Polypeptide silk dense moistening hair care mask and preparation method thereof

Abstract

The invention relates to a polypeptide silk dense moistening hair care mask and a preparation method thereof, and belongs to the technical field of daily chemicals. According to the hair care mask, acetyl hexapeptide-8 and a cationic surface active agent are subjected to a pre-compounding reaction under the weak acid condition, and a polypeptide-cationic compound is formed; and adding the oil phase into the water phase for emulsification, adding the compound and the hydrolyzed silk protein active matter, and finally carrying out a gradient cooling process. The obtained product integrates softening, repairing and long-acting nourishing, and is suitable for damaged hair.

Description

Technical Field

[0001] This invention belongs to the field of daily chemical products technology, and relates to a polypeptide silk intensive moisturizing hair mask and its preparation method. Background Technology

[0002] With rising living standards and changing aesthetic standards, people's demands for hair care are becoming increasingly refined and in-depth. Frequent perming, dyeing, and daily use of high-temperature styling tools can easily damage the hair cuticle, leading to the loss of internal protein and moisture, resulting in a series of problems such as dryness, frizz, brittleness, and decreased shine. Regular shampoos and conditioners mainly focus on cleansing and immediate surface smoothing. Their active ingredients have large molecular weights or are negatively charged, making it difficult for them to effectively penetrate into the hair shaft. They have limited ability to repair structural damage to the hair core, and their retention rate after rinsing is low, failing to provide long-lasting, deep nourishment and repair.

[0003] To enhance the repair efficacy of hair care products, existing technologies attempt to add various active ingredients to the formula, such as small molecule peptides, hydrolyzed proteins, amino acids, and plant extracts. For repairing damaged hair, the key lies in efficiently delivering active ingredients to the hair core and ensuring their long-lasting effect. However, effectively integrating these water-soluble, often negatively charged bioactive ingredients (such as hydrolyzed silk protein) into a hair care emulsification system centered on cationic conditioners presents significant technical challenges. Adverse electrostatic interactions may occur between the active ingredients and cationic surfactants, leading to formula instability, inactivation of active ingredients, or significant rinsing away during washing, making it difficult to achieve high-concentration, long-lasting targeted delivery to the hair strands.

[0004] In addition, traditional hair care products often use a process of high-temperature emulsification followed by rapid cooling during the preparation process. This method can easily lead to coarse crystals, uneven structure, and rough texture in the product paste, affecting the user experience and making it difficult to build a stable sustained-release system of active ingredients.

[0005] Therefore, how to design a new hair care product and its preparation method that can stably and efficiently load and deliver active repair ingredients such as peptides and silk proteins, and ensure that these ingredients can work on the hair strands for a long time, thereby achieving intensive moisturization and deep repair from the inside out, while the product itself has a delicate and stable paste texture, has become a technical problem that urgently needs to be solved in this field. Summary of the Invention

[0006] The purpose of this invention is to provide a polypeptide silk intensive moisturizing hair mask and its preparation method, which can effectively improve the stable loading and delivery efficiency of active ingredients.

[0007] The objective of this invention can be achieved through the following technical solutions: In a first aspect, the present invention provides a method for preparing a polypeptide silk intensive moisturizing hair mask, comprising the following steps: (1) Acetyl hexapeptide-8 was reacted with a cationic surfactant at pH 4.0-4.8 and temperature 30-45℃ to form a polypeptide-cationic complex; (2) Heat and mix the aqueous phase components; (3) Heat and mix the oil phase components, wherein the oil phase components include fatty alcohols and silicone oil; (4) Add the oil phase to the aqueous phase for emulsification and cool to 40-50℃; (5) Add the polypeptide-cationic complex and hydrolyzed silk protein active ingredients obtained in step (1) to the emulsion matrix of step (4) and mix evenly; (6) The mixture is subjected to gradient cooling to obtain the hair care film.

[0008] As used herein, the term "cationic surfactant" refers to compounds suitable for use in personal care products that dissociate into positively charged surfactant ions in aqueous solutions. In this invention, it particularly refers to quaternary ammonium salt surfactants that can form stable complexes with acetyl hexapeptide-8 under weakly acidic conditions and are used for hair conditioning, including but not limited to cetrimonium chloride and behenyltrimethylammonium methyl sulfate. A preferred formulation is a combination of cetrimonium chloride and behenyltrimethylammonium methyl sulfate.

[0009] As used in this text, "hydrolyzed silk protein active ingredients" refers to a general term for a class of water-soluble silk protein derivatives obtained through the hydrolysis and degradation of silk protein. They have a wide molecular weight range and are intended for use in repairing hair keratin. They include, but are not limited to: Hydrolyzed silk: usually refers to hydrolyzed fragments of silk protein with relatively small molecular weight.

[0010] Silk amino acids: refers to silk protein products that are more deeply hydrolyzed, have smaller molecular weights, and are mainly composed of amino acids and short peptides.

[0011] Preferably, in step (1), the cationic surfactant is cetrimonium chloride. Cetrimonium chloride is a commonly used and highly effective hair conditioner, and its complex with peptides has good water dispersibility.

[0012] More preferably, the cationic surfactant further comprises behenyltrimethylammonium methyl sulfate. Behenyltrimethylammonium methyl sulfate is a cationic agent with a larger molecular weight and a longer hydrophobic chain. When used in combination with cetrimonium chloride, the synergistic effect of cations with different chain lengths can be utilized to enhance the stability of the complex on the one hand, and form a stronger and smoother conditioning film on the hair on the other hand, further improving the post-wash feel and the durability of the repairing ingredients.

[0013] Preferably, in step (1), the pH of the reaction is 4.2-4.6, the temperature is 35-40℃, and the reaction time is 10-30 minutes. This mild acidic environment is conducive to cuticle closure and is also within the stable pH range for most peptides and proteins; the temperature and time are sufficient to ensure that the complex reaction proceeds fully, while avoiding the deactivation of active ingredients due to prolonged high temperature.

[0014] Preferably, in step (3), the fatty alcohol is cetearyl alcohol, which is a classic solid fatty alcohol in cream products, playing a role in thickening, stabilizing and emulsifying; the silicone oil contains polydimethylsiloxane alcohol. Polydimethylsiloxane alcohol is a reactive silicone oil, and its terminal hydroxyl groups can form strong hydrogen bonds with the hydroxyl groups of fatty alcohols, which is crucial for building a stable product structure.

[0015] Preferably, the silicone oil further comprises at least one selected from amino-terminated polydimethylsiloxane and bis-aminopropyl polydimethylsiloxane. These amino-modified silicone oils are positively charged, which not only provides excellent smoothness but also forms stronger adsorption on the hair strands and synergizes with the cationic compounds in the pre-composite system to further enhance the entire conditioning and repair network.

[0016] Preferably, the gradient cooling in step (6) includes: First stage: Cool the temperature of the mixture to 35°C at a cooling rate of 0.5°C / min, and keep it at this temperature for 10-20 minutes; Second stage: The material is further cooled to 25°C at a cooling rate of 1.0°C / min.

[0017] Traditional processes employ rapid cooling, which can cause crystallizing agents such as cetearyl alcohol to quickly form large, uneven crystals, resulting in a rough, inconsistent texture and consistency in the ointment. The "gradient cooling" process of this invention imparts a superior ointment texture—fine, smooth, and highly stable—and effectively encapsulates and fixes the formed active complex within a network. During use, through massage and body heat, this structure slowly releases the active ingredients, prolonging the duration of action and achieving a sustained-release repair effect.

[0018] This invention involves pre-reacting a negatively charged or amphoteric bioactive peptide (acetyl hexapeptide-8) with a positively charged cationic surfactant in a specific weakly acidic aqueous environment. Under these conditions, the two form a stable "peptide-cationic complex" through intermolecular forces such as electrostatic attraction and hydrogen bonding. The purpose is to: 1) pre-neutralize some of the charge, reducing the risk of flocculation or precipitation when the active ingredient is subsequently added to the main cationic emulsion system, thus improving formulation stability; 2) react with the peptide to make it positively charged overall, thereby facilitating strong electrostatic adsorption onto the equally negatively charged surface of damaged hair strands, significantly improving the adsorption rate and rinsing retention rate of the active ingredient, laying the foundation for long-lasting repair.

[0019] Secondly, the present invention provides a polypeptide silk intensive moisturizing hair mask, which is prepared by the preparation method described in the first aspect.

[0020] Preferably, by weight percentage, it comprises: 0.05%-0.3% acetyl hexapeptide-8, 2.0%-5.0% a combination of cetrimonium chloride and behenyltrimethylammonium methyl sulfate, 0.01%-0.5% hydrolyzed silk and silk amino acids, 5.0%-8.0% cetearyl alcohol, and 0.1%-0.5% polydimethylsiloxane alcohol.

[0021] Thirdly, the present invention provides the application of a polypeptide silk intensive moisturizing hair mask in the preparation of products for hair care.

[0022] The hair care film of this invention is especially suitable for caring for damaged hair caused by perming, dyeing, blow-drying, etc. It can provide deep moisturizing, repair and protection, and can be used to prepare high-end repair hair masks, hair creams and other products.

[0023] The beneficial effects of this invention are: This invention effectively improves the charge conflict between active ingredients and the cationic system by pre-forming a stable peptide-cationic complex, thereby enhancing the stability of the active ingredients and their adsorption and retention rate on the hair. At the same time, through a gradient cooling process, a fine and stable product is constructed, which not only makes the cream texture delicate and smooth, but also enables the encapsulation and sustained release of active repair ingredients. The two innovative processes work synergistically to ultimately give the product both stability and long-lasting repair function. Detailed Implementation

[0024] To further illustrate the technical means and effects of the present invention in achieving its intended purpose, the following detailed description of the specific implementation methods, structures, features, and effects of the present invention, in conjunction with embodiments, is provided below.

[0025] Example 1 A method for preparing a polypeptide silk intensive moisturizing hair mask includes: formula: Aqueous phase components: deionized water (to 1000 g), behenyltrimethylammonium methyl sulfate (90%) 20.0 g, glycerol 10.0 g, hydroxyethyl cellulose 2.0 g, disodium EDTA 0.5 g.

[0026] Oil phase components: 70.0 g cetearyl alcohol, 2.0 g polydimethylsiloxane alcohol, 5.0 g ammonia-terminated polydimethylsiloxane.

[0027] Pre-composite active ingredients: 20.0 g deionized water, 1.5 g cetrimonium chloride, 13.3 g behenyltrimethylammonium methyl sulfate (90%), 1.2 g acetyl hexapeptide-8, 3.0 g hydrolyzed silk, and 2.0 g silk amino acids.

[0028] Other components: 1.5 g panthenol, 8.0 g phenoxyethanol (and ethylhexylglycerin), 4.0 g fragrance, and an appropriate amount of 10% lactic acid aqueous solution.

[0029] Preparation process: (1) Weigh deionized water into a premixed container, and add cetrimonium chloride, behenryl trimethylammonium methyl sulfate and acetyl hexapeptide-8 in sequence, stirring until completely dissolved. Use a 10% lactic acid aqueous solution as a pH adjuster to adjust the pH of the mixture to 4.5. Place the container in a 38°C water bath, keep it warm and maintain gentle stirring, and react for 15 minutes to form a polypeptide-cationic complex.

[0030] (2) In the main reactor, add the following materials as aqueous phase components: deionized water (as a solvent, to a total weight of 1000 g), behenyltrimethylammonium methyl sulfate, glycerol, hydroxyethyl cellulose, and disodium EDTA. Turn on the stirring and heat to raise the system temperature to and maintain it at 78°C. Continue stirring for about 20 minutes until all components are completely dissolved or uniformly dispersed to obtain a homogeneous viscous liquid.

[0031] (3) In another heated container, add the following materials as oil phase components: cetearyl alcohol, polydimethylsiloxane alcohol, and ammonia-terminated polydimethylsiloxane. Heat to 78°C and stir until all solid components are completely melted to form a clear, homogeneous oil phase liquid.

[0032] (4) While continuously stirring, slowly and uniformly pour all the oil phase liquid obtained in step (3) into the aqueous phase prepared in step (2). During and after the addition, turn on the homogenizer of the main reactor and perform high-speed shear emulsification at a speed of 2000 rpm, while maintaining the system temperature at 78°C. Continue homogenizing and emulsifying for 5 minutes to obtain a uniform and delicate white primary emulsion. Stop heating and begin cooling.

[0033] (5) When the temperature of the primary emulsion obtained in step (4) drops to 45°C, the polypeptide-cationic complex prepared in step (1), as well as the hydrolyzed silk and silk amino acids, which are active ingredients of hydrolyzed silk protein, are slowly added to it under stirring. After the addition is complete, continue stirring for 10 minutes to ensure that all active ingredients are fully mixed and evenly dispersed. Subsequently, the following components are added in sequence: panthenol, phenoxyethanol (a preservative compounded with ethylhexylglycerin), and fragrance. A uniformly mixed paste is obtained.

[0034] (6) This step uses programmed temperature-controlled cooling water to cool the reactor jacket. First, a first cooling stage is performed: the material temperature is slowly reduced from 45℃ to 35℃ at a rate of 0.5℃ / min. After reaching 35℃, a heat preservation stage is initiated: stirring is maintained at 35℃ for 15 minutes. After heat preservation, a second cooling stage is performed: the material is further cooled to 25℃ at a rate of 1.0℃ / min. After cooling is complete, stirring is stopped, the material is discharged, and after passing inspection, it is packaged to obtain the polypeptide silk intensive moisturizing hair mask. The resulting product is a smooth and delicate paste.

[0035] Example 2 A method for preparing a polypeptide silk intensive moisturizing hair mask includes: The preparation method is the same as in Example 1, only the amount of the key active ingredient is adjusted: Acetyl hexapeptide-8 0.5 g, hydrolyzed silk 1.0 g, silk amino acids 4.0 g, with the amino-terminated polydimethylsiloxane replaced by an equal amount of bis-aminopropylpolydimethylsiloxane; the amounts of the remaining components and all process steps and parameters are consistent with those in Example 1.

[0036] Example 3 A method for preparing a polypeptide silk intensive moisturizing hair mask includes: The difference from Example 1 is that behenyltrimethylammonium methyl sulfate is not used, while the amounts of other components and all process steps and parameters are consistent with those in Example 1.

[0037] Comparative Example 1 The difference from Example 1 is that step (1) is omitted, and cetrimonium chloride and behenyltrimethylammonium methyl sulfate are dissolved in the aqueous phase by heating; acetyl hexapeptide-8, hydrolyzed silk, and silk amino acids are directly dissolved in a small amount of room temperature water for later use. After the main emulsification temperature is cooled to 45°C, this aqueous solution of active ingredients is added directly and mixed evenly. The subsequent cooling steps are the same as in Example 1.

[0038] Comparative Example 2 The difference from Example 1 is that a traditional rapid cooling process is used. After completing step (4), the reactor is placed in an ice-water bath, and stirring is turned on to rapidly cool the material from 45°C to 25°C within 15 minutes. The remaining steps are the same as in Example 1.

[0039] Comparative Example 3 The difference from Comparative Example 1 is that a traditional rapid cooling process was used. After emulsification, the reactor was placed in an ice-water bath, and stirring was started to rapidly cool the material from 45°C to 25°C within 15 minutes. The remaining steps were the same as in Comparative Example 1.

[0040] Performance testing: 1. Evaluation of Paste Texture: Take an appropriate amount of sample onto a clean glass plate and have three experienced personnel independently conduct a sensory evaluation under natural light, comprehensively assessing color, fineness, gloss, and uniformity. The rating criteria are: Excellent (fine and smooth), Good (uniform and free of particles), Fair (slightly grainy), and Poor (rough and grainy).

[0041] 2. Basic stability testing Heat resistance stability: Place the sample in a 45℃ constant temperature chamber for 28 days. After the expiration date, observe whether there are any changes in appearance, odor, and paste structure.

[0042] Cold resistance stability: Place the sample in a -5℃ refrigerator for 28 days. After the expiration period, restore it to room temperature and observe whether the paste is normal and whether there is any oil-water separation.

[0043] 3. Efficacy testing Wet combing force reduction rate: Using a standard bleached damaged hair strand (20 cm in length, 5.0 g in weight), 2.0 g of sample was evenly applied, left to stand for 3 minutes, rinsed with 37°C running deionized water for 30 seconds, and then the surface moisture was blotted dry. The maximum resistance during combing from root to tip was measured using a digital tension meter. The combing force reduction rate was calculated using an untreated hair strand as a baseline. Combing force reduction rate (%) = (F0 - F1) / F0 × 100% Durability of effect: After the hair bundle has undergone the above treatment and an initial 30-second rinse, it is placed under running deionized water at 37°C for continuous rinsing. The hair bundle is removed after rinsing for 2 minutes, 5 minutes, and 10 minutes respectively, the water is patted dry, and its wet combing ability is measured.

[0044] Combing force retention rate (%) = F1 / F t × 100%, where: F t The combing force (unit: cN) after rinsing for t minutes is the combing force after rinsing, where t is the rinsing time (2, 5, 10 minutes).

[0045] Table 1: Results of Paste Texture and Stability Tests Table 2: Results of efficacy tests Note: The combing force retention rate is based on the combing force in the "initial" state as 100%.

[0046] This invention utilizes a "pre-compound reaction" and "gradient cooling" process to prepare a polypeptide-silk intensive moisturizing hair mask with a delicate and stable paste texture, excellent immediate smoothing effect, and long-lasting repair efficacy that is resistant to rinsing. This product effectively delivers active ingredients to and adheres to the hair strands, providing long-lasting repair.

[0047] The above description is merely a preferred embodiment of the present invention and is not intended to limit the present invention in any way. Although the present invention has been disclosed above with reference to preferred embodiments, it is not intended to limit the present invention. Any person skilled in the art can make some modifications or alterations to the above-disclosed technical content to create equivalent embodiments without departing from the scope of the present invention. Any simple modifications, equivalent changes and alterations made to the above embodiments based on the technical essence of the present invention without departing from the scope of the present invention shall still fall within the scope of the present invention.

Claims

1. A method for preparing a polypeptide silk intensive moisturizing hair mask, characterized in that, Includes the following steps: (1) Acetyl hexapeptide-8 was reacted with a cationic surfactant at pH 4.0-4.8 and temperature 30-45℃ to form a polypeptide-cationic complex; (2) Heat and mix the aqueous phase components; (3) Heat and mix the oil phase components, wherein the oil phase components include fatty alcohols and silicone oil; (4) Add the oil phase to the aqueous phase for emulsification and cool to 40-50℃; (5) Add the polypeptide-cationic complex and hydrolyzed silk protein active ingredients obtained in step (1) to the emulsion matrix of step (4) and mix evenly; (6) The mixture is subjected to gradient cooling to obtain the hair care film.

2. The method for preparing the polypeptide silk intensive moisturizing hair mask according to claim 1, characterized in that, In step (1), the cationic surfactant is cetrimonium chloride.

3. The method for preparing the polypeptide silk intensive moisturizing hair mask according to claim 2, characterized in that, The cationic surfactant also contains behenyltrimethylammonium methyl sulfate.

4. The method for preparing the polypeptide silk intensive moisturizing hair mask according to claim 1, characterized in that, In step (1), the pH of the reaction is 4.2-4.6, the temperature is 35-40℃, and the reaction time is 10-30 minutes.

5. The method for preparing the polypeptide silk intensive moisturizing hair mask according to claim 1, characterized in that, In step (3), the fatty alcohol is cetearyl alcohol; the silicone oil contains polydimethylsiloxane alcohol.

6. The method for preparing the polypeptide silk intensive moisturizing hair mask according to claim 5, characterized in that, The silicone oil also contains at least one selected from amino-terminated polydimethylsiloxane and bis-aminopropyl polydimethylsiloxane.

7. The method for preparing the polypeptide silk intensive moisturizing hair mask according to claim 1, characterized in that, The gradient cooling described in step (6) includes: First stage: Cool the temperature of the mixture to 35°C at a cooling rate of 0.5°C / min, and keep it at this temperature for 10-20 minutes; Second stage: The material is further cooled to 25°C at a cooling rate of 1.0°C / min.

8. A polypeptide silk intensive moisturizing hair mask, characterized in that, It is prepared by any one of claims 1-7.

9. The polypeptide silk intensive moisturizing hair mask of claim 8, wherein, By weight percentage, it contains: 0.05%-0.3% acetyl hexapeptide-8, 2.0%-5.0% a combination of cetrimonium chloride and behenyltrimethylammonium methyl sulfate, 0.01%-0.5% hydrolyzed silk and silk amino acids, 5.0%-8.0% cetearyl alcohol, and 0.1%-0.5% polydimethylsiloxane alcohol.

10. The use of a polypeptide silk intensive moisturizing hair mask as described in claim 8 or 9 in the preparation of a hair care product.

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