Plant hair dye containing gallnut extract and walnut extract and preparation method thereof

Abstract

The invention discloses a plant hair dye containing a gallnut extract and a walnut extract. The plant hair dye comprises an agent I and an agent II, the agent I comprises a coloring agent, a reducing agent, a pH conditioning agent A, an emulsifying agent, a hair conditioning agent A, a thickening agent, an aromatic agent, a preservative A and the balance of water, and the coloring agent comprises a gallnut extract, a walnut extract and PAMAM according to the mass ratio of (1-10): (1-10): 1; the agent II comprises a mordant, a humectant, an antioxidant, a thickener, a pH conditioner B, an aromatic, a hair conditioner B, a preservative B and the balance of water, and the mordant contains ferrous ion salt. According to the plant hair dye disclosed by the invention, the PAMAM, the gallnut extract and the walnut extract are directly physically acted, so that the problem of insufficient color fastness of a traditional plant hair dye is effectively solved. The invention further provides a preparation method of the plant hair dye, the preparation process is simple, and the prepared hair dye is uniform in color and good in washing fastness after hair dyeing.

Description

Technical Field

[0001] The present invention relates to the technical field of cosmetics, and more particularly to a plant hair dye containing a gallnut extract and a walnut extract and a preparation method thereof. Background Art

[0002] Hair dye is a kind of cosmetic used to dye hair. Existing hair dyes are divided into: plant hair dyes, metal hair dyes and oxidative hair dyes. The mechanism of action of metal hair dyes is that the metal ions in the dyes penetrate into the hair and react with the sulfur in the cysteine ​​in the hair protein to generate black lead sulfide, etc., which dyes the hair black. The heavy metal ions contained in metal hair dyes are not only harmful to the health of the hair and prone to allergies, but can also easily cause cumulative poisoning, which is very harmful to the human body. Oxidative dyes are composed of intermediates, couplers and oxidants. Small molecule dye intermediates and couplers first penetrate into the cortex and medulla of the hair. The oxidants oxidize the intermediates and then react with the couplers to form larger dye molecules, which penetrate into the hair fibers, thereby achieving a lasting dyeing effect. The oxidants used mainly include hydrogen peroxide, p-phenylenediamine and some of its derivatives. There are safety hazards such as sensitization, carcinogenesis, hair loss, and damage to the liver and lungs. In addition, the combined action of couplers and oxidants during the dyeing process will cause the original melanin in the hair to fade, resulting in more and more gray hair.

[0003] Plant hair dyes are dyed using substances extracted from the flowers, stems and leaves of plants. They are less harmful to the human body and will not cause skin allergies. For example, the patent with application number 202010462464.X discloses a plant hair dye, which is prepared with plant extracts such as gallnut extract as the main dye. However, the plant hair dye has poor coloring ability and the color fades quickly after dyeing. Summary of the invention

[0004] One object of the present invention is to provide a plant hair dye containing gallnut extract and walnut extract, including agent I and agent II; The agent I comprises the following components in mass fractions: colorant 6.8-11.5%, reducing agent 4-6%, pH conditioner A 4-6.8%, emulsifier 2.1-4.2%, hair conditioner A 2.1-3.5%, thickener 0.7-1%, fragrance 0.6-0.8%, preservative A 0.1-0.4%, and the balance is water, wherein the colorant comprises gallnut extract, walnut extract, and PAMAM, and the mass ratio of the gallnut extract, the walnut extract, and the PAMAM is 1-10:1-10:1; The agent II comprises the following components in mass fractions: mordant 7-9%, moisturizer 1-2%, antioxidant 0.05-0.1%, thickener 1-1.2%, pH conditioner B 0.1-0.3%, fragrance 0.1-0.3%, hair conditioner B 1.1-2.2%, preservative B 0.03-0.05%, and the balance is water, wherein the mordant contains divalent iron ion salt.

[0005] Preferably, the reducing agent is cysteamine hydrochloride, the thickener is hydroxyethyl cellulose, the aromatic agent is essence, the humectant is propylene glycol, and the antioxidant is ascorbic acid.

[0006] Preferably, the pH adjuster A comprises the following components in the mass fraction of the total amount of the components of agent I: 2-2.8% ethanolamine and 2-4% ammonium hydroxide; The pH adjuster B is citric acid.

[0007] Preferably, the emulsifier includes the following components in weight fraction based on the total amount of the components of Agent I: 1-2% cetearyl alcohol, 1-2% cetearyl alcohol polyether-25, and 0.1-0.2% cocoyl monoethanolamine.

[0008] Preferably, the hair conditioner A comprises the following components in the mass fraction of the total amount of the components of agent I: 1-2% stearyl trimethyl ammonium chloride, 0.8-1% mineral oil, 0.1-0.2% silk amino acids, 0.07-0.1% ginkgo leaf extract, 0.08-0.1% ginger root extract, and 0.08-0.1% motherwort extract; The hair conditioner B comprises the following components in terms of mass fraction accounting for the total amount of the components of agent II: 1-2% stearyl trimethyl ammonium chloride and 0.1-0.2% silk amino acids.

[0009] Preferably, the preservative A comprises the following components in weight fractions of the total amount of the components of the dosage I: 0.1-0.3% methylparaben and 0.06-0.1% propylparaben; The preservative B is kason.

[0010] Preferably, the mordant includes one or more of ferrous sulfate, ferrous chloride, ferrous nitrate, ferrous gluconate, ferrous fumarate, ferrous lactate, and ferrous tartrate.

[0011] Preferably, the silk amino acids are water-soluble silk amino acids, and the specific preparation method thereof includes: opening cocoons, selecting cocoons, washing cocoons, separating silk amino acids, cooling and freezing, thawing, filtering and pressing, drying, grinding and steam boiler sterilization.

[0012] Provided is a method for preparing the plant hair dye containing gallnut extract and walnut extract, including a method for preparing agent I and a method for preparing agent II; The preparation method of the I agent comprises the following steps: Step 1, adding water to the gallnut extract, walnut extract, PAMAM, stearyltrimethylammonium chloride and hydroxyethyl cellulose, stirring and heating to 80-85° C. to obtain phase A; Step 2: Stir cetearyl alcohol, ceteareth-25, mineral oil, methylparaben, cocoyl monoethanolamine, and propylparaben, and heat to 80-85° C. to obtain phase B; Step 3: Mix phase A and phase B and emulsify them, homogenize for 3-5 minutes, and keep warm for 15-20 minutes; Step 4: Cool the product of step 3 to 58-60°C, add cysteamine hydrochloride, silk amino acids, ginkgo leaf extract, ginger root extract, motherwort extract, and water, stir evenly, and continue to cool to below 45°C; Step 5: Add ammonium hydroxide, ethanolamine and essence to the product of step 4 and stir evenly; The preparation method of the II agent comprises the following steps: S1, add water to propylene glycol, hydroxyethyl cellulose and stearyl trimethyl ammonium chloride, stir and heat to 60-70°C; S2. Cool the product of step S1 to 42-45°C, add ferrous sulfate, silk amino acids, citric acid, ascorbic acid and water, stir until completely dissolved, then add kasone and essence, and stir evenly.

[0013] The present invention has at least the following beneficial effects: First, the present invention uses PAMAM to directly physically interact with the gallnut extract and walnut extract to assist the gallnut extract and walnut extract in coloring and improving color fastness, thereby effectively solving the problem of insufficient color fastness of traditional plant hair dyes.

[0014] Second, the hair dye prepared by the present invention has simple components, wherein the gallnut extract, walnut extract, ginkgo leaf extract, ginger root extract and motherwort extract are all of natural origin. The prepared hair dye product is safe, non-toxic and has no allergic reaction.

[0015] Thirdly, the hair dye of the present invention has a simple preparation process and is easy to use. The prepared hair dye has uniform color after dyeing hair and has good washing resistance.

[0016] Other advantages, objectives and features of the present invention will be embodied in part through the following description, and in part will be understood by those skilled in the art through study and practice of the present invention. DETAILED DESCRIPTION

[0017] The present invention is further described in detail below in conjunction with embodiments so that those skilled in the art can implement the invention with reference to the description.

[0018] It should be noted that the experimental methods described in the following embodiments are conventional methods unless otherwise specified, and the reagents and materials can be obtained from commercial channels unless otherwise specified.

[0019] PAMAM is a polyamide-amine dendritic polymer, which has a large number of amino groups on the surface, a highly geometrically symmetrical molecular structure, and a cavity inside the molecule. The PAMAM used in the following examples was purchased from Aladdin Reagent Network, with a CAS number of 155773-72-1 and a molecular formula of C 22 H 48 N 10 O4, molecular weight is 516.68.

[0020] Mineral oil, also known as liquid paraffin, was purchased with a CAS number of 8012-95-1.

[0021] Silk amino acids are soluble silk amino acids, and the specific preparation method thereof includes: A1. Opening the cocoon: Open the cocoon, the opening should not be larger than one-third of the cocoon, but do not cut it off, and take out the silkworm pupa; A2. Cocoon selection: After removing the silkworm pupae, select the cocoons without silkworm excrement on the inner wall. The cocoons with silkworm excrement on the inner wall are inferior products and are used to make silk cotton for other purposes. A3. Washing cocoons: Wash the selected cocoons with clean water to remove dust and washable pollutants, then use a spin dryer to dry them and put them into mesh bags for later use; A4. Separation of silk amino acids: Put the cocoons in a net bag into a high-temperature distillation kettle, set the temperature to 120°C, mix the cocoons and water in a mass ratio of 1:3, and steam for 3 hours. Then, add pure water at not less than 60°C, wash the cocoons for 5 minutes, wash the silk amino acids trapped in the cocoons, and pour the obtained soluble silk amino acid solution into a liquid storage tank for cooling; A5. Cooling and freezing: naturally cool the soluble silk amino acid solution in the liquid storage tank to 40°C, and freeze the soluble silk amino acid solution in a freezing chamber at -2°C for 48 hours until the soluble silk amino acid solution is completely frozen into ice cubes; A6. Thawing: Put the soluble silk amino acid solution ice cubes into a constant temperature oven and set the temperature to 25°C. The water in the ice cubes will dissolve and the soluble silk amino acids will precipitate into muddy flocs. A7, Filtration and pressure: In a dust-free environment at 4~25℃, water and muddy soluble silk amino acids are separated by filtration and pressure equipment to obtain muddy soluble silk amino acids; A8. Drying: Spread out the mud-like soluble silk amino acid and bake it in a drying machine at 60°C until it is completely dry; A9. Grinding: Put the dried block-shaped soluble silk amino acid into a grinder and grind it to 200-5000 mesh to obtain silk amino acid; A10. Steam sterilization: Silk amino acids are sterilized in a steam pot and then vacuum packed.

[0022] <Example 1> A method for preparing a plant hair dye containing a gallnut extract and a walnut extract, including a method for preparing agent I and a method for preparing agent II; The preparation method of dose I comprises the following steps: Step 1, add 20.00 g of water to 5.00 g of gallnut extract, 5.00 g of walnut extract, 0.50 g of PAMAM, 2.00 g of stearyltrimethylammonium chloride, and 1.00 g of hydroxyethyl cellulose, stir and heat to 85° C. to obtain phase A; Step 2: 1.00 g of cetearyl alcohol, 1.00 g of ceteareth-25, 0.80 g of mineral oil, 0.20 g of methylparaben, 0.15 g of cocoyl monoethanolamine, and 0.08 g of propylparaben are stirred and heated to 85° C. to obtain phase B; Step 3: Mix phase A and phase B and emulsify them, homogenize for 5 minutes, and keep warm for 15 minutes; Step 4: Cool the product of step 3 to 58°C, add 4.00 g cysteamine hydrochloride, 0.10 g silk amino acids, 0.10 g ginkgo leaf extract, 0.10 g ginger root extract, 0.10 g motherwort extract, and 53.87 g water, stir evenly, and continue to cool to 40°C; Step 5: Add 2.00 g of ammonium hydroxide, 2.00 g of ethanolamine, and 1.00 g of essence to the product of step 4 and stir evenly; The preparation method of agent II comprises the following steps: S1, add 40.00 g of water to 2.00 g of propylene glycol, 1.00 g of hydroxyethyl cellulose and 1.00 g of stearyl trimethyl ammonium chloride, stir and heat to 60°C; S2. Cool the product of step S1 to 45°C, add 7.00 g ferrous sulfate, 0.20 g silk amino acids, 0.10 g citric acid, 0.10 g ascorbic acid, and 48.25 g water, stir until completely dissolved, then add 0.05 g kason and 0.30 g essence, and stir evenly.

[0023] The prepared agent I and agent II are sealed and packaged separately to form the plant hair dye packaging.

[0024] <Example 2> A method for preparing a plant hair dye containing a gallnut extract and a walnut extract, including a method for preparing agent I and a method for preparing agent II; The preparation method of dose I comprises the following steps: Step 1, add 20.00 g of water to 5.00 g of gallnut extract, 5.00 g of walnut extract, 1.00 g of PAMAM, 2.00 g of stearyltrimethylammonium chloride, and 1.00 g of hydroxyethyl cellulose, stir and heat to 85° C. to obtain phase A; Step 2: 1.00 g of cetearyl alcohol, 1.00 g of ceteareth-25, 0.80 g of mineral oil, 0.25 g of methylparaben, 0.15 g of cocoyl monoethanolamine, and 0.08 g of propylparaben are stirred and heated to 85° C. to obtain phase B; Step 3: Mix phase A and phase B and emulsify them, homogenize for 5 minutes, and keep warm for 15 minutes; Step 4: Cool the product of step 3 to 58°C, add 5.00 g cysteamine hydrochloride, 0.10 g silk amino acids, 0.10 g ginkgo leaf extract, 0.10 g ginger root extract, 0.10 g motherwort extract, and 50.82 g water, stir evenly, and continue to cool to 40°C; Step 5: Add 2.50 g of ammonium hydroxide, 3.00 g of ethanolamine and 1.00 g of essence to the product of step 4 and stir evenly; The preparation method of agent II comprises the following steps: S1, add 40.00 g of water to 2.00 g of propylene glycol, 1.00 g of hydroxyethyl cellulose and 1.00 g of stearyl trimethyl ammonium chloride, stir and heat to 60°C; S2. Cool the product of step S1 to 45°C, add 8.00 g ferrous sulfate, 0.20 g silk amino acids, 0.10 g citric acid, 0.10 g ascorbic acid, and 47.25 g water, stir until completely dissolved, then add 0.05 g kason and 0.30 g essence, and stir evenly.

[0025] The prepared agent I and agent II are sealed and packaged separately to form the plant hair dye packaging.

[0026] <Example 3> A method for preparing a plant hair dye containing a gallnut extract and a walnut extract, including a method for preparing agent I and a method for preparing agent II; The preparation method of dose I comprises the following steps: Step 1, add 20.00 g of water to 5.00 g of gallnut extract, 5.00 g of walnut extract, 1.50 g of PAMAM, 2.00 g of stearyltrimethylammonium chloride, and 0.70 g of hydroxyethyl cellulose, stir and heat to 85° C. to obtain phase A; Step 2: Stir 2.00 g of cetearyl alcohol, 2.00 g of ceteareth-25, 1.00 g of mineral oil, 0.30 g of methylparaben, 0.20 g of cocoyl monoethanolamine, and 0.10 g of propylparaben, and heat to 85° C. to obtain phase B; Step 3: Mix phase A and phase B and emulsify them, homogenize for 5 minutes, and keep warm for 15 minutes; Step 4: Cool the product of step 3 to 58°C, add 6.00 g cysteamine hydrochloride, 0.20 g silk amino acids, 0.10 g ginkgo leaf extract, 0.10 g ginger root extract, 0.10 g motherwort extract, and 45.90 g water, stir evenly, and continue to cool to 40°C; Step 5: Add 2.80 g of ammonium hydroxide, 4.00 g of ethanolamine, and 1.00 g of essence to the product of step 4 and stir evenly; The preparation method of agent II comprises the following steps: S1, add 40.00 g of water to 2.00 g of propylene glycol, 1.20 g of hydroxyethyl cellulose and 1.00 g of stearyl trimethyl ammonium chloride, stir and heat to 60°C; S2. Cool the product of step S1 to 45°C, add 9.00 g ferrous sulfate, 0.20 g silk amino acids, 0.10 g citric acid, 0.10 g ascorbic acid, and 46.05 g water, stir until completely dissolved, then add 0.05 g kason and 0.30 g essence, and stir evenly.

[0027] The prepared agent I and agent II are sealed and packaged separately to form the plant hair dye packaging.

[0028] <Example 4> A method for preparing a plant hair dye containing a gallnut extract and a walnut extract, including a method for preparing agent I and a method for preparing agent II; The preparation method of dose I comprises the following steps: Step 1, add 20.00 g of water to 4.00 g of gallnut extract, 6.00 g of walnut extract, 1.00 g of PAMAM, 2.00 g of stearyltrimethylammonium chloride, and 1.00 g of hydroxyethyl cellulose, stir and heat to 85° C. to obtain phase A; Step 2: 1.00 g of cetearyl alcohol, 1.00 g of ceteareth-25, 0.80 g of mineral oil, 0.25 g of methylparaben, 0.15 g of cocoyl monoethanolamine, and 0.08 g of propylparaben are stirred and heated to 85° C. to obtain phase B; Step 3: Mix phase A and phase B and emulsify them, homogenize for 5 minutes, and keep warm for 15 minutes; Step 4: Cool the product of step 3 to 58°C, add 5.00 g cysteamine hydrochloride, 0.10 g silk amino acids, 0.10 g ginkgo leaf extract, 0.10 g ginger root extract, 0.10 g motherwort extract, and 50.82 g water, stir evenly, and continue to cool to 40°C; Step 5: Add 2.50 g of ammonium hydroxide, 3.00 g of ethanolamine and 1.00 g of essence to the product of step 4 and stir evenly; The preparation method of agent II comprises the following steps: S1, add 40.00 g of water to 2.00 g of propylene glycol, 1.00 g of hydroxyethyl cellulose and 1.00 g of stearyl trimethyl ammonium chloride, stir and heat to 60°C; S2. Cool the product of step S1 to 45°C, add 8.00 g ferrous sulfate, 0.20 g silk amino acids, 0.10 g citric acid, 0.10 g ascorbic acid, and 47.25 g water, stir until completely dissolved, then add 0.05 g kason and 0.30 g essence, and stir evenly.

[0029] The prepared agent I and agent II are sealed and packaged separately to form the plant hair dye packaging.

[0030] <Example 5> A method for preparing a plant hair dye containing a gallnut extract and a walnut extract, including a method for preparing agent I and a method for preparing agent II; The preparation method of dose I comprises the following steps: Step 1, add 20.00 g of water to 6.00 g of gallnut extract, 4.00 g of walnut extract, 1.00 g of PAMAM, 2.00 g of stearyltrimethylammonium chloride, and 1.00 g of hydroxyethyl cellulose, stir and heat to 85° C. to obtain phase A; Step 2: 1.00 g of cetearyl alcohol, 1.00 g of ceteareth-25, 0.80 g of mineral oil, 0.25 g of methylparaben, 0.15 g of cocoyl monoethanolamine, and 0.08 g of propylparaben are stirred and heated to 85° C. to obtain phase B; Step 3: Mix phase A and phase B and emulsify them, homogenize for 5 minutes, and keep warm for 15 minutes; Step 4: Cool the product of step 3 to 58°C, add 5.00 g cysteamine hydrochloride, 0.10 g silk amino acids, 0.10 g ginkgo leaf extract, 0.10 g ginger root extract, 0.10 g motherwort extract, and 50.82 g water, stir evenly, and continue to cool to 40°C; Step 5: Add 2.50 g of ammonium hydroxide, 3.00 g of ethanolamine and 1.00 g of essence to the product of step 4 and stir evenly; The preparation method of agent II comprises the following steps: S1, add 40.00 g of water to 2.00 g of propylene glycol, 1.00 g of hydroxyethyl cellulose and 1.00 g of stearyl trimethyl ammonium chloride, stir and heat to 60°C; S2. Cool the product of step S1 to 45°C, add 8.00 g ferrous sulfate, 0.20 g silk amino acids, 0.10 g citric acid, 0.10 g ascorbic acid, and 47.25 g water, stir until completely dissolved, then add 0.05 g kason and 0.30 g essence, and stir evenly.

[0031] The prepared agent I and agent II are sealed and packaged separately to form the plant hair dye packaging.

[0032] <Blank Group> A method for preparing a plant hair dye containing a gallnut extract and a walnut extract, including a method for preparing agent I and a method for preparing agent II; The preparation method of dose I comprises the following steps: Step 1, add 20.00 g of water to 6.00 g of gallnut extract, 4.00 g of walnut extract, 2.00 g of stearyltrimethylammonium chloride and 1.00 g of hydroxyethyl cellulose, stir and heat to 85° C. to obtain phase A; Step 2: 1.00 g of cetearyl alcohol, 1.00 g of ceteareth-25, 0.80 g of mineral oil, 0.25 g of methylparaben, 0.15 g of cocoyl monoethanolamine, and 0.08 g of propylparaben are stirred and heated to 85° C. to obtain phase B; Step 3: Mix phase A and phase B and emulsify them, homogenize for 5 minutes, and keep warm for 15 minutes; Step 4: Cool the product of step 3 to 58°C, add 5.00 g cysteamine hydrochloride, 0.10 g silk amino acids, 0.10 g ginkgo leaf extract, 0.10 g ginger root extract, 0.10 g motherwort extract, and 51.82 g water, stir evenly, and continue to cool to 40°C; Step 5: Add 2.50 g of ammonium hydroxide, 3.00 g of ethanolamine and 1.00 g of essence to the product of step 4 and stir evenly; The preparation method of agent II comprises the following steps: S1, add 40.00 g of water to 2.00 g of propylene glycol, 1.00 g of hydroxyethyl cellulose and 1.00 g of stearyl trimethyl ammonium chloride, stir and heat to 60°C; S2. Cool the product of step S1 to 45°C, add 8.00 g ferrous sulfate, 0.20 g silk amino acids, 0.10 g citric acid, 0.10 g ascorbic acid, and 47.25 g water, stir until completely dissolved, then add 0.05 g kason and 0.30 g essence, and stir evenly.

[0033] The prepared agent I and agent II are sealed and packaged separately to form the plant hair dye packaging.

[0034] <Comparative Example 1> A method for preparing a plant hair dye containing a gallnut extract and a walnut extract, including a method for preparing agent I and a method for preparing agent II; The preparation method of dose I comprises the following steps: Step 1, add 20.00 g of water to 7.00 g of gallnut extract, 4.00 g of walnut extract, 2.00 g of stearyltrimethylammonium chloride and 1.00 g of hydroxyethyl cellulose, stir and heat to 85°C to obtain phase A; Step 2: 1.00 g of cetearyl alcohol, 1.00 g of ceteareth-25, 0.80 g of mineral oil, 0.25 g of methylparaben, 0.15 g of cocoyl monoethanolamine, and 0.08 g of propylparaben are stirred and heated to 85° C. to obtain phase B; Step 3: Mix phase A and phase B and emulsify them, homogenize for 5 minutes, and keep warm for 15 minutes; Step 4: Cool the product of step 3 to 58°C, add 5.00 g cysteamine hydrochloride, 0.10 g silk amino acids, 0.10 g ginkgo leaf extract, 0.10 g ginger root extract, 0.10 g motherwort extract, and 50.82 g water, stir evenly, and continue to cool to 40°C; Step 5: Add 2.50 g of ammonium hydroxide, 3.00 g of ethanolamine and 1.00 g of essence to the product of step 4 and stir evenly; The preparation method of agent II comprises the following steps: S1, add 40.00 g of water to 2.00 g of propylene glycol, 1.00 g of hydroxyethyl cellulose and 1.00 g of stearyl trimethyl ammonium chloride, stir and heat to 60°C; S2. Cool the product of step S1 to 45°C, add 8.00 g ferrous sulfate, 0.20 g silk amino acids, 0.10 g citric acid, 0.10 g ascorbic acid, and 47.25 g water, stir until completely dissolved, then add 0.05 g kason and 0.30 g essence, and stir evenly.

[0035] The prepared agent I and agent II are sealed and packaged separately to form the plant hair dye packaging.

[0036] <Comparative Example 2> A method for preparing a plant hair dye containing a gallnut extract and a walnut extract, including a method for preparing agent I and a method for preparing agent II; The preparation method of dose I comprises the following steps: Step 1, add 20.00 g of water to 6.00 g of gallnut extract, 4.00 g of walnut extract, 2.00 g of stearyltrimethylammonium chloride and 1.00 g of hydroxyethyl cellulose, stir and heat to 85° C. to obtain phase A; Step 2: 1.00 g of cetearyl alcohol, 1.00 g of ceteareth-25, 0.80 g of mineral oil, 0.25 g of methylparaben, 0.15 g of cocoyl monoethanolamine, and 0.08 g of propylparaben are stirred and heated to 85° C. to obtain phase B; Step 3: Mix phase A and phase B and emulsify them, homogenize for 5 minutes, and keep warm for 15 minutes; Step 4: Cool the product of step 3 to 58°C, add 5.00 g cysteamine hydrochloride, 0.10 g silk amino acids, 0.10 g ginkgo leaf extract, 0.10 g ginger root extract, 0.10 g motherwort extract, and 51.82 g water, stir evenly, and continue to cool to 40°C; Step 5: Add 2.50 g of ammonium hydroxide, 3.00 g of ethanolamine and 1.00 g of essence to the product of step 4 and stir evenly; The preparation method of agent II comprises the following steps: S1, add 40.00 g of water to 2.00 g of propylene glycol, 1.00 g of hydroxyethyl cellulose, 1.00 g of stearyl trimethyl ammonium chloride, and 1.00 g of PAMAM, stir and heat to 60°C; S2. Cool the product of step S1 to 45°C, add 8.00 g ferrous sulfate, 0.20 g silk amino acids, 0.10 g citric acid, 0.10 g ascorbic acid, and 46.25 g water, stir until completely dissolved, then add 0.05 g kason and 0.30 g essence, and stir evenly.

[0037] The prepared agent I and agent II are sealed and packaged separately to form the plant hair dye packaging.

[0038] <Dyeing Experiment> Washed and dried white hair samples were taken and evenly divided into multiple groups. The hair dyes prepared in Examples 1 to 5, Comparative Examples 1 to 2 and the blank group were used to dye the white hair samples. The amounts of Agent I and Agent II were determined according to the amount of hair, and were specifically determined based on the amount of hair that could be evenly applied to the hair samples. The hair dyeing method comprising the following steps: 1) Use a comb to evenly apply Agent I on the hair sample, put on a shower cap, and leave it at room temperature for 30 minutes; 2) Comb off the excess Agent I, then evenly apply Agent II, put on a shower cap, leave at room temperature for 20 minutes, rinse with clean water, and blow dry. The amount of Agent II to be applied should not be less than the amount of Agent I.

[0039] <Control group 1> The control group is a commercially available oxidative hair dye, including Agent Ⅰ and Agent Ⅱ: Composition of dose I: cetostearyl alcohol, octadecyltrimethylammonium chloride, oleyl alcohol ether, p-phenylenediamine, resorcinol, m-aminophenol, sulfurous acid, isoascorbic acid, ethanolamine, and the balance is water; Composition of dose II: cetostearyl alcohol, oleyl alcohol ether, hydrogen peroxide, disodium hydrogen phosphate, phosphoric acid, sodium stannate, and the balance is water.

[0040] Hair dyeing method: Mix Agent I and Agent II in a mass ratio of 1:1.5, stir evenly, and then apply evenly on the same white hair sample as above, keep at 30°C for 40 minutes, rinse the hair with clean water, and blow dry.

[0041] <Control group 2> This control group refers to the preparation method in the patent with application number 202010462464.X to prepare the plant hair dye, and the specific operation steps are as follows: 1.0 g AEO-3 (fatty alcohol polyoxyethylene ether), 0.3 g essence, 5.0 g propylene glycol and 69.7 g deionized water were added into a reactor, heated to 45°C, stirred until the mixture was evenly distributed, and then 0.2 g EDTA disodium salt, 5.0 g sodium lactate 50% solution, 10.0 g gallnut plant extract, 5.0 g Polygonum multiflorum root extract, 3.0 g Platycladus orientalis leaf extract, 0.3 g citric acid, and 0.5 g sodium citrate were added in sequence, and stirring was continued at the same temperature until homogeneous, and then the temperature was lowered to room temperature, and the plant hair dye was obtained by aseptic filling.

[0042] Hair dyeing method: Make the above-mentioned water-based plant hair dye product into a spray type, spray it directly on the same white hair sample as above, comb it repeatedly with a comb, leave it at room temperature for 40 minutes, rinse it with clean water, wash it with shampoo, and blow dry.

[0043] <Color fastness test> The coloring effect of the hair dyed with the hair dyes of Examples 1 to 5, Comparative Examples 1 to 2, the blank group and the control group 1 to 2 was observed, and a color fastness test was performed. The specific color fastness test process is as follows: The dyed hair is placed in an aqueous solution containing 5% shampoo, and then placed on a vortex machine, and the speed is controlled to rotate at 40 r / min, and the hair is rinsed and blow-dried for 10 minutes each time. The test is repeated, and the number of washings for the first fading is recorded. The specific operation of judging whether the hair is faded includes: comparing the hair with a color number card under the same pair of light sources in a standard light box, wherein the color number card contains color areas with different chromaticity values. In the usual color number card, 1 degree represents blue-black, 2 degrees represent black-blue-brown, 3 degrees represent dark brown-brown, 4 degrees represent dark brown-red, 5 degrees represent dark brown-orange, 6 degrees represent brown-orange-yellow, 7 degrees represent brown-yellow-orange, 8 degrees represent golden yellow, 9 degrees represent light yellow, and 10 degrees represent very light yellow. When the chromaticity value of the hair changes after two adjacent washings, it is judged to be faded.

[0044] The results of the coloring effect and the number of washes for the first fading are shown in Table 1 below: Table 1 Coloring effect of hair dyed with each group of hair dyes and the number of washings for the first fading Group Coloring effect Number of washes for first fading Example 1 Bright black gloss 88 Example 2 Bright black gloss 93 Example 3 Bright black gloss 90 Example 4 Bright black gloss 91 Example 5 Bright black gloss 95 Blank Group Dark Black 60 Comparative Example 1 Bright black gloss 61 Comparative Example 2 Dark Black 61 Control group 1 black 52 Control group 2 Bright black gloss 63 From the experimental data in Table 1, it can be seen that the coloring effect and the number of washing times of the hair dyes of Examples 1 to 5 of the present invention are better than those of the blank group and the control group 1 to 2, indicating that the use of gallnut extract and walnut extract as the dyeing component, with the assistance of PAMAM, can effectively improve the coloring effect and significantly improve the color fastness; the hair dyes of Examples 1 to 5 have excellent coloring effects and all have a bright black luster, and when the mass ratio of gallnut extract, walnut extract and PAMAM is 6:4:1, the color fastness of the prepared dye is the best. The reason is analyzed. On the basis of PAMAM assisting the gallnut extract and walnut extract in coloring and improving the color fastness, the gallic acid in the gallnut extract can effectively connect the juglone in the walnut extract and the hair keratin, Further improve color fastness; Comparative Example 1 is compared with the blank group, the coloring effect is improved, but the number of water washings is not much different, indicating that the increase in the mass fraction of the gallnut extract can improve the coloring effect, but cannot change the color fastness; Example 3 is compared with Comparative Examples 1-2, the number of water washings is significantly improved, indicating that PAMAM has a direct physical effect with the gallnut extract and the walnut extract, and has the effect of assisting the gallnut extract and the walnut extract in coloring and improving the color fastness. The reason is analyzed. The large amount of amino groups contained in PAMAM can form hydrogen bonds with the large amount of phenolic hydroxyl groups in the gallnut extract, the carbonyl groups in the walnut extract and the hair keratin to reduce the nucleophilic attack of water molecules on the gallnut extract and the walnut extract, thereby improving the color fastness.

[0045] <Skin allergy test> In accordance with the Technical Specifications for Safety of Cosmetics (2015 edition), a skin allergy test was conducted on the hair dye sample prepared in Example 4 (the relative content of walnut extract in each example is relatively high) using a local closed skin coating test method.

[0046] Test animals and feeding environment: Common British albino guinea pigs were randomly divided into three groups, namely, experimental group, positive group, and experimental control group, with 20 in each group, weighing 200-300g. The temperature in the feeding room was 19-26℃, and the relative humidity was 40-70%. Feed was fed regularly and quantitatively during the feeding process. Test method: 24 hours before the test, shave the left side of the guinea pig's back, an area of ​​about 6 cm 2 ; Induced contact: 0.2 g of the hair dye sample was applied to the skin of the 2 cm × 2 cm area on the left side of the experimental group animals, covered with two layers of gauze and one layer of cellophane, fixed with adhesive tape, and sealed for 6 hours. The same method was repeated once on the 7th and 14th days. The guinea pigs in the positive group were smeared with 0.4% 2,4-dinitrochlorobenzene acetone solution in the same way, and the control group was smeared with distilled water in the same way; Provocative contact: On the 14th day after the last induction, 0.2 g of hair dye sample was applied to the skin of the experimental group and the experimental control group on the right side of the animals, which had been shaved 24 hours ago in an area of ​​2 cm × 2 cm, and covered with two layers of gauze and one layer of cellophane, and fixed with adhesive tape for 6 hours. The guinea pigs in the positive group were applied with 0.2% 2,4-dinitrochlorobenzene in acetone solution in the same way for the same provocative contact. The skin reaction was observed 24 and 48 hours after the provocative contact, and the skin reaction score and sensitization intensity were graded according to the relevant provisions of the "Safety Technical Specifications for Cosmetics" (2015 Edition) (Chapter VI). The test results are shown in Table 2 below. The * in the table indicates the total score of the skin erythema and edema reaction intensity. The sensitization rate is the percentage of animals with a total score of erythema and edema of skin allergic reaction ≥ 2 to the total number of animals in the experiment: Table 2 Results of skin allergy test From the data in Table 2, it can be seen that the hair dye prepared in Example 2 had an allergic reaction to the guinea pig skin with a total score of erythema and edema ≥ 2 in 0 animals, the sensitization rate was 0%, and no skin allergic reaction was observed.

[0047] <Heavy Metal Test> With reference to the test method in the "Technical Specification for Safety of Cosmetics" (2015 edition), the contents of lead, mercury, arsenic and cadmium in the hair dyes prepared in Examples 1 to 5 were determined, wherein the lead content was determined by graphite furnace atomic absorption spectrophotometry, and wet digestion was selected for sample treatment; the mercury content was determined by hydride atomic fluorescence spectrophotometry, and microwave digestion was selected for sample treatment; the arsenic content was determined by hydride atomic fluorescence spectrophotometry, and dry ashing was selected for sample treatment; the cadmium content was determined by flame atomic absorption spectrophotometry, and wet digestion was selected for sample treatment.

[0048] After measurement, it was found that the lead content in the hair dyes prepared in Examples 1 to 5 was less than 1.8 mg / kg, which met the standard requirement of QB / T1978-2016 "Hair Dyes" that the lead content in hair dyes should be ≤10 mg / kg; it was found that the mercury content in the hair dyes prepared in Examples 1 to 5 was less than 0.005 mg / kg, which met the standard requirement of QB / T1978-2016 "Hair Dyes" that the mercury content in hair dyes should be ≤1 mg / kg; it was found that the arsenic content in the hair dyes prepared in Examples 1 to 5 was less than 0.03 mg / kg, which met the standard requirement of QB / T1978-2016 "Hair Dyes" that the arsenic content in hair dyes should be ≤2 mg / kg; it was found that the cadmium content in the hair dyes prepared in Examples 1 to 5 was less than 0.008 mg / kg, which met the standard requirement of QB / T1978-2016 "Hair Dyes" that the cadmium content in hair dyes should be ≤5 mg / kg. The heavy metal content of the invention does not exceed the standard requirements and is at a relatively low level. The invention uses gallnut extract and walnut extract as dyeing components, and does not add processing aids harmful to the human body, so that the heavy metal content is maintained at a relatively low level.

[0049] Although the embodiments of the present invention have been disclosed as above, they are not limited to the applications listed in the specification and the implementation modes. They can be fully applied to various fields suitable for the present invention. For those familiar with the art, additional modifications can be easily implemented. Therefore, without departing from the general concept defined by the claims and the scope of equivalents, the present invention is not limited to the specific details and the embodiments shown and described herein.

Claims

1. A plant hair dye containing a gallnut extract and a walnut extract, characterized in that: Includes doses I and II; The agent I comprises the following components in mass fractions: colorant 6.8-11.5%, reducing agent 4-6%, pH conditioner A 4-6.8%, emulsifier 2.1-4.2%, hair conditioner A 2.1-3.5%, thickener 0.7-1%, fragrance 0.6-0.8%, preservative A 0.1-0.4%, and the balance is water, wherein the colorant comprises gallnut extract, walnut extract, and PAMAM, and the mass ratio of the gallnut extract, the walnut extract, and the PAMAM is 1-10:1-10:1; The agent II comprises the following components in mass fractions: mordant 7-9%, moisturizer 1-2%, antioxidant 0.05-0.1%, thickener 1-1.2%, pH conditioner B 0.1-0.3%, fragrance 0.1-0.3%, hair conditioner B 1.1-2.2%, preservative B 0.03-0.05%, and the balance is water, wherein the mordant contains divalent iron ion salt.

2. The plant hair dye containing the gallnut extract and the walnut extract according to claim 1, characterized in that: The reducing agent is cysteamine hydrochloride, the thickener is hydroxyethyl cellulose, the aromatic agent is essence, the moisturizing agent is propylene glycol, and the antioxidant is ascorbic acid.

3. The plant hair dye containing the gallnut extract and the walnut extract according to claim 1, characterized in that: The pH adjuster A comprises the following components by mass fraction accounting for the total amount of the components of agent I: 2-2.8% ethanolamine and 2-4% ammonium hydroxide; The pH adjuster B is citric acid.

4. The plant hair dye containing the gallnut extract and the walnut extract according to claim 1, characterized in that: The emulsifier includes the following components in weight fractions accounting for the total amount of the components of Agent I: 1-2% of cetearyl alcohol, 1-2% of cetearyl alcohol polyether-25, and 0.1-0.2% of cocoyl monoethanolamine.

5. The plant hair dye containing the gallnut extract and the walnut extract according to claim 1, characterized in that: The hair conditioning agent A comprises the following components in weight fraction of the total amount of the components of agent I: 1-2% stearyl trimethyl ammonium chloride, 0.8-1% mineral oil, 0.1-0.2% silk amino acids, 0.07-0.1% ginkgo leaf extract, 0.08-0.1% ginger root extract, and 0.08-0.1% motherwort extract; The hair conditioner B comprises the following components in terms of mass fraction accounting for the total amount of the components of agent II: 1-2% stearyl trimethyl ammonium chloride and 0.1-0.2% silk amino acids.

6. The plant hair dye containing the gallnut extract and the walnut extract according to claim 1, characterized in that: The preservative A includes the following components by mass fraction accounting for the total amount of the components of the first agent: 0.1-0.3% of methylparaben and 0.06-0.1% of propylparaben; The preservative B is kason.

7. The plant hair dye containing the gallnut extract and the walnut extract according to claim 1, characterized in that: The mordant includes one or more of ferrous sulfate, ferrous chloride, ferrous nitrate, ferrous gluconate, ferrous fumarate, ferrous lactate, and ferrous tartrate.

8. The plant hair dye containing the gallnut extract and the walnut extract according to claim 5, characterized in that: The silk amino acids are water-soluble silk amino acids, and the specific preparation method thereof comprises: opening silkworm cocoons, selecting cocoons, washing cocoons, separating silk amino acids, cooling and freezing, thawing, filtering and pressing, drying, grinding and steam boiler sterilization.

9. A method for preparing a plant hair dye containing a gallnut extract and a walnut extract according to any one of claims 1 to 8, characterized in that: Including a preparation method of dose I and a preparation method of dose II; The preparation method of the I agent comprises the following steps: Step 1, adding water to the gallnut extract, walnut extract, PAMAM, stearyltrimethylammonium chloride and hydroxyethyl cellulose, stirring and heating to 80-85° C. to obtain phase A; Step 2: Stir cetearyl alcohol, ceteareth-25, mineral oil, methylparaben, cocoyl monoethanolamine, and propylparaben, and heat to 80-85° C. to obtain phase B; Step 3: Mix phase A and phase B and emulsify them, homogenize for 3-5 minutes, and keep warm for 15-20 minutes; Step 4: Cool the product of step 3 to 58-60°C, add cysteamine hydrochloride, silk amino acids, ginkgo leaf extract, ginger root extract, motherwort extract, and water, stir evenly, and continue to cool to below 45°C; Step 5: Add ammonium hydroxide, ethanolamine and essence to the product of step 4 and stir evenly; The preparation method of the II agent comprises the following steps: S1, add water to propylene glycol, hydroxyethyl cellulose and stearyl trimethyl ammonium chloride, stir and heat to 60-70°C; S2. Cool the product of step S1 to 42-45°C, add ferrous sulfate, silk amino acids, citric acid, ascorbic acid and water, stir until completely dissolved, then add kasone and essence, and stir evenly.

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