Plant component hair dye with flexibility and preparation method thereof

Abstract

The invention discloses a plant component hair dye with flexibility and a preparation method thereof, and relates to the technical field of hair dyes, and the preparation method comprises the following steps: placing hydroxyethylidene-1, 1-diphosphonic acid, xanthan gum, hydroxyethyl cellulose and propylene glycol in deionized water, heating to 60-70 DEG C, uniformly stirring, cooling to 40-50 DEG C, adding a dye intermediate, a coupling agent and panthenol, uniformly stirring, cooling to 40-50 DEG C, adding an emulsifier, and uniformly stirring to obtain the plant component hair dye with flexibility. The preparation method comprises the following steps: uniformly stirring, adjusting the pH value to 8-10, adding polyquaternium-10, uniformly stirring, adding gallic acid microcapsules, ethyl cellulose coated bisabolol and modified graphene oxide, uniformly stirring, and removing impurities to obtain the hair dye.

Description

Technical Field

[0001] This invention relates to the field of hair dye technology, specifically to a plant-based hair dye with a smoothing effect and its preparation method. Background Technology

[0002] With the accelerating pace of modern life and increasing work pressure, people's pursuit of personal image management is becoming increasingly prominent. Hair dye, as an important tool for enhancing beauty, is driving the rapid development of China's hair dyeing industry. Hair dyes can be categorized into temporary, semi-permanent, and permanent types based on their duration. Permanent hair dyes are widely used due to their high colorfastness. The permanent hair dyeing process requires an oxidizing agent to bleach natural melanin and initiate a reaction between dye precursors to ultimately synthesize the dye compound.

[0003] However, current permanent hair dyes have problems such as poor color retention, risk of allergies, and dry, dull hair.

[0004] Therefore, it is of great significance to develop a hair dye with plant-based ingredients that has a smoothing effect. Summary of the Invention

[0005] The purpose of this invention is to provide a plant-based hair dye with smoothing properties and its preparation method, so as to solve the problems raised in the prior art.

[0006] To achieve the above objectives, the present invention provides the following technical solution:

[0007] A method for preparing a plant-based hair dye with softening properties includes the following steps:

[0008] Hydroxyethylidene diphosphate, xanthan gum, hydroxyethyl cellulose, and propylene glycol are placed in deionized water, heated to 60-70℃, stirred until homogeneous, cooled to 40-50℃, and dye intermediates, coupling agents, and panthenol are added. The mixture is stirred until homogeneous, and the pH is adjusted to 8-10. Polyquaternium-10 is added and stirred until homogeneous. Gallic acid microcapsules, ethyl cellulose-coated bisabolol, and modified graphene oxide are then added and stirred until homogeneous. Impurities are removed to obtain the hair dye.

[0009] Further, the dye intermediate is one or more of hydroxyethyl p-phenylenediamine sulfate, toluene-2,5-diamine sulfate, N,N-bis(2-hydroxyethyl) p-phenylenediamine sulfate, 2,4-diaminophenoxyethanol hydrochloride, and 4-amino-2-hydroxytoluene; the coupling agent is one or more of resorcinol, 2-amino-3-hydroxypyridine, p-aminophenol, m-aminophenol, and p-phenylenediamine.

[0010] Furthermore, the mass percentages of each component in the hair dye are as follows: 0.1-0.3% hydroxyethylidene diphosphate, 0.4-0.8% xanthan gum, 0.5-1.5% hydroxyethyl cellulose, 4-8% propylene glycol, 1-3% dye intermediate, 0.4-0.8% coupling agent, 0.5-1.5% panthenol, 1-2% polyquaternium-10, 0.5-1.5% gallic acid microcapsules, 0.3-0.5% hydroxyethyl cellulose-coated bisabolol, 0.01-0.03% modified graphene oxide, and the remainder is deionized water.

[0011] Furthermore, the preparation method of the gallic acid microcapsules is as follows: hydroxypropyl-β-cyclodextrin is dissolved in deionized water, magnetically stirred, gallic acid is added, ultrasonically mixed, purified, and freeze-dried to obtain gallic acid microcapsules.

[0012] Furthermore, in the preparation process of the gallic acid microcapsules, the mass ratio of hydroxypropyl-β-cyclodextrin to gallic acid is (6-8):1.

[0013] Further, the preparation method of the ethyl cellulose coated bisabolol is as follows: ethyl cellulose is added to anhydrous ethanol, ultrasonically mixed, sprayed, and vacuum dried to obtain a coating material. Then, bisabolol nanocapsules are placed in a container, preheated, and the coating material is sprayed to obtain ethyl cellulose coated bisabolol.

[0014] In the preparation process of the ethyl cellulose-coated bisabolol, the mass ratio of ethyl cellulose to bisabolol nanocapsules is (2-3):1.

[0015] Furthermore, the preparation method of the bisabolol nanocapsules is as follows: polyacrylic acid resin, sorbitan monooleate and bisabolol are dissolved in acetone to form an organic phase, Tween 80 is dissolved in deionized water, added to the organic phase, stirred and mixed, and then rotary evaporated to obtain bisabolol nanocapsules.

[0016] In the preparation process of the bisabolol nanocapsules, the mass ratio of polyacrylic acid resin, sorbitan monooleate, bisabolol and Tween 80 is 1:(0.05-0.15):(0.3-0.5):(0.1-0.3).

[0017] Furthermore, the modified graphene oxide is prepared as follows: graphene oxide is placed in deionized water, ultrasonically mixed, arginine is added, stirred in a water bath, washed and dried to obtain modified graphene oxide.

[0018] Furthermore, in the preparation process of the modified graphene, the mass ratio of graphene oxide to arginine is 1:(0.5-1.5).

[0019] Compared with the prior art, the beneficial effects of the present invention are:

[0020] 1. This invention introduces gallic acid microcapsules. Gallic acid is encapsulated with hydroxypropyl-β-cyclodextrin to improve its stability in hair dyes. During the dyeing process, on the one hand, it prevents the phenolic hydroxyl groups on gallic acid from being over-oxidized in an alkaline environment, maintaining the conjugation effect of the phenolic hydroxyl groups to donate electrons to the benzene ring, making the 2-position of the benzene ring the only highly active site. This facilitates the formation of an intermediate between the imine cation formed from the dye precursor and the active site at the 2-position of gallic acid, which then undergoes oxidative dehydrogenation in air to form a stable compound containing a double benzene ring and a carbon-nitrogen double bond, thus improving product stability. On the other hand, the carboxyl group of gallic acid can form ionic or hydrogen bonds with the amino groups on hair keratin, enhancing the color-fixing effect and thus improving the durability of gallic acid microcapsule hair dye. In addition, compared with the traditional coupling agent 1,2,4-phenylpyrogallol, naturally derived gallic acid significantly reduces sensitization, minimizes skin irritation, and improves the safety of hair dyes.

[0021] 2. This invention involves coating bisabolol. First, bisabolol is encapsulated with polyacrylic acid resin to form stable nanoparticles, which facilitates the spraying of a thin film with ethyl cellulose. Second, the ethyl cellulose film coating of the bisabolol nanocapsules effectively isolates alkaline substances in the hair dye, improving the chemical stability of the bisabolol nanocapsules during hair dye storage. During the hair dyeing process, due to friction and temperature changes, the ethyl cellulose coating ruptures, exposing the bisabolol nanocapsules. Under alkaline conditions, the polyacrylic acid resin gradually swells, releasing bisabolol, effectively alleviating the irritation of the hair dye to the scalp, reducing hair dyeing damage, and improving the mildness and smoothness of the hair dye.

[0022] 3. This invention introduces modified graphene oxide. By modifying the surface of graphene oxide with arginine, on the one hand, it prevents graphene oxide from agglomerating, improving its dispersibility and stability in hair dyes; on the other hand, during the dyeing process, the keratin in damaged hair carries a negative charge, while the arginine on the graphene oxide surface carries a positive charge. Therefore, the modified graphene oxide is adsorbed onto the damaged hair through electrostatic attraction, thereby improving the dyeing effect and durability of the hair dye. Simultaneously, the nanosheet structure of graphene oxide can form a dense film on the hair surface, improving the shine and smoothness of the hair, thus enhancing the smoothness of the hair dye. Furthermore, since arginine is a naturally occurring amino acid in the human body, its modification of graphene oxide not only reduces the skin irritation of graphene oxide, improving the gentleness and user experience of the hair dye, but also works synergistically with panthenol to moisturize during the dyeing process, increasing the softness and shine of the hair. Attached Figure Description

[0023] Figure 1 This invention relates to the hair dyeing effect of a smoothing black hair dye;

[0024] Figure 2 This invention relates to the hair dyeing effect of a smooth chestnut brown hair dye. Detailed Implementation

[0025] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0026] In the following examples, the CAS number for hydroxypropyl-β-cyclodextrin is 128446-35-5; the CAS number for gallic acid is 149-91-7; the CAS number for ethyl cellulose is 9004-57-3; the CAS number for bisabolol is 515-69-5; the CAS number for arginine is 74-79-3; the CAS number for hydroxyethylidene diphosphate is 2809-21-4; the CAS number for xanthan gum is 11138-66-2; the CAS number for hydroxyethyl cellulose is 9004-62-0; and the CAS number for toluene-2,5-diamine sulfate is 615. -50-9; N,N-bis(2-hydroxyethyl)-p-phenylenediamine sulfate CAS number 54381-16-7; 2,4-diaminophenoxyethanol hydrochloride CAS number 66422-95-5; panthenol CAS number 16485-10-2; monoethanolamine CAS number 141-43-5; polyquaternium-10 CAS number 68610-92-4; sorbitan monooleate CAS number 1338-43-8; Tween 80 CAS number 9005-65-6; polyacrylic acid resin model Eudragit RS100.

[0027] Example 1: A plant-based hair dye with softening properties and its preparation method: S1: Dissolve 6g of hydroxypropyl-β-cyclodextrin in deionized water, stir magnetically, add 1g of gallic acid, sonicate at 40℃ for 3h, purify, freeze dry, and obtain gallic acid microcapsules.

[0028] S2: Dissolve 1g of polyacrylic acid resin, 0.05g of sorbitan monooleate and 0.3g of bisabolol in acetone to form an organic phase. Dissolve 0.1g of Tween 80 in deionized water, add to the organic phase, stir and mix well, and then evaporate by rotary evaporation to obtain bisabolol nanocapsules.

[0029] S3: Add 2g of ethyl cellulose to anhydrous ethanol, mix ultrasonically, spray, and vacuum dry at 50℃ for 24h to obtain the coating material. Then place 1g of bisabolol nanocapsules in a container, preheat at 45℃ for 15min, and spray the coating material to obtain ethyl cellulose coated bisabolol.

[0030] S4: Place 1g of graphene oxide in deionized water, mix by ultrasonication, add 0.5g of arginine, stir in a 60℃ water bath for 30min, wash and dry to obtain modified graphene oxide.

[0031] S5: Place 0.1g hydroxyethylidene diphosphate, 0.4g xanthan gum, 0.5g hydroxyethyl cellulose and 4g propylene glycol in 91.39g deionized water, heat to 70℃, stir evenly, cool to 40℃, add 0.3g toluene-2,5-diamine sulfate, 0.3g N,N-bis(2-hydroxyethyl)-p-phenylenediamine sulfate, 0.3g 2,4-diaminophenoxyethanol hydrochloride, 0.2g resorcinol, 0.2g p-phenylenediamine and 0.5g panthenol, stir evenly, adjust the pH to 9 with monoethanolamine, add 1g polyquaternium-10, stir magnetically evenly, then add 0.5g gallic acid microcapsules, 0.3g ethyl cellulose-coated bisabolol and 0.01g modified graphene oxide, stir evenly, remove impurities to obtain hair dye.

[0032] Example 2: A plant-based hair dye with softening properties and its preparation method: S1: Dissolve 7g of hydroxypropyl-β-cyclodextrin in deionized water, stir magnetically, add 1g of gallic acid, sonicate at 40℃ for 3h, purify, freeze dry, and obtain gallic acid microcapsules.

[0033] S2: Dissolve 1g of polyacrylic acid resin, 0.05g of sorbitan monooleate and 0.3g of bisabolol in acetone to form an organic phase. Dissolve 0.1g of Tween 80 in deionized water, add to the organic phase, stir and mix well, and then evaporate by rotary evaporation to obtain bisabolol nanocapsules.

[0034] S3: Add 2g of ethyl cellulose to anhydrous ethanol, mix ultrasonically, spray, and vacuum dry at 50℃ for 24h to obtain the coating material. Then place 1g of bisabolol nanocapsules in a container, preheat at 45℃ for 15min, and spray the coating material to obtain ethyl cellulose coated bisabolol.

[0035] S4: Place 1g of graphene oxide in deionized water, mix by ultrasonication, add 0.5g of arginine, stir in a 60℃ water bath for 30min, wash and dry to obtain modified graphene oxide.

[0036] S5: Place 0.1g hydroxyethylidene diphosphate, 0.4g xanthan gum, 0.5g hydroxyethyl cellulose and 4g propylene glycol in 91.39g deionized water, heat to 70℃, stir evenly, cool to 40℃, add 0.3g toluene-2,5-diamine sulfate, 0.3g N,N-bis(2-hydroxyethyl)-p-phenylenediamine sulfate, 0.3g 2,4-diaminophenoxyethanol hydrochloride, 0.2g resorcinol, 0.2g p-phenylenediamine and 0.5g panthenol, stir evenly, adjust the pH to 9 with monoethanolamine, add 1g polyquaternium-10, stir magnetically evenly, then add 0.5g gallic acid microcapsules, 0.3g ethyl cellulose-coated bisabolol and 0.01g modified graphene oxide, stir evenly, remove impurities to obtain hair dye.

[0037] Example 3: A plant-based hair dye with softening properties and its preparation method: S1: Dissolve 8g of hydroxypropyl-β-cyclodextrin in deionized water, stir magnetically, add 1g of gallic acid, sonicate at 40℃ for 3h, purify, freeze dry, and obtain gallic acid microcapsules.

[0038] S2: Dissolve 1g of polyacrylic acid resin, 0.05g of sorbitan monooleate and 0.3g of bisabolol in acetone to form an organic phase. Dissolve 0.1g of Tween 80 in deionized water, add to the organic phase, stir and mix well, and then evaporate by rotary evaporation to obtain bisabolol nanocapsules.

[0039] S3: Add 2g of ethyl cellulose to anhydrous ethanol, mix ultrasonically, spray, and vacuum dry at 50℃ for 24h to obtain the coating material. Then place 1g of bisabolol nanocapsules in a container, preheat at 45℃ for 15min, and spray the coating material to obtain ethyl cellulose coated bisabolol.

[0040] S4: Place 1g of graphene oxide in deionized water, mix by ultrasonication, add 0.5g of arginine, stir in a 60℃ water bath for 30min, wash and dry to obtain modified graphene oxide.

[0041] S5: Place 0.1g hydroxyethylidene diphosphate, 0.4g xanthan gum, 0.5g hydroxyethyl cellulose and 4g propylene glycol in 91.39g deionized water, heat to 70℃, stir evenly, cool to 40℃, add 0.3g toluene-2,5-diamine sulfate, 0.3g N,N-bis(2-hydroxyethyl)-p-phenylenediamine sulfate, 0.3g 2,4-diaminophenoxyethanol hydrochloride, 0.2g resorcinol, 0.2g p-phenylenediamine and 0.5g panthenol, stir evenly, adjust the pH to 9 with monoethanolamine, add 1g polyquaternium-10, stir magnetically evenly, then add 0.5g gallic acid microcapsules, 0.3g ethyl cellulose-coated bisabolol and 0.01g modified graphene oxide, stir evenly, remove impurities to obtain hair dye.

[0042] Example 4: A plant-based hair dye with softening properties and its preparation method: S1: Dissolve 8g of hydroxypropyl-β-cyclodextrin in deionized water, stir magnetically, add 1g of gallic acid, sonicate at 40℃ for 3h, purify, freeze dry, and obtain gallic acid microcapsules.

[0043] S2: Dissolve 1g of polyacrylic acid resin, 0.1g of sorbitan monooleate and 0.4g of bisabolol in acetone to form an organic phase. Dissolve 0.2g of Tween 80 in deionized water, add to the organic phase, stir and mix well, and then evaporate by rotary evaporation to obtain bisabolol nanocapsules.

[0044] S3: Add 2g of ethyl cellulose to anhydrous ethanol, mix ultrasonically, spray, and vacuum dry at 50℃ for 24h to obtain the coating material. Then place 1g of bisabolol nanocapsules in a container, preheat at 45℃ for 15min, and spray the coating material to obtain ethyl cellulose coated bisabolol.

[0045] S4: Place 1g of graphene oxide in deionized water, mix by ultrasonication, add 0.5g of arginine, stir in a 60℃ water bath for 30min, wash and dry to obtain modified graphene oxide.

[0046] S5: Place 0.1g hydroxyethylidene diphosphate, 0.4g xanthan gum, 0.5g hydroxyethyl cellulose and 4g propylene glycol in 91.39g deionized water, heat to 70℃, stir evenly, cool to 40℃, add 0.3g toluene-2,5-diamine sulfate, 0.3g N,N-bis(2-hydroxyethyl)-p-phenylenediamine sulfate, 0.3g 2,4-diaminophenoxyethanol hydrochloride, 0.2g resorcinol, 0.2g p-phenylenediamine and 0.5g panthenol, stir evenly, adjust the pH to 9 with monoethanolamine, add 1g polyquaternium-10, stir magnetically evenly, then add 0.5g gallic acid microcapsules, 0.3g ethyl cellulose-coated bisabolol and 0.01g modified graphene oxide, stir evenly, remove impurities to obtain hair dye.

[0047] Example 5: A plant-based hair dye with softening properties and its preparation method: S1: Dissolve 8g of hydroxypropyl-β-cyclodextrin in deionized water, stir magnetically, add 1g of gallic acid, sonicate at 40℃ for 3h, purify, freeze dry, and obtain gallic acid microcapsules.

[0048] S2: Dissolve 1g of polyacrylic acid resin, 0.15g of sorbitan monooleate and 0.5g of bisabolol in acetone to form an organic phase. Dissolve 0.3g of Tween 80 in deionized water, add to the organic phase, stir and mix well, and then evaporate by rotary evaporation to obtain bisabolol nanocapsules.

[0049] S3: Add 3g of ethyl cellulose to anhydrous ethanol, mix ultrasonically, spray, and vacuum dry at 50℃ for 24h to obtain the coating material. Then place 1g of bisabolol nanocapsules in a container, preheat at 45℃ for 15min, and spray the coating material to obtain ethyl cellulose coated bisabolol.

[0050] S4: Place 1g of graphene oxide in deionized water, mix by ultrasonication, add 0.5g of arginine, stir in a 60℃ water bath for 30min, wash and dry to obtain modified graphene oxide.

[0051] S5: Place 0.1g hydroxyethylidene diphosphate, 0.4g xanthan gum, 0.5g hydroxyethyl cellulose and 4g propylene glycol in 91.39g deionized water, heat to 70℃, stir evenly, cool to 40℃, add 0.3g toluene-2,5-diamine sulfate, 0.3g N,N-bis(2-hydroxyethyl)-p-phenylenediamine sulfate, 0.3g 2,4-diaminophenoxyethanol hydrochloride, 0.2g resorcinol, 0.2g p-phenylenediamine and 0.5g panthenol, stir evenly, adjust the pH to 9 with monoethanolamine, add 1g polyquaternium-10, stir magnetically evenly, then add 0.5g gallic acid microcapsules, 0.3g ethyl cellulose-coated bisabolol and 0.01g modified graphene oxide, stir evenly, remove impurities to obtain hair dye.

[0052] Example 6: A plant-based hair dye with softening properties and its preparation method: S1: Dissolve 8g of hydroxypropyl-β-cyclodextrin in deionized water, stir magnetically, add 1g of gallic acid, sonicate at 40℃ for 3h, purify, freeze dry, and obtain gallic acid microcapsules.

[0053] S2: Dissolve 1g of polyacrylic acid resin, 0.15g of sorbitan monooleate and 0.5g of bisabolol in acetone to form an organic phase. Dissolve 0.3g of Tween 80 in deionized water, add to the organic phase, stir and mix well, and then evaporate by rotary evaporation to obtain bisabolol nanocapsules.

[0054] S3: Add 3g of ethyl cellulose to anhydrous ethanol, mix ultrasonically, spray, and vacuum dry at 50℃ for 24h to obtain the coating material. Then place 1g of bisabolol nanocapsules in a container, preheat at 45℃ for 15min, and spray the coating material to obtain ethyl cellulose coated bisabolol.

[0055] S4: Place 1g of graphene oxide in deionized water, mix by ultrasonication, add 1g of arginine, stir in a water bath at 60℃ for 30min, wash and dry to obtain modified graphene oxide.

[0056] S5: Place 0.2g hydroxyethylidene diphosphate, 0.6g xanthan gum, 1g hydroxyethyl cellulose and 6g propylene glycol in 85.88g deionized water, heat to 70℃, stir evenly, cool to 40℃, add 0.6g toluene-2,5-diamine sulfate, 0.6g N,N-bis(2-hydroxyethyl)-p-phenylenediamine sulfate, 0.6g 2,4-diaminophenoxyethanol hydrochloride, 0.3g resorcinol, 0.3g p-phenylenediamine and 1g panthenol, stir evenly, adjust the pH to 9 with monoethanolamine, add 1.5g polyquaternium-10, stir magnetically evenly, then add 1g gallic acid microcapsules, 0.4g ethyl cellulose-coated bisabolol and 0.02g modified graphene oxide, stir evenly, remove impurities to obtain hair dye.

[0057] Example 7: A plant-based hair dye with softening properties and its preparation method: S1: Dissolve 8g of hydroxypropyl-β-cyclodextrin in deionized water, stir magnetically, add 1g of gallic acid, sonicate at 40℃ for 3h, purify, freeze dry, and obtain gallic acid microcapsules.

[0058] S2: Dissolve 1g of polyacrylic acid resin, 0.15g of sorbitan monooleate and 0.5g of bisabolol in acetone to form an organic phase. Dissolve 0.3g of Tween 80 in deionized water, add to the organic phase, stir and mix well, and then evaporate by rotary evaporation to obtain bisabolol nanocapsules.

[0059] S3: Add 3g of ethyl cellulose to anhydrous ethanol, mix ultrasonically, spray, and vacuum dry at 50℃ for 24h to obtain the coating material. Then place 1g of bisabolol nanocapsules in a container, preheat at 45℃ for 15min, and spray the coating material to obtain ethyl cellulose coated bisabolol.

[0060] S4: Place 1g of graphene oxide in deionized water, mix by ultrasonication, add 1.5g of arginine, stir in a water bath at 60℃ for 30min, wash and dry to obtain modified graphene oxide.

[0061] S5: Place 0.3g hydroxyethylidene diphosphate, 0.8g xanthan gum, 1.5g hydroxyethyl cellulose and 8g propylene glycol in 80.07g deionized water, heat to 70℃, stir evenly, cool to 50℃, add 1g toluene-2,5-diamine sulfate, 1g N,N-bis(2-hydroxyethyl)-p-phenylenediamine sulfate, 1g 2,4-diaminophenoxyethanol hydrochloride, 0.4g resorcinol, 0.4g p-phenylenediamine and 1.5g panthenol, stir evenly, adjust the pH to 9 with monoethanolamine, add 2g polyquaternium-10, stir magnetically evenly, then add 1.5g gallic acid microcapsules, 0.5g ethyl cellulose-coated bisabolol and 0.03g modified graphene oxide, stir evenly, remove impurities to obtain hair dye.

[0062] Comparative Example 1: A plant-based hair dye with smoothing properties and its preparation method: S1: 1g of polyacrylic acid resin, 0.15g of sorbitan monooleate and 0.5g of bisabolol were dissolved in acetone to form an organic phase. 0.3g of Tween 80 was dissolved in deionized water and added to the organic phase. The mixture was stirred and mixed, and then evaporated by rotary evaporation to obtain bisabolol nanocapsules.

[0063] S2: Add 3g of ethyl cellulose to anhydrous ethanol, mix ultrasonically, spray, and vacuum dry at 50℃ for 24h to obtain the coating material. Then place 1g of bisabolol nanocapsules in a container, preheat at 45℃ for 15min, and spray the coating material to obtain ethyl cellulose coated bisabolol.

[0064] S3: Place 1g of graphene oxide in deionized water, mix by ultrasonication, add 1.5g of arginine, stir in a 60℃ water bath for 30min, wash and dry to obtain modified graphene oxide.

[0065] S4: Place 0.3g hydroxyethylidene diphosphate, 0.8g xanthan gum, 1.5g hydroxyethyl cellulose and 8g propylene glycol in 80.07g deionized water, heat to 70℃, stir evenly, cool to 50℃, add 1g toluene-2,5-diamine sulfate, 1g N,N-bis(2-hydroxyethyl)-p-phenylenediamine sulfate, 1g 2,4-diaminophenoxyethanol hydrochloride, 0.4g resorcinol, 0.4g p-phenylenediamine and 1.5g panthenol, stir evenly, adjust the pH to 9 with monoethanolamine, add 2g polyquaternium-10, stir magnetically evenly, then add 1.5g gallic acid, 0.5g ethyl cellulose-coated bisabolol and 0.03g modified graphene oxide, stir evenly, remove impurities to obtain hair dye.

[0066] Comparative Example 2: A plant-based hair dye with softening properties and its preparation method: S1: Dissolve 8g of hydroxypropyl-β-cyclodextrin in deionized water, stir magnetically, add 1g of gallic acid, sonicate at 40℃ for 3h, purify, freeze dry, and obtain gallic acid microcapsules.

[0067] S2: Place 1g of graphene oxide in deionized water, mix by ultrasonication, add 1.5g of arginine, stir in a water bath at 60℃ for 30min, wash and dry to obtain modified graphene oxide.

[0068] S3: Place 0.3g hydroxyethylidene diphosphate, 0.8g xanthan gum, 1.5g hydroxyethyl cellulose and 8g propylene glycol in 80.07g deionized water, heat to 70℃, stir evenly, cool to 50℃, add 1g toluene-2,5-diamine sulfate, 1g N,N-bis(2-hydroxyethyl)-p-phenylenediamine sulfate, 1g 2,4-diaminophenoxyethanol hydrochloride, 0.4g resorcinol, 0.4g p-phenylenediamine and 1.5g panthenol, stir evenly, adjust the pH to 9 with monoethanolamine, add 2g polyquaternium-10, stir magnetically evenly, then add 1.5g gallic acid microcapsules, 0.5g bisabolol and 0.03g modified graphene oxide, stir evenly, remove impurities to obtain hair dye.

[0069] Comparative Example 3: A plant-based hair dye with softening properties and its preparation method: S1: Dissolve 8g of hydroxypropyl-β-cyclodextrin in deionized water, stir magnetically, add 1g of gallic acid, sonicate at 40℃ for 3h, purify, freeze dry, and obtain gallic acid microcapsules.

[0070] S2: Dissolve 1g of polyacrylic acid resin, 0.15g of sorbitan monooleate and 0.5g of bisabolol in acetone to form an organic phase. Dissolve 0.3g of Tween 80 in deionized water, add to the organic phase, stir and mix well, and then evaporate by rotary evaporation to obtain bisabolol nanocapsules.

[0071] S3: Add 3g of ethyl cellulose to anhydrous ethanol, mix ultrasonically, spray, and vacuum dry at 50℃ for 24h to obtain the coating material. Then place 1g of bisabolol nanocapsules in a container, preheat at 45℃ for 15min, and spray the coating material to obtain ethyl cellulose coated bisabolol.

[0072] S4: Place 1g of graphene oxide in deionized water, mix by ultrasonication, add 1.5g of glutamic acid, stir in a water bath at 60℃ for 30min, wash and dry to obtain modified graphene oxide.

[0073] S5: Place 0.3g hydroxyethylidene diphosphate, 0.8g xanthan gum, 1.5g hydroxyethyl cellulose and 8g propylene glycol in 80.07g deionized water, heat to 70℃, stir evenly, cool to 50℃, add 1g toluene-2,5-diamine sulfate, 1g N,N-bis(2-hydroxyethyl)-p-phenylenediamine sulfate, 1g 2,4-diaminophenoxyethanol hydrochloride, 0.4g resorcinol, 0.4g p-phenylenediamine and 1.5g panthenol, stir evenly, adjust the pH to 9 with monoethanolamine, add 2g polyquaternium-10, stir magnetically evenly, then add 1.5g gallic acid microcapsules, 0.5g ethyl cellulose-coated bisabolol and 0.03g modified graphene oxide, stir evenly, remove impurities to obtain hair dye.

[0074] Testing: Take the hair dye samples prepared by the above examples and comparative examples, and test the color fastness to soap washing and color fastness to rubbing according to the methods of GB / T3921-2008 and GB / T29865-2013.

[0075] Table 1 Performance Test Data of Plant-Based Hair Dyes

[0076] Conclusion: By adjusting the proportions of each component of the hair dye, it was found to have good smoothness and coloring effect.

[0077] In Comparative Example 1, gallic acid was not microencapsulated with hydroxypropyl-β-cyclodextrin, which reduced the stability of gallic acid in the hair dye and thus affected the dyeing effect.

[0078] In Comparative Example 2, bisabolol was not coated. As an oil-soluble component, bisabolol exhibits uneven distribution in water-based hair dyes. Furthermore, bisabolol is unstable in the alkaline environment of hair dyes, reducing its anti-inflammatory and soothing biological activity, thereby decreasing the mildness and smoothness of the hair dye.

[0079] In Comparative Example 3, glutamic acid was used instead of arginine to modify graphene oxide. Glutamic acid carries a negative charge in an alkaline environment, and keratin also carries a negative charge after hair is damaged. This reduces the binding force between the modified graphene oxide and the hair, making it easier to wash off. This not only reduces the coloring effect and durability of the hair dye, but also makes it difficult for graphene oxide to form a film on the hair surface, thereby reducing the smoothness of the hair dye.

[0080] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above, and that the invention can be implemented in other specific forms without departing from its spirit or essential characteristics. Therefore, the embodiments should be considered in all respects as exemplary and non-limiting, and the scope of the invention is defined by the appended claims rather than the foregoing description. Thus, all variations falling within the meaning and scope of equivalents of the claims are intended to be included within the present invention. No reference numerals in the claims should be construed as limiting the scope of the claims.

Claims

1. A method of preparing a plant component hair dye having suppleness, characterized by: The method comprises the following steps: The hydroxyethylidene diphosphonic acid, xanthan gum, hydroxyethyl cellulose and propylene glycol are placed in deionized water, heated to 60-70 DEG C, stirred uniformly, cooled to 40-50 DEG C, dye intermediate, coupling agent and panthenol are added, stirred uniformly, the pH value is adjusted to 8-10, polyquaternary ammonium salt-10 is added, stirred uniformly, then gallic acid microcapsule, ethyl cellulose coated bisabolol and modified graphene oxide are added, stirred uniformly, impurities are removed, and a hair dye is obtained.

2. A method of preparing a plant component hair dye having flexibility according to claim 1, characterized by: The dye intermediate is one or more of hydroxyethyl p-phenylenediamine sulfate, toluene-2, 5-diamine sulfate, N, N-bis (2-hydroxyethyl) p-phenylenediamine sulfate, 2, 4-diaminophenoxy ethanol hydrochloride and 4-amino-2-hydroxytoluene; the coupling agent is one or more of m-dihydroxybenzene, 2-amino-3-hydroxypyridine, p-aminophenol, m-aminophenol and p-phenylenediamine.

3. A method of preparing a plant component hair dye having flexibility according to claim 1, characterized in that: The mass percentage of each component in the hair dye is: 0.1-0.3% hydroxyethylidene diphosphonic acid, 0.4-0.8% xanthan gum, 0.5-1.5% hydroxyethyl cellulose, 4-8% propylene glycol, 1-3% dye intermediate, 0.4-0.8% coupling agent, 0.5-1.5% panthenol, 1-2% polyquaternary ammonium salt-10, 0.5-1.5% gallic acid microcapsule, 0.3-0.5% hydroxyethyl cellulose coated bisabolol, 0.01-0.03% modified graphene oxide, and the rest is deionized water.

4. The method for preparing a plant-based hair dye with softening properties according to claim 1, characterized in that: The preparation method of the gallic acid microcapsule is as follows: hydroxypropyl-beta-cyclodextrin is dissolved in deionized water, magnetic stirring, adding gallic acid, ultrasonic mixing, purification, freeze-drying, and obtaining gallic acid microcapsule.

5. The method for preparing a plant-based hair dye with softening properties according to claim 4, characterized in that: In the preparation process of the gallic acid microcapsule, the mass ratio of hydroxypropyl-beta-cyclodextrin to gallic acid is (6-8):

1.

6. A method of preparing a plant component hair dye having flexibility according to claim 1, characterized by: The preparation method of the ethyl cellulose coated bisabolol is as follows: ethyl cellulose is added to anhydrous ethanol, ultrasonic mixing, spraying, vacuum drying, obtaining coating material, then bisabolol nanocapsule is placed in a container, preheating, spraying coating material, and obtaining ethyl cellulose coated bisabolol. In the preparation process of the ethyl cellulose coated bisabolol, the mass ratio of ethyl cellulose to bisabolol nanocapsule is (2-3):

1.

7. A method of preparing a plant component hair dye having flexibility according to claim 6, characterized by: The preparation method of the bisabolol nanocapsule is as follows: polyacrylic acid resin, sorbitan monooleate and bisabolol are dissolved in acetone to form an organic phase, Tween 80 is dissolved in deionized water, the organic phase is added, stirred uniformly, and rotary evaporation is performed to obtain bisabolol nanocapsule. In the preparation process of the bisabolol nanocapsule, the mass ratio of polyacrylic acid resin, sorbitan monooleate, bisabolol and Tween 80 is 1:(0.05-0.15):(0.3-0.5):(0.1-0.3).

8. The method for preparing a plant-based hair dye with softening properties according to claim 1, characterized in that: The preparation method of the modified graphene oxide is as follows: graphene oxide is placed in deionized water, ultrasonic mixing, adding arginine, water bath stirring, washing and drying to obtain modified graphene oxide.

9. A method of preparing a plant component hair dye having flexibility according to claim 8, characterized by: In the preparation process of the modified graphene, the mass ratio of graphene oxide to arginine is 1:(0.5-1.5).

10. A plant-derived hair dye prepared by the process according to any one of claims 1 to 9.

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