CN110974753A

CN110974753A - Anti-allergic hair dye containing plant extract and preparation method thereof

Info

Publication number: CN110974753A
Application number: CN201911420611.0A
Authority: CN
Inventors: 岳双辰
Original assignee: Beijing Jiuzhou Yihua Cosmetics Co ltd
Current assignee: Beijing Jiuzhou Yihua Cosmetics Co ltd
Priority date: 2019-12-31
Filing date: 2019-12-31
Publication date: 2020-04-10

Abstract

The invention discloses an anti-sensitivity hair dye containing plant extracts and a preparation method thereof, wherein the anti-sensitivity hair dye comprises 10-20 parts of cetearyl alcohol, 10-20 parts of ceteareth-20, 5-8 parts of ammonia, 5-8 parts of thioglycolic acid, 120-140 parts of water, 80-100 parts of chitosan, 10-13 parts of ferrous sulfate, 2-4 parts of maltodextrin, 5-15 parts of polygonum multiflorum extract, 10-20 parts of black mulberry extract, 20-40 parts of grape seed extract, 2-5 parts of methyl hydroxybenzoate, 2-5 parts of propyl hydroxybenzoate, 2-4 parts of zinc oxide, 3-8 parts of β -sitosterol, 15-20 parts of modified coloring agent and 30-40 parts of glycerin, and solves the problems of hair damage caused by chemical hair dyeing, poor durability of plant hair dyeing ingredients, difficult forming after hair dyeing, easy anaphylactic reaction of human bodies caused by hair perming and low plant extraction effectiveness in the existing hair dye.

Description

Anti-allergic hair dye containing plant extract and preparation method thereof

Technical Field

The invention belongs to the technical field of hair dyes, and particularly relates to an anti-allergy hair dye containing plant extracts and a preparation method thereof.

Background

Permanent hair dyes work by opening up 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.

In addition, the polygonum multiflorum and the black mulberry belong to traditional Chinese medicine components, and in order to effectively extract effective substances of the polygonum multiflorum and the black mulberry, a traditional extraction method mostly adopts a method of multiple reflux and oil extraction. The extraction method is easy to generate impurities, and influences the use effect. Meanwhile, the medicinal dry powder of the polygonum multiflorum and the black mulberry cannot be effectively eliminated in the preparation process because the medicinal dry powder contains trace metal of lead and arsenic.

Disclosure of Invention

The invention provides an anti-sensitivity hair dye containing plant extracts and a preparation method thereof, and solves the problems of hair quality damage caused by chemical hair dyeing, poor durability of plant hair dyeing components, difficult hair perming after hair dyeing, easy anaphylactic reaction to a human body and low plant extraction effectiveness in the existing hair dye.

The specific technical scheme is as follows:

an anti-allergy hair dye containing plant extracts comprises 10-20 parts of cetearyl alcohol, 10-20 parts of ceteareth-20, 5-8 parts of ammonia, 5-8 parts of thioglycolic acid, 140 parts of water, 80-100 parts of chitosan, 10-13 parts of ferrous sulfate, 2-4 parts of maltodextrin, 5-15 parts of polygonum multiflorum extract, 10-20 parts of black mulberry extract, 20-40 parts of grape seed extract, 2-5 parts of methyl hydroxybenzoate, 2-5 parts of propyl hydroxybenzoate, 2-4 parts of zinc oxide, 3-8 parts of β -sitosterol, 15-20 parts of modified colorant and 30-40 parts of glycerol.

Preferably, the preparation method of the modified colorant is as follows: adding sodium metasilicate solution into petroleum ether solution, continuously stirring to form sol gel, adding silane cross-linking agent, tannic acid and gallic acid, finally adding ammonium chloride solution, evaporating and washing to obtain agent A; 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, distilling to remove the absolute ethyl alcohol, reducing pressure, and distilling unreacted raw materials at the temperature of 100-150 ℃ to obtain an agent B; mixing the agent A and the agent B to obtain the modified colorant.

Preferably, the method comprises the following steps:

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 a10 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 chitin; then placing the chitosan nano sol into 40% NaOH solution, keeping the temperature in an oven at 84 ℃ for 17 hours, then filtering, and washing the chitosan nano sol to be neutral to obtain chitosan nano sol;

adding cetearyl alcohol and ceteareth-20 to glycerol, and dispersing with glycerol to form a glycerol dispersion; weighing raw material water, adding into a water phase tank, and heating to 85-90 deg.C;

adding the glycerol dispersion into an oil phase tank, heating to 85-90 ℃, pumping the water phase into an emulsification tank, starting stirring, pumping into the oil phase, homogenizing for 5-10 minutes, adding ferrous sulfate, methyl hydroxybenzoate, propyl hydroxybenzoate, chitosan nano sol, maltodextrin, polygonum multiflorum extract, black mulberry extract, grape seed extract, modified colorant, zinc oxide and β -sitosterol, and continuously stirring for 30 minutes to obtain the hair dye.

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.

Preferably, the process for extracting black mulberry and polygonum multiflorum comprises the following specific steps:

(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 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 by a rotary evaporator to prepare dye concentrated solution.

Preferably, the grape seed extraction process 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.

Has the advantages that:

1. in order to solve the problems of the traditional chemical hair dye, the invention adopts the following methods to protect the hair quality and resist allergy: on the basis of using chemical hair dyeing, the hydrogen peroxide rinsing process of the traditional hair dye is abandoned, and the infiltration process of the polygonum multiflorum extract and the black mulberry extract of Chinese herbal medicine components is adopted, so that the hair dyeing effect is further ensured, and the secondary damage to the hair quality is avoided;

the cetearyl alcohol and ceteareth-20 are dispersed with glycerin to make them better combined with other materials, and the added β -sitosterol has good permeability to skin.

2. When the fleece-flower root and the black mulberry are extracted, the obtained supernatant is filtered by a carbon-based tungsten ion grid at the temperature of 50 ℃, high-speed centrifugation is adopted in cooperation with the carbon-based tungsten ion grid, free solid small particle impurities in the extract can be effectively filtered by the adsorption of the carbon-based tungsten, and lead and arsenic in the extract can be effectively removed by the cooperation with the ion grid, so that the toxicity in the extract is removed, and the effectiveness is improved.

3. Adding a sodium metasilicate solution into a petroleum ether solution, continuously stirring to form sol-gel, adding a silane cross-linking agent, tannic acid and gallic acid, finally adding an ammonium chloride solution, evaporating and washing to obtain an agent A; 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, distilling to remove the absolute ethyl alcohol, reducing pressure, and distilling unreacted raw materials at the temperature of 100-150 ℃ to obtain an agent B; the method for obtaining the modified colorant by mixing the agent A and the agent B ensures that the colorant is fixed in the nano particles by the silane cross-linking agent, and a plurality of dye molecules are combined in a single silicon particle to be isolated from the surrounding environment and skin, thereby avoiding anaphylactic reaction and having good washing fastness and hair color retention.

4. 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 vitamin E antioxidant and free radical scavenging agent is a substance which is found in nature and has the strongest capacity of resisting oxidation and scavenging free radicals, the antioxidant activity of the vitamin E antioxidant and free radical scavenging agent is 50 times that of vitamin E and 20 times that of vitamin C, the vitamin E antioxidant and free radical scavenging agent can effectively scavenge redundant free radicals in a human body, and the vitamin E antioxidant and free radical scavenging agent has the superstrong functions of delaying senility and enhancing immunity. Resisting oxidation, resisting allergy, relieving fatigue, improving body condition, improving sub-health state, and delaying aging.

5. 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. Meanwhile, the technical scheme of mixing the chitosan nano sol and the raw materials can fill and repair damaged loose and blank pores on the surface of the hair. 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.

6. 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.

7. 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.

8. 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.

Detailed Description

Example 1:

an anti-sensitivity hair dye containing plant extracts comprises 10 parts of cetearyl alcohol, 18 parts of ceteareth-20, 5 parts of ammonia, 8 parts of thioglycolic acid, 120 parts of water, 90 parts of chitosan, 12 parts of ferrous sulfate, 3 parts of maltodextrin, 10 parts of polygonum multiflorum extract, 15 parts of black mulberry extract, 25 parts of grape seed extract, 3 parts of methylparaben, 3 parts of propylhydroxybenzoate, 2 parts of zinc oxide, 5 parts of β -sitosterol, 18 parts of modified colorant and 35 parts of glycerol.

The preparation method of the modified colorant comprises the following steps: adding sodium metasilicate solution into petroleum ether solution, continuously stirring to form sol gel, adding silane cross-linking agent, tannic acid and gallic acid, finally adding ammonium chloride solution, evaporating and washing to obtain agent A; adding epoxy modified silicone oil and secondary amine compound into a container, adding absolute ethyl alcohol, heating to 70 ℃ for reaction for 3 hours, distilling to remove the absolute ethyl alcohol, reducing pressure,distilling the unreacted starting materials at a temperature of 120 ℃To obtain a B agent; mixing the agent A and the agent B to obtain the modified colorant.

adding cetearyl alcohol and ceteareth-20 into glycerol, dispersing with glycerol to form a glycerol dispersion, weighing raw material water, adding the raw material water into a water phase tank, heating to 87 ℃, adding the glycerol dispersion into an oil phase tank, heating to 87 ℃, pumping the water phase into an emulsification tank, starting stirring, pumping into an oil phase, homogenizing for 5 minutes, adding ferrous sulfate, methyl hydroxybenzoate, propyl hydroxybenzoate, chitosan nanosol, maltodextrin, a polygonum multiflorum extract, a black mulberry fruit extract, a grape seed extract, a modified colorant, zinc oxide and β -sitosterol, and continuously stirring for 30 minutes to obtain the hair dye.

The extraction process of the black mulberry and the polygonum multiflorum comprises the following specific steps:

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

Wherein, the grape seed extraction process 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.

Example 2:

an anti-sensitivity hair dye containing plant extracts comprises 15 parts of cetearyl alcohol, 19 parts of ceteareth-20, 7 parts of ammonia, 6 parts of thioglycolic acid, 130 parts of water, 100 parts of chitosan, 13 parts of ferrous sulfate, 4 parts of maltodextrin, 15 parts of polygonum multiflorum extract, 20 parts of black mulberry extract, 30 parts of grape seed extract, 5 parts of methylparaben, 5 parts of propylparaben, 3 parts of zinc oxide, 8 parts of β -sitosterol, 15 parts of modified colorant and 39 parts of glycerin.

The preparation method of the modified colorant comprises the following steps: adding sodium metasilicate solution into petroleum ether solution, continuously stirring to form sol gel, adding silane cross-linking agent, tannic acid and gallic acid, finally adding ammonium chloride solution, evaporating and washing to obtain agent A; adding epoxy modified silicone oil and a secondary amine compound into a container, adding absolute ethyl alcohol, heating to 72 ℃ for reaction for 4 hours, distilling to remove the absolute ethyl alcohol, reducing pressure, and distilling unreacted raw materials at 110 ℃ to obtain an agent B; mixing the agent A and the agent B to obtain the modified colorant.

Cleaning shrimp and crab shells, drying, soaking in 5% dilute hydrochloric acid at room temperature for 2h, removing calcium carbonate in the raw materials, filtering, washing to be neutral, boiling in 10% NaOH solution for 2h to remove protein, filtering, washing to be neutral, drying to obtain chitin, then placing in 40% NaOH solution, keeping the temperature in an oven at 84 ℃ for 17h, filtering, washing to be neutral to obtain chitosan nano sol, adding cetearyl alcohol and cetearyl polyether-20 into glycerol, dispersing with glycerol to form glycerol dispersion, weighing raw material water, adding into a water phase tank, heating to 85 ℃, adding the glycerol dispersion into an oil phase tank, heating to 85 ℃, pumping a water phase into an emulsifying tank, starting stirring, pumping into an oil phase, homogenizing for 7 min, adding ferrous sulfate, methyl hydroxybenzoate, propyl hydroxybenzoate, chitosan nano sol, maltodextrin, a polygonum multiflorum extract, a black mulberry fruit extract, a grape seed extract, a modified colorant, zinc oxide and β -sitosterol, and continuously stirring for 30 min to obtain the hair dye.

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

Example 3:

an anti-sensitivity hair dye containing plant extracts comprises 17 parts of cetearyl alcohol, 20 parts of ceteareth-20, 6 parts of ammonia, 7 parts of thioglycolic acid, 135 parts of water, 80 parts of chitosan, 10 parts of ferrous sulfate, 2 parts of maltodextrin, 5 parts of polygonum multiflorum extract, 10 parts of black mulberry extract, 40 parts of grape seed extract, 4 parts of methylparaben, 4 parts of propylhydroxybenzoate, 4 parts of zinc oxide, 7 parts of β -sitosterol, 20 parts of modified colorant and 31 parts of glycerol.

The preparation method of the modified colorant comprises the following steps: adding sodium metasilicate solution into petroleum ether solution, continuously stirring to form sol gel, adding silane cross-linking agent, tannic acid and gallic acid, finally adding ammonium chloride solution, evaporating and washing to obtain agent A; adding epoxy modified silicone oil and a secondary amine compound into a container, adding absolute ethyl alcohol, heating to 75 ℃ for reaction for 3 hours, distilling to remove the absolute ethyl alcohol, reducing pressure, and distilling unreacted raw materials at 140 ℃ to obtain an agent B; mixing the agent A and the agent B to obtain the modified colorant.

Cleaning shrimp and crab shells, drying, soaking in 5% dilute hydrochloric acid at room temperature for 2h, removing calcium carbonate in the raw materials, filtering, washing to be neutral, boiling in 10% NaOH solution for 2h to remove protein, filtering, washing to be neutral, drying to obtain chitin, then placing in 40% NaOH solution, keeping the temperature in an oven at 84 ℃ for 17h, filtering, washing to be neutral to obtain chitosan nano sol, adding cetearyl alcohol, cetearyl polyether-20 into glycerol, dispersing with glycerol to form glycerol dispersion, weighing raw material water, adding into a water phase tank, heating to 90 ℃, adding the glycerol dispersion into an oil phase tank, heating to 90 ℃, pumping a water phase into an emulsifying tank, starting stirring, pumping into an oil phase, homogenizing for 9 min, adding ferrous sulfate, methyl hydroxybenzoate, propyl hydroxybenzoate, chitosan nano sol, maltodextrin, a polygonum multiflorum extract, a black mulberry extract, a grape seed extract, a modified colorant, zinc oxide and β -sitosterol, and continuously stirring for 30 min to obtain the hair dye.

(2)mixing the pulverized medicinal powder with absolute ethyl alcohol according to the ratio of 1: 2 after mixingExtracting at 40 deg.C, filtering to obtain water solution; stirring and standing for 2 hours;

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

Example 4:

an anti-sensitivity hair dye containing plant extracts comprises 20 parts of cetearyl alcohol, 10 parts of ceteareth-20, 8 parts of ammonia, 5 parts of thioglycolic acid, 140 parts of water, 85 parts of chitosan, 11 parts of ferrous sulfate, 3 parts of maltodextrin, 10 parts of polygonum multiflorum extract, 15 parts of black mulberry extract, 35 parts of grape seed extract, 3 parts of methylparaben, 4 parts of propylparaben, 3 parts of zinc oxide, 3 parts of β -sitosterol, 17 parts of modified colorant and 40 parts of glycerol.

The preparation method of the modified colorant comprises the following steps: adding sodium metasilicate solution into petroleum ether solution, continuously stirring to form sol gel, adding silane cross-linking agent, tannic acid and gallic acid, finally adding ammonium chloride solution, evaporating and washing to obtain agent A; adding epoxy modified silicone oil and a secondary amine compound into a container, adding absolute ethyl alcohol, heating to 73 ℃ for reaction for 3 hours, distilling to remove the absolute ethyl alcohol, reducing pressure, and distilling unreacted raw materials at 150 ℃ to obtain an agent B; mixing the agent A and the agent B to obtain the modified colorant.

adding cetearyl alcohol and ceteareth-20 into glycerol, dispersing with glycerol to form a glycerol dispersion, weighing raw material water, adding the raw material water into a water phase tank, heating to 89 ℃, adding the glycerol dispersion into an oil phase tank, heating to 89 ℃, pumping the water phase into an emulsification tank, starting stirring, pumping an oil phase into the emulsification tank, homogenizing for 10 minutes, adding ferrous sulfate, methyl hydroxybenzoate, propyl hydroxybenzoate, chitosan nanosol, maltodextrin, a polygonum multiflorum extract, a black mulberry fruit extract, a grape seed extract, a modified colorant, zinc oxide and β -sitosterol, and continuously stirring for 30 minutes to obtain the hair dye.

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

Experimental data:

1. hair flexibility test

The test is carried out by collecting common hair, carrying out stretching and bending tests on the hair dyed by the product of the invention and the hair dyed by the traditional hair dye, additionally arranging a comparison test, and the steps of other raw materials of the comparison test are the same as those of the example 1, except that no chitosan nano sol is added, and the results are as follows:

	tension of hair	Bending stress of hair
			Normal hair	1.53N	2.34N
After the product of the invention is dyed	1.44N	2.21N
			Comparative test	1.01N	1.74N
After the traditional hair dye has been used for dyeing hair	0.47N	0.55N

The experimental data show that the stress of the hair dyed by the product of the invention is almost the same as that of the normal hair, while the stress of the hair dyed by the traditional hair dye is obviously different from that of the normal hair, and the comparative test shows that the protection effect of the hair dyed by the hair dye without chitosan nano sol is obviously lower than that of the hair dye with chitosan nano sol, which shows that the hair dye prepared by the invention can not cause secondary damage to the hair quality while further ensuring the hair dyeing effect, and can effectively reduce the damage to the hair quality.

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 infection 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:

	integrity of hair	Moulding time	Molding retention ratio
				Normal hair	Is substantially intact	11min	78％
After the product of the invention is dyed	Is substantially intact	13min	77％
				After the traditional hair dye has been used for dyeing hair	Partial coke	35min	17％

Experimental data show that the hair dyed by the invention can be shaped in the conventional hair perming time, the damage degree of the hair is low due to the plant extract, the hair can have similar shaping retention rate with the normal hair, and the plasticity of the hair can be recovered through repairing the hair by the chitosan nano sol, so that the hair dyed by the invention can be subjected to normal hair perming.

2. Hair dyeing effect experiment

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

the experimental data can show that the hair dye is similar to the traditional hair dye in the satisfaction degree of users, the hair dyeing rate is similar, the hair color retention time is longer, the plasticity of the hair can be recovered through repairing the hair by the chitosan nano sol, so that the hair after hair dyeing can be normally permed, meanwhile, the chitosan nano sol is adopted to carry out wrapping protection on the surface of the hair, the adhesion of extracts such as polygonum multiflorum, black mulberry fruits, grape seeds and the like on the surface of the hair can be ensured, the adhesion of the dye in the wrapping on the hair can also be ensured, and the hair color retention time is longer. In addition, the preparation of the modified colorant allows the colorant to be immobilized in the nanoparticle by the silane crosslinker, allowing a plurality of dye molecules to be incorporated into one monosilicon particle, isolating it from the surrounding environment and skin, avoiding allergic reactions, while having good wash fastness and color retention.

3. Ion detection

The effective component of the extracts of the polygonum multiflorum and the black mulberry is stilbene glucoside, and the lead content is not more than 40mg/kg and the arsenic content is not more than 2mg/kg according to the national requirements of cosmetics.

In the experiment, the lead and arsenic ions of the product before and after passing through the ion grid are measured by adopting an atomic absorption spectrometry, and the content of the stilbene glucoside is measured by adopting HPLC.

Experimental data show that after passing through the ion grid, the content of lead ions and the content of arsenic ions are both obviously reduced and are obviously lower than the national requirements. Has no influence on the content of stilbene glucoside in the effective components.

4. Skin allergy test

The test object is prepared by directly testing by using stock solution.

The test animals and the breeding environment, common UK albino guinea pigs, were divided into three groups, test subject experimental group and positive subject experimental group, each group containing 20 animals, and test subject control group containing 10 animals. The weight is 226-292g, the temperature of the experimental animal feeding room is 19-26 ℃, and the relative mixing degree is 40-70%.

Test method the left side of the back of guinea pigs was shaved 24h before the test and the area was about 6cm 2. Inducing contact, applying 0.2m1 of inducing test substance on skin of 2cm × 2cm area of left hair of test substance experimental group animal, covering with two layers of gauze and one layer of cellophane, fixing with adhesive tape, and sealing for 6 hr. The same procedure is repeated for 7d and 14 d. The positive test group was treated with 0.4% 2, 4-dinitrochloropropyl benzene solution, and the test control group was treated with the same solvent. Excitation contact 14 days after the last induction, the right side of the animals in the test and control groups, which had been shaved before 24h, was coated with 0.2ml of the test substance, covered with two layers of gauze and a layer of glass, and sealed with adhesive tape for 6h, and the positive test group was similarly contacted with 0.2% 2, 4-dinitro-chlorophenyl acrylate solution. Skin reactions were observed 24h and 48h after challenge, and skin reaction scores and sensitization intensity were graded according to the regulations of the cosmetic hygiene code.

The experimental results are as follows:

the conclusion is that the test result of the skin allergy of the guinea pig by the test object shows that 0 case of animals with the total erythema edema score more than or equal to 2, the sensitization rate is 0 percent, and no skin allergy is seen.

5. Salmonella typhimurium/reverse mutation experiment

Materials and methods: test bacteria TA97, TA98, TA100 and TA102 were preserved in liquid nitrogen.

Metabolism activating system adopting polychlorinated biphenyl to induce SD rat liver homogenate S₉Protein content 37.7mg/ml, S₉The mixed solution contains S₉The component is 10%As an in vitro metabolic activation system.

The sample preparation method comprises the following steps: the test substances were prepared as 400g/ml, 200mg/ml, 100mg/m1, 50mg/m1, 20mg/m1 solutions with sterile distilled water.

Pre-test results and experimental design:

test results

The dissolution characteristic is that the water-soluble polymer can be mutually dissolved

Addition of S₉(+S₉) Maximum dose of 40 mg/dish

Without addition of S₉(-S₉) Maximum dose of 20 mg/dish

And (3) experimental design: the solvent is sterile distilled water according to the using method of the sample and the result of the preliminary test.

The test dose is as follows:

+S₉the highest dose of the test is 40 mg/vessel, and 20 mg/vessel, 10 mg/vessel and 5 mg/vessel are arranged below the test vessel;

-S₉the highest dose of the test is 20 mg/dish, and 10 mg/dish, 5 mg/dish and 2 mg/dish are arranged below the test.

Test control group:

blank control, spontaneous reversion; solvent control, sterile distilled water 100 mu 1/dish; positive control:

-S₉TA97ICR-191 (1. mu.g/dish), TA98 p-nitroquinoline (200. mu.g/dish), TA100, TA102 Methyl Methanesulfonate (MMS) (1. mu.1/dish);

+S₉TA97, TA98, TA 1002-aminofluorene (10. mu.g/dish), TA1021, 8-dihydroxyanthraquinone (50. mu.g/m).

The test method comprises the following steps:

according to the laboratory test of Salmonella typhimurium/reversion mutation of the sanitary ministry of cosmetics, the mutagenicity of the sample is detected, 0.1ml of test strain enrichment liquid, 0.1ml of test substance solution and S are sequentially added into top agar at the temperature of 2m and 145 DEG C₉Mixed solution 0.5ml (+ S)₉0.1mol/LPBS (pH7.4)0.5ml (-S)₉In the preparation method, the mixture is fully and uniformly mixed, quickly poured onto an agar plate at the bottom layer, the plate is rotated to be uniformly distributed and horizontally placed, the plate is inverted after being cooled and solidified, the plate is cultured at 37 ℃ for 48 hours, and the number of recovered colonies in each dish is recorded.

-S₉The experimental results are as follows:

+S₉the experimental results are as follows:

as can be seen from the experimental results, the test substance is 2mg to 20mg per plate, without adding S₉The number of recovered colonies detected by an activation system plate doping method is 2 times lower than that of solvent control, and a dose response relation is not presented; per m5mg to 40mg of test substance, S is added₉The number of recovered colonies detected by the activation system plate incorporation method is 2 times lower than that of the solvent control, the dose response relationship is not shown, and the Ames test detection result 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. An anti-allergy hair dye containing plant extracts is characterized by comprising 10-20 parts of cetearyl alcohol, 10-20 parts of ceteareth-20, 5-8 parts of ammonia, 5-8 parts of thioglycolic acid, 120-140 parts of water, 80-100 parts of chitosan, 10-13 parts of ferrous sulfate, 2-4 parts of maltodextrin, 5-15 parts of polygonum multiflorum extracts, 10-20 parts of black mulberry extracts, 20-40 parts of grape seed extracts, 2-5 parts of methyl hydroxybenzoate, 2-5 parts of propyl hydroxybenzoate, 2-4 parts of zinc oxide, 3-8 parts of β -sitosterol, 15-20 parts of modified colorants and 30-40 parts of glycerol.

2. The anti-sensitivity hair dye containing plant extracts according to claim 1, wherein the modified hair dye is prepared by the following method: adding sodium metasilicate solution into petroleum ether solution, continuously stirring to form sol gel, adding silane cross-linking agent, tannic acid and gallic acid, finally adding ammonium chloride solution, evaporating and washing to obtain agent A; 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, distilling to remove the absolute ethyl alcohol, reducing pressure, and distilling unreacted raw materials at the temperature of 100-150 ℃ to obtain an agent B; mixing the agent A and the agent B to obtain the modified colorant.

3. The method for producing an anti-sensitivity hair dye containing a plant extract as claimed in claim 1 or 2, comprising the steps of:

4. The method for preparing an anti-sensitivity hair dye containing plant extracts as claimed in claim 3, wherein the black mulberry and polygonum multiflorum are extracted by the following steps:

5. The method for preparing an anti-sensitivity hair dye containing plant extracts as claimed in claim 4, wherein the process for extracting black mulberry and polygonum multiflorum comprises the following specific steps:

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

6. The method for preparing an anti-sensitivity hair dye containing plant extracts as claimed in claim 3, wherein the grape seed extraction process comprises: 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.