A Ti3C2T x Preparation method of hair dye and dyeing method

By using the method of combining modified Ti3C2Tx with film forming agents and antioxidants, a safe, low-toxic and superior hair dye is prepared, which solves the problems of strong irritation, long hair dyeing time and carcinogenic risk of existing hair dye products, and achieves uniform coating and long-term hair care effects.

CN118615172BActive Publication Date: 2025-04-25GUANGDONG PHARMA UNIV
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Patent Information

Application Number
CN202410834207.2
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-06-26
Publication Date
2025-04-25
Estimated Expiration
2044-06-26

AI Technical Summary

Technical Problem

Existing hair dye products have problems such as strong irritation, long hair dyeing time, damage to hair quality and carcinogenic risks, making it difficult to meet the needs of safety, low toxicity and superior performance.

Method used

Ti3C2Tx is used as hair dye, and the Ti3C2Tx dispersion is formed by selective etching and surface modification is carried out to bring an amino or carboxylic functional group. Then, a film-forming agent and an antioxidant are combined to prepare a hair dye that is sprayable liquid formula.

Benefits of technology

A uniform coating is achieved, and the stability and color depth of the hair dye are enhanced, which significantly improves the antistatic, antioxidant ability and physical strength of the hair, while ensuring the non-toxic and low-irritating properties of the hair dyeing process.

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Abstract

The invention discloses a Ti3C2T x A preparation method and a dyeing method for a hair dye, the preparation method comprising: x Modification treatment was performed to obtain modified Ti3C2T x , making the Ti3C2T x The hair dye preparation method adopted by the present invention is simple, fast and safe, and the sprayable liquid formula can be made to achieve simple and fast hair dyeing. x After modification, a hair dye with good dispersion uniformity is obtained, which can be tightly combined with hair keratin to achieve uniform coating. At the same time, the hair dye has good biocompatibility, and other raw materials used are safe, non-toxic and environmentally friendly, so that the prepared hair dye can be safely used on hair.
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Description

Technical Field

[0001] The present invention relates to the technical field of daily chemical products, and in particular to a Ti 3 C 2 T x The invention relates to a preparation method of a hair dye and a dyeing method. Background Art

[0002] Hair dyeing is a widely adopted beauty method that enhances the beauty of personal image through color change. It is extremely popular in contemporary society. Especially driven by the global aging population trend, the demand for dark and black hair dyes is increasing. The essence of hair color comes from the presence and content of melanin, which is gradually lost with age, resulting in the appearance of gray hair.

[0003] Currently, hair dye products generally have problems such as strong irritation, long dyeing time, and damage to hair. Traditional permanent hair dyeing technology uses an alkaline environment to allow paraphenylenediamine to penetrate and oxidatively polymerize and color, causing damage to the hair cuticle and the risk of skin allergies and cancer. For example, a 2020 study in the British Medical Journal showed that frequent use of paraphenylenediamine is associated with an increased risk of specific cancers, especially basal cell carcinoma of the skin and specific subtypes of breast cancer (especially estrogen receptor-negative and progesterone receptor-negative cases). In view of this, it is particularly urgent to develop a new hair dye that is both safe and low-toxic.

[0004] In view of the above limitations, there is an urgent need to develop a safe, low-toxic, cost-effective and superior alternative. 3 C 2 T x MXene (hereinafter referred to as Ti 3 C 2 T x ) is an advanced material with a two-dimensional planar structure that combines excellent electrical conductivity, thermal conductivity, oxidation resistance and high mechanical strength. Its natural dark black color, hydrophilic properties and excellent film-forming durability bring an innovative, safe and efficient solution to the hair dyeing field. 3 C 2 T x Multifunctional hair dyes can form a strong and durable covering layer, significantly improving the antistatic, antioxidant, heat dissipation and physical strength of hair. At the same time, based on its water-based formula, it ensures the non-toxic and low-irritation characteristics of the hair dyeing process, precisely catering to the dual concerns of modern society for personal health and environmental protection. 3 C 2 T x The development of multifunctional hair dyes is not only a breakthrough in the safety and functionality of hair dyeing technology, but also marks an important step towards building a healthier and more sustainable hair dyeing industry system.3 C 2 T x There are dispersion problems when using it for hair dyeing, and it cannot be stably and evenly combined with the hair. Therefore, it is necessary to explore Ti 3 C 2 T x The invention relates to a method for preparing a hair dye which is stable, uniform and has good performance. Summary of the invention

[0005] The purpose of the present invention is to provide a Ti 3 C 2 T x The invention discloses a method for preparing a hair dye and a dyeing method. The method adopted by the invention is simple and fast, and a sprayable liquid formula is prepared, so that simple and fast dyeing can be achieved.

[0006] The embodiment of the present invention provides a Ti 3 C 2 T x A method for preparing a hair dye, wherein the hair dye comprises at least Ti 3 C 2 T x , including the following steps:

[0007] S1、Ti 3 C 2 T x Dispersion Synthesis: Ti 3 AlC 2 Selective etching is performed to form Ti 3 C 2 T x Dispersion, Ti 3 C 2 T x The surface is capped with mixed functional groups of -F, -O and -OH;

[0008] S2. For Ti 3 C 2 T x Modification treatment is performed to obtain modified Ti 3 C 2 T x , so that the Ti 3 C 2 T x End-capped with amino or carboxyl functional groups;

[0009] S3, preparation of hair dye base liquid: select a certain amount of pH adjuster and dissolve it in an appropriate amount of solvent, heat to dissolve, then add antioxidant and film-forming agent in a preset proportion under continuous stirring, and mix thoroughly;

[0010] S4、Ti 3 C 2 Tx Preparation of hair dye: Maintain heating conditions to allow the hair dye base liquid to react stably for a long time, then add the modified Ti 3 C 2 T x , through ultrasonic treatment, Ti 3 C 2 T x Hair dye.

[0011] Optionally, the hair dye base liquid and the Ti 3 C 2 T x When preparing the hair dye, the heating temperature is 30 to 80°C; the hair dye base liquid and the Ti 3 C 2 T x The pH of hair dye is 3-9.

[0012] Optionally, the hair dye contains 0.1wt% to 3.0wt% Ti 3 C 2 T x ; 0.01wt% to 0.1wt% of film-forming agent; 93.8wt% to 99.87wt% of solvent; 0.01wt% to 0.1wt% of pH adjusting agent; 0.01wt% to 3wt% of antioxidant.

[0013] Optionally, the film-forming agent includes at least one of chitosan, hyaluronic acid, oxidized hyaluronic acid, polyquaternium-7, polyquaternium-10, polydimethylsiloxane, cyclopentasiloxane, trimethylsiloxysilicate and acrylate copolymer.

[0014] Optionally, the solvent includes at least one of water, ethanol, isopropanol, benzyl alcohol, acetone, ethyl acetate, and ethylene glycol monoethyl ether.

[0015] Optionally, the pH adjuster includes at least one of acetic acid, citric acid, lactic acid, ammonium acetate, sodium hexametaphosphate, sodium dihydrogen phosphate, disodium hydrogen phosphate, L-ascorbic acid, oxalic acid, tartaric acid, and gallic acid.

[0016] Optionally, the antioxidant is at least one of L-ascorbic acid, sodium isoascorbate, tea polyphenols, oxalic acid, tocopherol, gallic acid, propyl gallate, lipoic acid, butylated p-hydroxyanisole, butylated hydroxytoluene and tert-butylhydroquinone.

[0017] Another embodiment of the present invention provides a Ti 3 C 2 T x Hair dyeing method using hair dye, the Ti 3 C2 T x The hair dye is prepared by any of the above-mentioned preparation methods.

[0018] Optional, Ti 3 C 2 T x The hair dyeing method of the hair dye comprises the steps of: 3 C 2 T x Spray the hair dye on your hair, apply it evenly, comb it, and then heat and dry it.

[0019] Optionally, the heating temperature is 40 to 80° C.; the heating time is 5 to 30 minutes.

[0020] The beneficial effects of the present invention are:

[0021] (1) Innovative material application: The present invention uses advanced Ti 3 C 2 T x After modification, the high specific surface area and rich surface functional groups of two-dimensional nanomaterials can be tightly combined with hair keratin, which not only achieves uniform coating but also enhances the stability and coloring depth of hair dyes.

[0022] (2) Rapid dyeing process: Ti prepared by the present invention 3 C 2 T x The hair dye is a sprayable liquid formula, which is very convenient to use and can significantly shorten the time required for hair dyeing. Users can complete hair dyeing in about 5 to 30 minutes. The specific time varies depending on the hair quality and the desired depth of black.

[0023] (3) Multifunctional hair care performance: Ti 3 C 2 T x Through its excellent electrical and thermal conductivity, it gives dyed hair excellent anti-static and heat dissipation capabilities, creating a healthier and more comfortable scalp environment. Because of the moisturizing properties of the film-forming agent, it will synergistically enhance the hair's moisturizing and anti-static capabilities and reduce static electricity accumulation.

[0024] (4) Enhance physical strength: through Ti 3 C 2 T x The surface modification can cooperate with the film-forming agent to form a protective film to strengthen the physical barrier of the hair, reduce external damage, enhance the tensile strength and toughness of the hair, reduce breakage, and improve the overall health of the hair.

[0025] (5) The preparation method is simple and safe: 3 C 2 T xThe surface of the hair dye is modified to obtain a hair dye with good dispersion uniformity. The prepared hair dye can be directly applied to the hair for dyeing. At the same time, the hair dye has good biocompatibility, and other raw materials used are safe, non-toxic and environmentally friendly, so that the prepared hair dye can be safely used on the hair. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] The accompanying drawings are used to provide a further understanding of the present invention and constitute a part of the specification. Together with the embodiments of the present invention, they are used to explain the present invention and do not constitute a limitation of the present invention. In the accompanying drawings:

[0027] Figure 1 is a Ti according to one embodiment of the present invention 3 C 2 T x A method for preparing a hair dye.

[0028] Figure 2 is Ti prepared according to one embodiment of the present invention 3 C 2 T x XRD pattern of .

[0029] Figure 3 is Ti prepared according to one embodiment of the present invention 3 C 2 T x SEM image of . DETAILED DESCRIPTION

[0030] The present invention will now be further described in detail with reference to the accompanying drawings, but it should be understood that the protection scope of the present invention is not limited by the specific embodiments.

[0031] like Figure 1 As shown, a Ti according to a specific embodiment of the present invention 3 C 2 T x A method for preparing a hair dye, wherein the hair dye comprises at least Ti 3 C 2 T x , including the following steps:

[0032] S1、Ti 3 C 2 T x Dispersion Synthesis: Ti 3 AlC 2 Selective etching is performed to form Ti 3 C 2 T x Dispersion, Ti 3 C 2 T x The surface is capped with mixed functional groups of -F, -O and -OH;

[0033] S2. For Ti 3 C 2 T x Modification treatment is performed to obtain modified Ti 3 C 2 T x , so that the Ti 3 C 2 T x End-capped with amino or carboxyl functional groups;

[0034] S3, preparation of hair dye base liquid: select a certain amount of pH adjuster and dissolve it in an appropriate amount of solvent, heat to dissolve, then add antioxidant and film-forming agent in a preset proportion under continuous stirring, and mix thoroughly;

[0035] S4、Ti 3 C 2 T x Preparation of hair dye: Maintain heating conditions to allow the hair dye base liquid to react stably for a long time, then add the modified Ti 3 C 2 T x , through ultrasonic treatment, Ti 3 C 2 T x Hair dye.

[0036] The present invention is to Ti 3 C 2 T x Modification treatment is carried out to make Ti 3 C 2 T x The surface contains abundant hydrophilic groups such as amino, carboxyl, hydroxyl, and fluorine, which can form strong chemical bonds with the amino and carboxyl groups on the surface of hair keratin, thereby using Ti 3 C 2 T x As a hair dye, it can closely bind to the hair keratin to achieve uniform coverage.

[0037] In some specific embodiments, the above step S1 includes the following steps:

[0038] Lithium fluoride (LiF) and hydrochloric acid (HCl) were stirred in a covered polytetrafluoroethylene beaker, and then Ti 3 AlC 2 -MAX was slowly added into the beaker, the reaction temperature was adjusted to 40°C, and stirring was continued for 24 hours; after the reaction was completed, the reaction solution was centrifuged to discard the supernatant, and washed with deionized water, and the process was repeated several times until the pH value of the supernatant was about 6, deionized water was added, ultrasonicated in an ice water bath, and the upper dispersion was collected by centrifugation to obtain Ti 3 C2 T x Dispersion.

[0039] It should be noted that MXene is usually synthesized from the corresponding MAX phase, where M represents a transition metal element (such as Ti, Nb, Mo, V, W, etc.), A represents a main group element, and X represents C or N. HF is used to selectively etch the main group element so that MXene is terminated with a mixture of F, O, and OH functional groups, usually expressed as T x .

[0040] In some specific embodiments, the above step S2 includes the following steps:

[0041] Ti 3 C 2 T x The dispersion was added to a solution containing ammonia water and stirred for 12 hours to make Ti 3 C 2 T x Surface functionalization to form Ti 3 C 2 T x -NH 2 .

[0042] In some other specific embodiments, the above step S2 includes the following steps:

[0043] Add an appropriate amount of NaOH and p-aminobenzoic acid to the water, keep the temperature between 0 and 5°C, and slowly add an appropriate amount of sodium nitrite to the solution. Subsequently, quickly add an excess of hydrochloric acid solution (6M / L) to the solution and stir for 45 minutes. Then, add it to the MXene colloid solution and stir at 1000r / min for 4 hours. After the reaction time is over, the solution is ultrasonically treated for 15 minutes and centrifuged at 9000r / min for 30 minutes. After pouring the upper liquid, wash with water, acetone and ethanol in turn to remove salt (5 minutes each time, 9000r / min) to obtain Ti 3 C 2 T x -COOH. Finally, the product is stored in oxygen-free water.

[0044] Furthermore, the hair dye base liquid and the Ti 3 C 2 T x When preparing the hair dye, the heating temperature is 30 to 80°C; the hair dye base liquid and the Ti 3 C 2 T x The pH of hair dye is 3-9.

[0045] Furthermore, if Figure 1As shown, the hair dye comprises, by mass percentage: 0.1wt% to 3.0wt% of Ti 3 C 2 T x ; 0.01wt% to 0.1wt% of film-forming agent; 93.8wt% to 99.87wt% of solvent; 0.01wt% to 0.1wt% of pH adjusting agent; 0.01wt% to 3wt% of antioxidant.

[0046] Ti 3 C 2 T x Within this mass percentage range, a good coloring effect can be shown. 3 C 2 T x Contains rich hydrophilic groups, based on Ti 3 C 2 T x The hair dye can be prepared without potentially toxic chemical additives, overcoming the limitations of traditional dyes and achieving comfort in hair dyeing. Its high specific surface area and rich surface functional groups can tightly combine with hair keratin, not only achieving uniform coating but also enhancing the stability and coloring depth of the hair dye.

[0047] Furthermore, the film-forming agent includes at least one of chitosan, hyaluronic acid, oxidized hyaluronic acid, polyquaternium-7, polyquaternium-10, polydimethylsiloxane, cyclopentasiloxane, trimethylsiloxysilicate and acrylate copolymer.

[0048] Chitosan, hyaluronic acid, oxidized hyaluronic acid, etc. are used as film-forming agents to 3 C 2 T x The rich groups on the surface interact with each other through hydrogen bonds, which have high surface adhesion and adhere to the hair surface during the coating process, making it resistant to washing. In addition, in the film-forming agent, such as chitosan molecules, the amino groups in the molecules become cations under acidic conditions, while the hair surface becomes anions under the same conditions. Chitosan is adsorbed on the hair surface through ionic interactions, so the addition of film-forming agents can enhance the color fastness of hair dyes to washing. Film-forming agents also have a moisturizing effect, and Ti 3 C 2 T x They work together on the hair to achieve the dyeing effect while also moisturizing the hair to achieve a maintenance effect.

[0049] Furthermore, the solvent includes at least one of water, ethanol, isopropanol, benzyl alcohol, acetone, ethyl acetate, and ethylene glycol monoethyl ether.

[0050] Ti 3 C2 T x The two-dimensional geometry and high surface area provide excellent film forming properties. 3 C 2 T x Hair dyes can be formulated in water without harmful ingredients or other harmful solvents, thus achieving the safety of hair dyeing technology.

[0051] Furthermore, the pH adjuster includes at least one of acetic acid, citric acid, lactic acid, ammonium acetate, sodium hexametaphosphate, sodium dihydrogen phosphate, disodium hydrogen phosphate, L-ascorbic acid, oxalic acid, tartaric acid, and gallic acid.

[0052] The pH regulator can adjust the acid-base environment of the hair dye, so that the hair dye can be more firmly combined with the hair during the action process. The pH regulator is preferably mild, environmentally friendly, and non-toxic to ensure the safety of the hair dye.

[0053] Furthermore, the antioxidant is selected from at least one of L-ascorbic acid, sodium isoascorbate, tea polyphenols, oxalic acid, tocopherol, gallic acid, propyl gallate, lipoic acid, butylated p-hydroxyanisole, butylated hydroxytoluene and tert-butylhydroquinone.

[0054] The antioxidant can improve the stability of the hair dye, thereby achieving the durability of the hair dye.

[0055] According to a specific embodiment of the present invention, a Ti 3 C 2 T x Hair dyeing method using hair dye, the Ti 3 C 2 T x The hair dye is prepared by any of the above-mentioned preparation methods.

[0056] Further, a Ti according to a specific embodiment of the present invention 3 C 2 T x A hair dyeing method comprising the steps of: 3 C 2 T x Spray the hair dye on your hair, apply it evenly, comb it, and then heat and dry it.

[0057] Furthermore, the hair dyeing heating temperature is 40 to 80° C.; the heating time is 5 to 30 minutes.

[0058] Understandably, when dyeing hair, use Ti 3 C 2 T x Hair dye can quickly achieve color in just 5 to 30 minutes, greatly shortening the time required for hair dyeing.

[0059] The following is a more detailed description of a Ti of the present invention by way of specific embodiments. 3 C 2 T x Regarding the application in hair dye, it should be understood that the present invention is not limited thereto.

[0060] Comparative Example:

[0061] 1. Ti 3 C 2 T x Preparation:

[0062] 1 g of lithium fluoride (LiF) and 40 mL of 9 M hydrochloric acid (HCl) were stirred in a covered polytetrafluoroethylene beaker for 30 min. 3 AlC 2 Slowly add it to the above beaker, adjust the reaction temperature to 40°C, and continue stirring for 24 hours; after the reaction is completed, centrifuge the reaction solution (3500rpm, 5min), discard the supernatant, wash with deionized water, repeat several times until the pH value of the supernatant is about 6, add deionized water, ultrasonicate in an ice water bath for 10-20min, centrifuge (3500rpm, 10min) to collect the upper dispersion, and obtain Ti 3 C 2 T x Dispersion.

[0063] The Ti prepared in this example 3 C 2 T x , its XRD is as follows Figure 2 As shown, the characteristic peak (002) is located at 6.78°, which not only confirms that Ti 3 C 2 T x The typical crystal phase of the material can effectively eliminate the possibility of residual MAX phase or other impurities in the synthesis process, ensuring the purity of the material.

[0064] Ti 3 C 2 T x SEM Figure 3 As shown, the two-dimensional layered structural characteristics of the material are clearly displayed, where the lateral size of a single sheet ranges from approximately 1 to 4.6 μm. This morphological feature helps it form a uniform covering layer on the hair, which is crucial for its application as a hair dye.

[0065] 2. Preparation of chitosan solution:

[0066] Take 20 mg of L-ascorbic acid and add it to a 50 mL round-bottom flask. Add 10 mL of distilled water. Place the container containing the L-ascorbic acid solution on a magnetic stirrer at 70 °C. ℃ Heat and stir. Then, add 20 mg of chitosan to the solution. Continue heating and stirring the mixture at a speed of 600 r / min for about 12 hours to obtain a chitosan aqueous solution.

[0067] 3. Ti 3 C 2 T x Preparation of hair dye:

[0068] 100 mg Ti was added to the obtained chitosan aqueous solution. 3 C 2 T x Then, in an ice-water bath, under nitrogen protection, the mixed solution was ultrasonically treated for 30 min using an ultrasonic disperser to obtain a stable Ti 3 C 2 T x Hair dye, Ti 3 C 2 T x The concentration in hair dye is 10 mg / mL.

[0069] 4. Hair dyeing method:

[0070] Ti 3 C 2 T x Transfer the hair dye to a 20mL spray bottle, spray the dye on the hair, apply it evenly, comb it, and then dry it at 50℃ for 20 minutes.

[0071] Example 1

[0072] In this embodiment, a Ti-based 3 C 2 T x -NH 2 The hair dye uses oxalic acid as a pH regulator, aiming to further optimize the mildness and environmental friendliness of the hair dyeing process.

[0073] 1. Ti 3 C 2 T x -NH 2 Preparation:

[0074] Take 1g of Ti 3 AlC 2 The material was added to a polytetrafluoroethylene beaker containing 1 g lithium fluoride (LiF) and 40 mL 9 M hydrochloric acid (HCl). After stirring for 30 min, the temperature was adjusted to 40 ℃, stirring continuously for 24 hours to carry out etching reaction. After the reaction is completed, centrifuge (3500rpm, 5min), discard the supernatant, and wash repeatedly with deionized water until the pH value of the supernatant is close to 6. Ultrasonic treatment in an ice water bath for 10 to 20 minutes, centrifuge again (3500rpm, 10min), collect the upper dispersion, which is Ti 3 C 2 T x Dispersion. 3 C 2 T x The dispersion was added to a solution containing ammonia water and stirred for 12 hours to make Ti 3 C 2 T x Surface functionalization to form Ti 3 C 2 T x -NH 2 .

[0075] 2. Preparation of hair dye base liquid:

[0076] Dissolve 20 mg of chitosan in 5 mL of oxalic acid solution containing 10 mg, and heat and stir at 30-80° C. until the chitosan is completely dissolved.

[0077] 3. Ti 3 C 2 T x -NH 2 Preparation of hair dye:

[0078] 100 mg Ti prepared above 3 C 2 T x -NH 2 Add to chitosan solution and treat with ultrasound for 30 min to ensure Ti 3 C 2 T x -NH 2 Evenly dispersed in chitosan solution, Ti 3 C 2 T x -NH 2 Solution. Slowly add 5 mL of 10 mg / mL oxalic acid solution to the Ti 3 C 2 T x -NH 2 The solution was stirred for 60 min to obtain Ti 3 C 2 T x -NH 2 Hair dye.

[0079] 4. Hair dyeing method:

[0080] Ti 3 C 2 T x -NH 2 Transfer the hair dye to a 20mL spray bottle, spray the dye on the hair, apply it evenly, comb it, and then dry it at 50℃ for 20 minutes.

[0081] Example 2

[0082] In this embodiment, a Ti-based 3 C 2 T x -COOH-containing hair dye uses L-ascorbic acid as a pH regulator, aiming to further optimize the mildness and environmental friendliness of the hair dyeing process.

[0083] 1. Ti 3 C 2 T x Preparation of -COOH:

[0084] (1) Take 1g of Ti 3 AlC 2 The material was added to a polytetrafluoroethylene beaker containing 1g lithium fluoride (LiF) and 40mL 9M hydrochloric acid (HCl). After stirring for 30min, the temperature was adjusted to 40°C and stirring was continued for 24h to carry out the etching reaction. After the reaction was completed, centrifuged (3500rpm, 5min), the supernatant was discarded, and the supernatant was repeatedly washed with deionized water until the pH value of the supernatant was close to 6. Ultrasonic treatment was performed in an ice water bath for 10 to 20min, and centrifuged again (3500rpm, 10min), and the upper dispersion was collected, which was Ti 3 C 2 T x Dispersion.

[0085] (2) Add 280 mg of NaOH and 960 mg of p-aminobenzoic acid to 80 ml of water. Then, keep the temperature between 0 and 5 °C and slowly add 526 mg of sodium nitrite to the solution. Finally, quickly add 6 mL of hydrochloric acid solution (6 M / L) to the solution and stir for 45 minutes. Next, add 40 mL of Ti 3 C 2 T x The colloid solution (5 mg / ml) was stirred at 1000 r / min for 4 h. After the reaction time was over, the solution was subjected to ultrasonic treatment for 15 min and centrifuged at 9000 r / min for 30 min. After the upper layer was poured, it was washed with water, acetone and ethanol in sequence to remove salt (5 min each time, 9000 r / min). Finally, the product was stored in oxygen-free water.

[0086] 2. Preparation of hair dye base liquid:

[0087] 20 mg of chitosan was dissolved in 5 mL of a solution containing 10 mg of L-ascorbic acid, and the mixture was heated and stirred at 30 to 80° C. until the chitosan was completely dissolved.

[0088] 3. Ti 3 C 2 T x Preparation of -COOH hair dye:

[0089] 100 mg Ti prepared above 3 C 2 T x -COOH was added to the chitosan solution and treated with ultrasound for 30 min to ensure that Ti 3 C 2 T x -COOH is evenly dispersed in the chitosan solution to obtain Ti 3 C 2 T x -COOH solution. 5 mL of 10 mg / mL L-ascorbic acid solution was slowly added dropwise to the Ti 3 C 2 T x -COOH solution, stirring was maintained for 60 min to obtain Ti 3 C 2 T x -COOH hair dye.

[0090] 4. Hair dyeing method:

[0091] Ti 3 C 2 T x Transfer the -COOH hair dye to a 20mL spray bottle, spray the dye on the hair, apply it evenly, comb it, and then dry it at 50℃ for 20min.

[0092] Using Comparative Example 1, Ti of Examples 1 to 2 3 C 2 T x The hair dyes were used in hair dyeing experiments and all successfully achieved the transformation of hair color to a dark black tone, demonstrating good coloring effects.

[0093] The hair dye durability of the hair dye of the embodiment of the present invention was evaluated. The specific method is as follows: the dyed hair sample is completely immersed in a 50mL conical flask containing 40mL of 5% (v / v) shampoo, vortexed for 30 seconds each time, then rinsed with clean water and dried. This process is repeated 20 times to simulate the hair dye durability under long-term washing and care conditions. The brightness change is evaluated by comparing the average RGB values ​​of the hair samples before and after shampooing.

[0094] As shown in Table 1, the 10 mg / mL Ti 3 C 2 T x The average brightness of the hair sample after 20 washes of the hair dye only increased from the initial 11.8% to 17.5%. 3 C 2 T x The average brightness of the dyed hair was lower than that of the comparative example 1, indicating a good coloring effect. After 20 shampooings, the increase in brightness was smaller, proving that the modified Ti 3 C 2 T x Hair dye compared to unmodified Ti 3 C 2 T x Excellent durability of hair dye.

[0095] Table 1 Ti prepared in the embodiment of the present invention 3 C 2 T x Comparison of average brightness of hair after dyeing with hair dye

[0096] Comparative Example 1 Example 1 Example 2 Before shampooing 11.8% 10.4% 10.8% After 20 shampooings 17.5% 13.6% 15.2%

[0097] The electrostatic voltage of the hair samples after being combed 10 times with a plastic comb was tested using a surface DC voltmeter to evaluate the electrostatic accumulation under different treatment conditions. The results are shown in Table 2. The surface electrostatic voltage of the hair without any treatment after combing was as high as about 0.21 kV, while the hair with 10 mg / mL Ti 3 C 2 T x The surface electrostatic voltage of the hair sample with hair dye was significantly reduced to only 0.06 kV. 3 C 2 T x -NH 2 Hair dye and Ti of Example 2 3 C 2 T x -COOH hair dye, the surface electrostatic voltage of the hair samples was significantly reduced to only 0.06kV, 0.03kV, and 0.05kV, indicating that the hair dye effectively inhibited the accumulation of static electricity in the hair and improved the anti-static properties of the hair.

[0098] Table 2 Ti prepared in the present invention 3 C 2 T x Comparison of surface electrostatic voltage after hair dyeing

[0099] No treatment Comparative Example 1 Example 1 Example 2 After combing 10 times 0.21kV 0.06kV 0.03kV 0.05kV

[0100] The present invention uses advanced Ti 3 C 2 T x After modification, the high specific surface area and rich surface functional groups of two-dimensional nanomaterials can be tightly combined with hair keratin, which not only achieves uniform coating but also enhances the stability and coloring depth of hair dyes.

[0101] Ti prepared by the present invention 3 C 2 T x The hair dye is a sprayable liquid formula, which is very convenient to use and can significantly shorten the time required for hair dyeing. Users can complete hair dyeing in about 5 to 30 minutes. The specific time varies depending on the hair quality and the desired depth of black.

[0102] Ti 3 C 2 T x Through its excellent electrical and thermal conductivity, it gives dyed hair excellent anti-static and heat dissipation capabilities, creating a healthier and more comfortable scalp environment. Because of the moisturizing properties of the film-forming agent, it will enhance the hair's moisturizing and anti-static capabilities and reduce static electricity accumulation.

[0103] The present invention adopts Ti 3 C 2 T x The surface modification can cooperate with the film-forming agent to form a protective film to strengthen the physical barrier of the hair, reduce external damage, enhance the tensile strength and toughness of the hair, reduce breakage, and improve the overall health of the hair.

[0104] The present invention adopts Ti 3 C 2 T x The surface of the hair dye is modified to obtain a hair dye with good dispersion uniformity. The prepared hair dye can be directly applied to the hair for dyeing. At the same time, the hair dye has good biocompatibility, and other raw materials used are safe, non-toxic and environmentally friendly, so that the prepared hair dye can be safely used on the hair.

[0105] The above description is only a preferred specific implementation manner of the present invention, but the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can make equivalent replacements or changes according to the technical scheme and inventive concept of the present invention within the technical scope disclosed by the present invention, which should be covered by the protection scope of the present invention.

Claims

1. A Ti3C2T x A method for preparing a hair dye, wherein the hair dye comprises at least Ti3C2T x , characterized in that, The steps include: S1、Ti3C2T x Dispersion Synthesis: Selective etching of Ti3AlC2 to form Ti3C2T x Dispersion, Ti3C2T x The surface is capped with mixed functional groups of -F, -O and -OH; S2, Ti3C2T x Modification treatment was performed to obtain modified Ti3C2T x , making the Ti3C2T x End-capped with amino or carboxyl functional groups; wherein, Ti3C2T x The modification method comprises: x The dispersion was added into a solution containing aqueous ammonia and stirred to react to obtain modified Ti3C2T ... x Or, add an appropriate amount of sodium nitrite and hydrochloric acid solution to the solution of NaOH and p-aminobenzoic acid, and x The dispersion was stirred and dispersed in the above solution, and after ultrasonication, centrifugation and washing, the modified Ti3C2T ... x ; S3, preparation of hair dye base liquid: select a certain amount of pH adjuster and dissolve it in an appropriate amount of solvent, heat to dissolve, then add antioxidant and film-forming agent in a preset proportion under continuous stirring, and mix thoroughly; S4、Ti3C2T x Preparation of hair dye: Maintain heating conditions to allow the hair dye base liquid to react stably for a long time, and then add the modified Ti3C2T x , through ultrasonic treatment, Ti3C2T x Hair dye.

2. Ti3C2T according to claim 1 x A method for preparing a hair dye, characterized in that: The hair dye base liquid and the Ti3C2T x When preparing the hair dye, the heating temperature is 30-80°C; the hair dye base liquid and the Ti3C2T x The pH of hair dye is 3-9.

3. Ti3C2T according to claim 1 x A method for preparing a hair dye, characterized in that: In terms of mass percentage, the Ti3C2T x The hair dye contains: 0.1wt% to 3.0wt% Ti3C2T x ; 0.01wt% to 0.1wt% of film-forming agent; 93.8wt% to 99.87wt% of solvent; 0.01wt% to 0.1wt% of pH adjusting agent; 0.01wt% to 3wt% of antioxidant.

4. Ti3C2T according to claim 1 x A method for preparing a hair dye, characterized in that: The film-forming agent comprises at least one of chitosan, hyaluronic acid, oxidized hyaluronic acid, polyquaternium-7, polyquaternium-10, polydimethylsiloxane, cyclopentasiloxane, trimethylsiloxysilicic acid ester and acrylate copolymer.

5. Ti3C2T according to claim 1 x A method for preparing a hair dye, characterized in that: The solvent includes at least one of water, ethanol, isopropanol, benzyl alcohol, acetone, ethyl acetate, and ethylene glycol monoethyl ether.

6. The Ti3C2T3 according to claim 1 x A method for preparing a hair dye, characterized in that: The pH regulator includes at least one of acetic acid, citric acid, lactic acid, ammonium acetate, sodium hexametaphosphate, sodium dihydrogen phosphate, disodium hydrogen phosphate, L-ascorbic acid, oxalic acid, tartaric acid and gallic acid.

7. The Ti3C2T3 according to claim 1 x A method for preparing a hair dye, characterized in that: The antioxidant is selected from at least one of L-ascorbic acid, sodium isoascorbate, tea polyphenols, oxalic acid, tocopherol, gallic acid, propyl gallate, lipoic acid, tert-butyl-p-hydroxyanisole, butylated hydroxytoluene and tert-butylhydroquinone.

8. A Ti3C2T x A hair dyeing method using a hair dye, characterized in that: The Ti3C2T x The hair dye is prepared by the preparation method according to any one of claims 1 to 7.

9. The Ti3C2T3 according to claim 8 x A hair dyeing method using a hair dye, characterized in that: The steps include: x Spray the hair dye on your hair, apply it evenly, comb it, and then heat and dry it.

10. The Ti3C2T3 according to claim 9 x The hair dyeing method using a hair dye comprises the following steps: the heating temperature is 40 to 80° C.; and the heating time is 5 to 30 minutes.

Citation Information

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