novel plant hair dye comprises the following steps:

preparation of an agent A: weighing raw material water according to a formula, adding the raw material water into a water phase tank, heating, weighing raw materials cetearyl alcohol and ceteareth-20 according to the formula, adding the raw materials into an oil phase tank, and heating; pumping the water phase into an emulsification tank, starting stirring, pumping the oil phase into the emulsification tank, homogenizing, continuing stirring, starting cooling water, cooling, adding ammonia and thioglycollic acid, and uniformly stirring;

preparation of agent B:

cleaning and drying shrimp and crab shells, soaking the shrimp and crab shells in dilute hydrochloric acid at room temperature to remove calcium carbonate in the raw materials, then filtering and washing the raw materials to be neutral, then putting the raw materials in NaOH solution to boil and remove protein, filtering and washing the raw materials to be neutral, and drying the raw materials to obtain chitin; then placing the chitosan nano sol into 40% NaOH solution, keeping the temperature in an oven at 85 ℃ for 17 hours, then filtering, and washing the chitosan nano sol to be neutral to obtain chitosan nano sol; weighing raw material water, adding into a water phase tank, and heating to 85-90 deg.C;

weighing raw materials of cetearyl alcohol and ceteareth-20 according to the formula, adding into an oil phase tank, and heating to 85-90 ℃; pumping the water phase into an emulsification tank, starting stirring, pumping the oil phase into the emulsification tank, homogenizing, adding ferrous sulfate, methyl hydroxybenzoate, propyl hydroxybenzoate, modified silicone oil and chitosan nano sol, and continuing stirring;

preparation of agent C:

cleaning and drying shrimp and crab shells, soaking the shrimp and crab shells in dilute hydrochloric acid at room temperature to remove calcium carbonate in the raw materials, then filtering and washing the raw materials to be neutral, then putting the raw materials in NaOH solution to boil and remove protein, filtering and washing the raw materials to be neutral, and drying the raw materials to obtain chitin; then placing the chitosan nano sol into 40% NaOH solution, keeping the temperature in an oven at 85 ℃ for 17 hours, then filtering, and washing the chitosan nano sol to be neutral to obtain chitosan nano sol; weighing raw materials of water and methyl hydroxybenzoate, adding into a water phase tank, and heating to 85-90 deg.C; weighing raw materials of cetearyl alcohol and ceteareth-20 according to the formula, adding into an oil phase tank, and heating to 85-90 ℃; pumping the water phase into an emulsifying tank, stirring, pumping the oil phase into the emulsifying tank, homogenizing, adding gallic acid, maltodextrin, Polygoni Multiflori radix extract, black mulberry extract, tannic acid, grape seed extract, propyl hydroxybenzoate, and chitosan nanometer sol, and stirring.

Preferably, when the agent C is prepared, pumping the water phase into an emulsification tank, starting stirring, pumping the oil phase into the emulsification tank, homogenizing, starting cooling water, cooling to 40-45 ℃, adding the rest raw materials, and continuing stirring for 30 min.

Preferably, the extraction process of the grape seeds in the agent C comprises the following steps: fully mixing fermented grape seeds with petroleum ether, standing for 6h for degreasing, and crushing by a crusher; cleaning fine sand, sieving with 200 mesh sieve, mixing with grape seed powder at a ratio of 2:1, and placing into an extraction chamber; pumping n-hexane into an extraction chamber by a high-pressure pump, and heating the extraction chamber to 80 ℃ and 40 MPa; after 20 minutes, the heating was stopped, and after 30 minutes of standing, nitrogen gas was introduced and the extract was collected by nitrogen-blown concentration.

Preferably, the preparation method of the modified silicone oil is as follows: adding epoxy modified silicone oil and a secondary amine compound into a container, adding absolute ethyl alcohol, heating to 70-75 ℃ for reaction for 3-4 hours, heating to 80 ℃ for atmospheric distillation to remove the absolute ethyl alcohol, reducing the pressure to below-0.095 MPa, distilling unreacted raw materials at 100 ℃ and 150 ℃, and then adding minoxidil and ketoconazole to obtain the modified silicone oil.

Preferably, the extraction process of the black mulberry and the polygonum multiflorum comprises the following steps:

cleaning black mulberry/radix Polygoni Multiflori, and pulverizing; mixing with ethanol, extracting, and filtering to obtain water solution; stirring and standing for 2 hours; centrifuging, and taking supernatant; filtering the obtained supernatant at 50 deg.C with carbon-based tungsten ion grid; drying and concentrating.

Has the advantages that:

1. the invention adopts the following method to protect the hair quality, abandons the hydrogen peroxide rinsing process of the traditional hair dye on the basis of using chemical hair dye, adopts the infiltration process of the polygonum multiflorum extract and the black mulberry extract of Chinese herbal medicine components, further ensures the hair dyeing effect and does not cause secondary damage to the hair quality. The invention abandons the traditional AB dosage form, adopts the 3 dosage forms, also carries out hair care and repair during hair dyeing, and protects the hair quality. Instead of simply using the additive of chitosan, the chitosan is made into nano sol to be a supporting body.

2. The grape seed extract is used as an anti-allergy agent, so that the stimulation of a sensitizing substance in the hair dye to the skin is reduced, and the skin is protected. The grape seed extract is a nutritional food prepared by refining effective active nutritional ingredients extracted from natural grape seeds and main raw materials such as vitamin E and the like. The grape seed extract is a novel high-efficiency natural antioxidant substance which can not be synthesized in a human body and is extracted from grape seeds, the antioxidant activity of the grape seed extract is 50 times of that of vitamin E and 20 times of that of vitamin C, the grape seed extract can effectively remove redundant free radicals in the human body, and the grape seed extract has the functions of ultra-strong delaying senility and enhancing immunity. Resisting oxidation, resisting allergy, relieving fatigue, improving body condition, improving sub-health state, and delaying aging.

3. In order to effectively protect hair, the invention adopts extracts of polygonum multiflorum and black mulberry. Extracts such as polygonum multiflorum, black mulberry, grape seeds and the like are also used in the traditional hair dye, but because the extracts cannot be effectively treated, the extracts cannot be effectively attached with hair, and fall off after being washed once or twice, so that the effective effect cannot be achieved. Therefore, in order to effectively promote the attachment of the extract and wrap and protect the hair, the invention adopts the chitosan nano sol polymerization process. The extract can be effectively polymerized by the chitosan nano sol polymerization process, and is attached to the hair, so that the coating protection effect is achieved on the hair. Prevent the hair from secondary damage. The polygonum multiflorum and the black mulberry are centrifugally extracted to avoid impurities so as to solve the problem of the traditional chemical hair dye.

4. When the agent B and the agent C are prepared, shrimp and crab shells are cleaned and dried, and then are soaked for 2 hours at room temperature by using 5 percent of dilute hydrochloric acid to remove calcium carbonate in the raw materials, then are filtered and washed to be neutral, then are placed in a 10 percent NaOH solution to be boiled and deproteinized, are filtered and washed to be neutral, and are dried to obtain chitin; then placing the chitosan nano sol into 40% NaOH solution, keeping the temperature in an oven at 85 ℃ for 17 hours, then filtering, and washing the chitosan nano sol to be neutral to obtain chitosan nano sol; then the hair restoring agent is mixed with the raw materials, so that the damaged loose and blank pores on the surface of the hair can be filled and restored. The ammonia in the hair dye has the function of expanding and softening the cuticular layer of the hair so as to facilitate the penetration and absorption of the hydrosulfide of the main agent, and after the thioglycolate and the ammonia water are used, the hair protein can be damaged, and the hair structure is loose, porous and inelastic. The defects generated by hair dyeing on the surface of the hair can be filled up through the permeation absorption and the surface attachment and wrapping of the chitosan nano sol, and the softness and elasticity of the hair are recovered.

5. Prevent the hair dye from falling off. The method is characterized in that the dye for dyeing the hair enters a space opened by the hair from an alkaline environment in the process of dyeing the hair, in order to keep the retention time of the dye as much as possible and prevent the dye from falling off due to cleaning and other reasons, chitosan nano sol is adopted to carry out wrapping protection on the surface of the hair, so that the attachment of extracts such as polygonum multiflorum, black mulberry and grape pip on the surface of the hair can be ensured, and the attachment of the dye in wrapping on the hair can also be ensured.

6. The plasticity of the hair is increased. Because the hair is seriously damaged after the traditional hair dyeing process, the loss of fiber and protein in the hair is serious, the thermal plasticity of the hair is reduced, and the same hair perming process can cause the problems of difficult plasticity or shortened plasticity time and the like. The plasticity of the hair can be recovered through the restoration of the chitosan nano sol to ensure that the hair dyed can be normally permed.

7. Can be used at low temperature. The traditional hair dye is easy to coagulate at low temperature, and needs to be heated when in use. The chitosan nano sol can keep liquid state at the environment temperature of 5 ℃, the hair dyeing effect is not influenced, the chitosan nano sol polymerization process can effectively polymerize the effective components of the polygonum multiflorum, the black mulberry and the grape seed extract, the coating protection of the polymer is formed on the outer layer of the hair, and the elasticity and the plasticity of the hair can be improved while the effective components are ensured to be attached to the hair.

Description of the drawings:

FIG. 1: and the hair protection degree result is shown schematically.

Detailed Description

The ingredient proportion table of the invention is as follows:

TABLE 1A Agents

TABLE 2 agent B

TABLE 3C Agents

Example 1

Preparation of agent A

Weighing raw material water according to the formula, adding the raw material water into a water phase tank, and heating to 85 ℃. Weighing raw materials of cetearyl alcohol and ceteareth-20 according to the formula, adding into an oil phase tank, and heating to 85 ℃. Pumping the water phase into an emulsification tank, starting stirring, pumping the oil phase into the emulsification tank, homogenizing for 5 minutes, and continuing stirring for 30 minutes. Cooling water is started, ammonia (25%) and mercaptoacetic acid (99%) are added when the temperature is reduced to 45 ℃, and the mixture is stirred uniformly.

Preparation of the agent B

Cleaning and drying shrimp and crab shells, soaking the shrimp and crab shells for 2 hours at room temperature by using 5 percent dilute hydrochloric acid, removing calcium carbonate in the raw materials, filtering and washing the raw materials to be neutral, then placing the raw materials in a 10 percent NaOH solution for boiling for 2 hours to remove protein, filtering and washing the raw materials to be neutral, and drying the raw materials to obtain the chitin. Then placing the mixture into a 40% NaOH solution, keeping the temperature in an oven at 85 ℃ for 17 hours, then filtering, washing the mixture to be neutral, weighing raw material water, adding the raw material water into a water phase tank, and heating the mixture to 85 ℃. Weighing raw materials of cetearyl alcohol and ceteareth-20 according to the formula, adding into an oil phase tank, and heating to 85 ℃. Pumping the water phase into an emulsification tank, starting stirring, pumping the oil phase into the emulsification tank, homogenizing for 5 minutes, adding ferrous sulfate, modified silicone oil, methyl hydroxybenzoate and propyl hydroxybenzoate, and continuing stirring for 30 minutes.

The preparation method of the modified silicone oil comprises the following steps: adding epoxy modified silicone oil and a secondary amine compound into a container, adding absolute ethyl alcohol, heating to 70-75 ℃ for reaction for 3-4 hours, heating to 80 ℃ for atmospheric distillation to remove the absolute ethyl alcohol, reducing the pressure to below-0.095 MPa, distilling unreacted raw materials at 100 ℃ and 150 ℃, and then adding minoxidil and ketoconazole to obtain the tertiary amine modified silicone oil.

Preparation of the agent C

Black mulberry and fleece-flower root extraction process

(1) Cleaning black mulberry/polygonum multiflorum, and crushing into 60-mesh plant powder by using a traditional Chinese medicine crusher;

(2) mixing the pulverized medicinal powder with absolute ethyl alcohol according to the ratio of 1: 2, extracting and filtering at 40 ℃ to obtain an aqueous solution; stirring and standing for 2 hours;

(3) centrifuging at 5000r/min, collecting supernatant, and filtering with carbon-based tungsten ion grid at 50 deg.C;

(4) drying and concentrating the filtered dye solution through a rotary evaporator to prepare a dye concentrated solution;

the grape seed extraction process comprises the following steps:

mixing fermented grape seed with petroleum ether, standing for 6 hr for defatting, and pulverizing with pulverizer.

Cleaning fine sand, sieving with 200 mesh sieve, mixing with grape seed powder at a ratio of 2:1, and placing into an extraction chamber.

Pumping n-hexane into the extraction chamber via a high-pressure pump, and heating the extraction chamber to 80 deg.C and 40 MPa. After 20 minutes, the heating was stopped, and after 30 minutes of standing, nitrogen gas was introduced and the extract was collected by nitrogen-blown concentration.

Cleaning and drying shrimp and crab shells, soaking the shrimp and crab shells for 2 hours at room temperature by using 5 percent dilute hydrochloric acid, removing calcium carbonate in the raw materials, filtering and washing the raw materials to be neutral, then placing the raw materials in a 10 percent NaOH solution for boiling for 2 hours to remove protein, filtering and washing the raw materials to be neutral, and drying the raw materials to obtain the chitin. Then placing the mixture into a 40% NaOH solution, keeping the temperature in an oven at 85 ℃ for 17 hours, then filtering, washing the mixture to be neutral, weighing raw materials of water and methyl hydroxybenzoate, adding the raw materials into a water phase tank, and heating the mixture to 85 ℃. Weighing raw materials of cetearyl alcohol and ceteareth-20 according to the formula, adding into an oil phase tank, and heating to 85 ℃. Pumping the water phase into an emulsifying tank, stirring, pumping the oil phase, homogenizing for 5 min, adding gallic acid, maltodextrin, Polygoni Multiflori radix extract, black mulberry fruit extract, tannic acid, grape seed extract, and propyl hydroxybenzoate, and stirring for 30 min.

Example 2:

preparation of agent A

Weighing raw material water according to the formula, adding the raw material water into a water phase tank, and heating to 90 ℃. Weighing raw materials of cetearyl alcohol and ceteareth-20 according to the formula, adding the raw materials into an oil phase tank, and heating to 90 ℃. Pumping the water phase into an emulsification tank, starting stirring, pumping the oil phase into the emulsification tank, homogenizing for 5 minutes, and continuing stirring for 40 minutes. Cooling water is started, ammonia (25%) and mercaptoacetic acid (99%) are added when the temperature is reduced to 50 ℃, and the mixture is stirred uniformly.

Preparation of the agent B

Cleaning and drying shrimp and crab shells, soaking the shrimp and crab shells for 2 hours at room temperature by using 10% dilute hydrochloric acid, removing calcium carbonate in the raw materials, filtering and washing the raw materials to be neutral, then placing the raw materials in a 15% NaOH solution for boiling for 2 hours to remove protein, filtering and washing the raw materials to be neutral, and drying the raw materials to obtain the chitin. Then placing the mixture into a 40% NaOH solution, keeping the temperature in an oven at 85 ℃ for 17 hours, then filtering, washing the mixture to be neutral, weighing raw material water, adding the raw material water into a water phase tank, and heating the mixture to 90 ℃. Weighing raw materials of cetearyl alcohol and ceteareth-20 according to the formula, adding the raw materials into an oil phase tank, and heating to 90 ℃. Pumping the water phase into an emulsification tank, starting stirring, pumping the oil phase into the emulsification tank, homogenizing for 5 minutes, adding the modified silicone oil, the ferrous sulfate, the methyl hydroxybenzoate and the propyl hydroxybenzoate, and continuing stirring for 30 minutes.

Preparation of the agent C

The extraction process of black mulberry and fleece-flower root comprises the following steps:

(3) centrifuging at 5000r/min to obtain supernatant;

(4) filtering the obtained supernatant at 50 deg.C with carbon-based tungsten ion grid;

(5) drying and concentrating the filtered dye solution through a rotary evaporator to prepare a dye concentrated solution;

the grape seed extraction process comprises the following steps:

Pumping n-hexane into the extraction chamber by high pressure pump, and heating the extraction chamber to 90 deg.C and 40 MPa. After 30 minutes, the heating was stopped, and after 30 minutes of standing, nitrogen gas was introduced and the extract was collected by nitrogen-blown concentration.

Cleaning and drying shrimp and crab shells, soaking the shrimp and crab shells for 2 hours at room temperature by using 10% dilute hydrochloric acid, removing calcium carbonate in the raw materials, filtering and washing the raw materials to be neutral, then placing the raw materials in a 15% NaOH solution for boiling for 2 hours to remove protein, filtering and washing the raw materials to be neutral, and drying the raw materials to obtain the chitin. Then placing the mixture into a 40% NaOH solution, keeping the temperature in an oven at 85 ℃ for 17 hours, then filtering, washing the mixture to be neutral, weighing raw materials of water and methyl hydroxybenzoate, adding the raw materials into a water phase tank, and heating the mixture to 90 ℃. Weighing raw materials of cetearyl alcohol and ceteareth-20 according to the formula, adding the raw materials into an oil phase tank, and heating to 90 ℃. Pumping the water phase into an emulsifying tank, stirring, pumping the oil phase, homogenizing for 5 min, adding gallic acid, maltodextrin, Polygoni Multiflori radix extract, black mulberry fruit extract, tannic acid, grape seed extract, and propyl hydroxybenzoate, and stirring for 30 min.

Example 3:

preparation of agent A

Weighing raw material water according to the formula, adding the raw material water into a water phase tank, and heating to 95 ℃. Weighing raw materials of cetearyl alcohol and ceteareth-20 according to the formula, adding into an oil phase tank, and heating to 95 ℃. Pumping the water phase into an emulsification tank, starting stirring, pumping the oil phase into the emulsification tank, homogenizing for 5 minutes, and continuing stirring for 30 minutes. Cooling water is started, ammonia (25%) and mercaptoacetic acid (99%) are added when the temperature is reduced to 40 ℃, and the mixture is stirred uniformly.

Preparation of the agent B

Cleaning and drying shrimp and crab shells, soaking the shrimp and crab shells for 2 hours at room temperature by using 10% dilute hydrochloric acid, removing calcium carbonate in the raw materials, filtering and washing the raw materials to be neutral, then placing the raw materials in a 5% NaOH solution for boiling for 2 hours to remove protein, filtering and washing the raw materials to be neutral, and drying the raw materials to obtain the chitin. Then placing the mixture into a 40% NaOH solution, keeping the temperature in an oven at 85 ℃ for 17 hours, then filtering, washing the mixture to be neutral, weighing raw material water, adding the raw material water into a water phase tank, and heating the mixture to 88 ℃. Weighing raw materials of cetearyl alcohol and ceteareth-20 according to the formula, adding the raw materials into an oil phase tank, and heating to 88 ℃. Pumping the water phase into an emulsification tank, starting stirring, pumping the oil phase into the emulsification tank, homogenizing for 5 minutes, adding the modified silicone oil, the ferrous sulfate, the methyl hydroxybenzoate and the propyl hydroxybenzoate, and continuing stirring for 30 minutes.

Preparation of the agent C

Black mulberry and fleece-flower root extraction process

(3) centrifuging at 5000r/min to obtain supernatant;

grape seed extraction process

Pumping n-hexane into an extraction chamber by a high-pressure pump, heating the extraction chamber to 100 ℃ under 40MPa for 30 minutes, stopping heating, standing for 30 minutes, introducing nitrogen, and collecting the extract by a nitrogen blowing concentration method.

Cleaning and drying shrimp and crab shells, soaking the shrimp and crab shells for 2 hours at room temperature by using 10% dilute hydrochloric acid, removing calcium carbonate in the raw materials, filtering and washing the raw materials to be neutral, then placing the raw materials in a 5% NaOH solution for boiling for 2 hours to remove protein, filtering and washing the raw materials to be neutral, and drying the raw materials to obtain the chitin.

Then placing the mixture into a 40% NaOH solution, keeping the temperature in an oven at 85 ℃ for 17 hours, then filtering, washing the mixture to be neutral, weighing raw materials of water and methyl hydroxybenzoate, adding the raw materials into a water phase tank, and heating the mixture to 88 ℃. Weighing raw materials of cetearyl alcohol and ceteareth-20 according to the formula, adding the raw materials into an oil phase tank, and heating to 88 ℃.

Pumping the water phase into an emulsifying tank, stirring, pumping the oil phase, homogenizing for 5 min, adding gallic acid, maltodextrin, Polygoni Multiflori radix extract, black mulberry fruit extract, tannic acid, grape seed extract, and propyl hydroxybenzoate, and stirring for 30 min.

Experimental data:

1. test of hair protection

1.1 Hair surface protection test

The results of this test are shown in fig. 1, which compares the hair dyed by the product of the present invention with the hair dyed by the conventional hair dye under an electron microscope.

The surface of the hair dyed by the common product is rough, while the surface of the hair dyed by the product is smooth, so that the product has a coating protection effect on the hair.

The test was carried out by collecting normal hair, preparing the hair itself, cutting off the tips, cutting to a length of about 15cm, washing with l 0% SLS aqueous solution, and air-drying naturally. Measuring the diameter of each hair, and taking the hair with the diameter of 0.08mm-0.09mm for standby.

And (3) instruments and tests: tensiometer, relative humidity controlled at 50%, cycle stretch times: 50 times, 100 times, 150 times, 200 times; 10 hairs were used per cycle, with 10% per stretch.

After the hair was stretched a different number of times, the relative humidity was controlled at 50%, the hair was broken with a tensiometer and the force exerted to break the hair was observed to determine the work of breaking, i.e. the force of breaking and the distance over which the hair was broken. The bending force is measured by a tension meter, namely, an external force is applied to the middle position of the hair to bend and deform the hair on the basis of stretching, and the force of bending deformation is measured.

The results are as follows:

experimental data show that the hair after dyeing has good toughness, and is slightly reduced compared with normal hair, which indicates that the hair is slightly damaged by the hair dyeing agent.

1.3 Hair thermoplasticity test

According to the test, normal hair is collected, the hair dyed by the product and the hair dyed by the traditional hair dye are subjected to a conventional thermoplastic test, the time required for shaping is detected at 140 ℃, and the plasticity retention rate of the hair is detected by repeatedly washing for 10 times after plasticity. The experimental results are as follows:

the experimental data show that the hair can be shaped in the conventional perming time after being dyed with the hair dye, and the hair has the similar shaping retention rate with the normal hair.

2. Hair dyeing effect experiment

The hair dye is used in the experiment, and a common chemical hair dye and a common natural Chinese herbal medicine hair dye are used in the market, and the hair dyeing results are compared by dyeing the hair of a user. By comparing the questionnaire survey of the user with the actual hair dyeing effect, the experimental results are as follows:

the experimental data show that the hair dye has similar satisfaction degree with the traditional hair dye, similar hair dyeing rate and slightly longer hair color retention time, and the hair dye has advantages in hair dyeing effect compared with the conventional hair dye.

3. In vitro mammalian cell chromosome aberration experiments:

materials and methods:

1) the test substance: solvent selection, dissolving in 1640 culture solution. The preparation method comprises preparing hair dye into test solutions with different concentrations with 1640 culture solution.

2) The tested cell is a Chinese hamster lung cell strain.

3) Metabolic activation system:

3.1S₉preparation of

S prepared by inducing SD rat liver homogenate with polychlorinated biphenyl₉，S₉The mixed solution contains S₉10 percent of the component, and supplementary cofactors are used as an in vitro metabolism activation system of the experiment.

3.2S₉Preparing a mixed solution:

S₉:1ml,MgCl₂(0.4mo10.2ml of KCI (1.65mol/L), 0.2m1, 17.9mg of G-6-P and 30.6mg of NADP, and the serum-free 1640 culture solution is used to make up to 10 ml.

4) Positive control, adding S₉Using cyclophosphamide 20 mug/ml without S₉Using 0.25ug/ml mitomycin

5) Negative control 1640 culture medium.

6) The culture solution is 1640 culture solution containing 10% fetal bovine serum.

7) Dose selection according to pre-test without S₉The cell division index 50% test substance concentration is 600. mu.g/ml, so the test substance concentration is tested by selecting the high concentration group to be 600. mu.g/ml, the medium concentration group to be 300ug/ml and the low concentration group to be 150 pg/ml.

Adding S₉The cell division index 50% test substance concentration is 1200. mu.g/ml, so the test substance concentration is selected, the test is performed with the high concentration group being 1200. mu.g/ml, the medium concentration group being 600. mu.g/ml, and the low concentration group being 300. mu.g/ml.

8) The test method comprises selecting well-growing cells, digesting, and preparing into 1 × 10 with culture medium containing 10% fetal calf serum⁶Per ml cell suspension, 1m1 cell suspension was inoculated into each flask (25ml), 4ml of 10% fetal bovine serum-containing medium was added, and the mixture was placed at 37 ℃ in CO₂The incubator is used for 24 h. Dumping the culture solution for 24h, adding 4.5ml of test solution or negative and positive control solution with different concentrations, and adding S into each culture bottle when activation is required₉0.5ml of mixed solution, adding 0.5m11640 of culture solution into each culture bottle when activation is not needed, mixing, and placing in CO₂The culture was carried out in an incubator for 4 hours, the supernatant was discarded, washed three times with HanK's solution, and cultured at 37 ℃ for 24 hours with 5m1 of a culture solution containing 10% fetal bovine serum. 4h before harvesting cells, colchicine (final concentration of 1ug/ml) is added, and digestion, hypotonic, fixation, flaking and staining are performed according to a conventional method. 100 well-dispersed metaphase cells are selected in each group, the type and the number of the chromatid distortion are observed and recorded, and the cell distortion rate is calculated.

Table 1: record of dissolution of test substance

Test substance concentration μ g/ml	Name of solvent	Whether or not there is precipitation
			300	1640 culture solution	Is free of
600	1640 culture solution	Is free of
			1200	1640 culture solution	Is free of
2400	1640 culture solution	Is free of

Table 2: without addition of S₉Cell division index of test substance

Table 3: adding S₉Cell division index of test substance

Table 4: 4h without adding S₉Test article detection knotFruit

And (3) statistical treatment: x for rate of deformity²And (5) checking and analyzing.

Table 5: 4h plus S₉Test results of the test substance

Evaluation of results the test group was compared with the negative control group without addition of S₉Compared with the control group, the in vitro mammal cell chromosome aberration rates of the high, medium and low concentration groups of the test object have P value of more than 0.05 and have no significant difference. Adding S₉Compared with the control group, the in vitro mammal cell chromosome aberration rates of the high, medium and low concentration groups of the test object have P value of more than 0.05 and have no significant difference. The test result of the chromosome aberration test of the mammalian cells in vitro of the test object is negative.

It is to be understood that the invention is not limited to the specific embodiments described above, but is intended to cover various insubstantial modifications of the inventive process concepts and solutions, or its application to other applications without modification.

Claims

1.A novel plant hair dye is characterized by comprising an agent A, an agent B and an agent C,

the agent B comprises: water, chitosan, cetearyl alcohol, ceteareth-20, ferrous sulfate, methyl hydroxybenzoate, propyl hydroxybenzoate and modified silicone oil;

2. A preparation method of a novel plant hair dye is characterized by comprising the following steps:

preparation of agent B:

preparation of agent C:

3. The method for preparing the novel plant hair dye according to claim 2, wherein in the preparation of the agent C, the water phase is pumped into the emulsifying tank, the stirring is started, then the oil phase is pumped, after the homogenization, the cooling water is started, the temperature is reduced to 40-45 ℃, the rest raw materials are added, and the stirring is continued for 30 min.

4. The method for preparing a novel plant hair dye according to claim 2, wherein the extraction process of the grape seeds in the agent C comprises the following steps: fully mixing fermented grape seeds with petroleum ether, standing for 6h for degreasing, and crushing by a crusher; cleaning fine sand, sieving with 200 mesh sieve, mixing with grape seed powder at a ratio of 2:1, and placing into an extraction chamber; pumping n-hexane into the extraction chamber by a high-pressure pump, heating the extraction chamber, standing, introducing nitrogen, and collecting the extract by nitrogen blowing concentration.

5. The method for preparing a novel plant hair dye according to claim 2, wherein the modified silicone oil is prepared by the following steps: adding epoxy modified silicone oil and a secondary amine compound into a container, adding absolute ethyl alcohol, heating to 70-75 ℃ for reaction for 3-4 hours, heating to 80 ℃ for atmospheric distillation to remove the absolute ethyl alcohol, reducing the pressure to below-0.095 MPa, distilling unreacted raw materials at 100 ℃ and 150 ℃, and then adding minoxidil and ketoconazole to obtain the modified silicone oil.

6. The method for preparing the novel plant hair dye according to claim 2, wherein the process for extracting the black mulberry and the polygonum multiflorum comprises the following steps: