Shampoo containing plant squalane small molecule oil and preparation method thereof

Abstract

The invention relates to shampoo containing plant squalane small molecule oil and a preparation method of the shampoo. The shampoo containing the plant squalane small molecule oil is prepared from the following components in parts by mass: 3 to 5 parts of fatty alcohol-polyoxyethylene ether, 2 to 5 parts of cocamidopropyl betaine, 2 to 4 parts of sodium fatty alcohol-polyoxyethylene ether carboxylate, 0.1 to 2 parts of a cationic surfactant, 0.1 to 2 parts of amino acid, 1 to 2 parts of squalane, 0.1 to 1 part of modified squalene and a solvent, wherein the modified squalene is a product obtained by copolymerizing squalene, sodium methacrylate and methacrylic acid. According to the shampoo containing the plant squalane small molecule oil, the specific modified squalene and various surfactants are compounded with the active ingredients, so that the stability and dispersity of the ingredients are enhanced, the effect that the shampoo can be stored for a long time is ensured, the effects of cleaning and nourishing hair are achieved, and the shampoo has a good application prospect.

Description

Technical Field

[0001] The invention relates to the technical field of daily chemical products, and in particular to a shampoo containing plant squalane small molecule oil and a preparation method thereof. Background Art

[0002] Squalane is a natural ingredient highly compatible with human sebum, offering excellent moisturizing and repairing properties. It quickly penetrates the skin, forming a thin, breathable protective layer that effectively locks in moisture and prevents dryness and moisture loss. Squalane also possesses antioxidant and soothing properties, helping to repair a damaged skin barrier and reduce the effects of external irritants, leaving skin softer and smoother. Its mild, non-irritating properties also make it suitable for sensitive skin and all skin types.

[0003] Squalane is also commonly added to hair care products such as shampoos, conditioners, and hair masks, improving hair health with its exceptional nourishing and repairing properties. It penetrates deeply into the hair, filling the gaps between the cuticles, reducing frizz and split ends, and enhancing hair's smoothness and shine. Furthermore, squalane can help repair hair damage caused by perming, dyeing, and high-temperature blow-drying, providing long-lasting moisturization and strengthening hair. It is particularly suitable for those with dry, damaged hair.

[0004] However, squalane is highly hydrophobic and has stability issues in water-based shampoo and other products. It is prone to stratification, precipitation or aggregation, affecting the uniformity of the product and the user experience. In addition, when using shampoo, if the active ingredients such as squalane are unevenly distributed, it will be difficult to fully adhere to the hair in a short period of time and it will be more likely to be washed away, which will greatly reduce the effectiveness of the product and fail to achieve the ideal moisturizing and repairing hair functions. Therefore, how to improve the stability of squalane-based shampoo products, enhance the dispersion and uniformity of the components, avoid precipitation or stratification during storage or use, and thus improve the quality of the product and the user experience, is a difficult problem faced by this field.

[0005] Based on this, it is necessary to develop a new product to overcome the defects in the prior art. Summary of the Invention

[0006] The present invention aims to address the shortcomings of the prior art by providing a shampoo containing plant-based squalane small molecule oil. This shampoo, containing plant-based squalane small molecule oil, utilizes a specific modified squalene and a combination of multiple surfactants and active ingredients to enhance the stability and dispersibility of the components, ensuring long-term storage and achieving the desired cleansing and nourishing effects on hair. The shampoo has promising application prospects.

[0007] One object of the present invention is to provide a shampoo containing plant squalane small molecule oil, comprising the following components in parts by weight:

[0008]

[0009]

[0010] solvents;

[0011] Wherein, the modified squalene is a product obtained by copolymerization of squalene, sodium methacrylate and methacrylic acid.

[0012] Furthermore, the molar ratio of squalene, sodium methacrylate and methacrylic acid is 1:1:1-1:0.3:0.3.

[0013] Furthermore, the amino acid is selected from one or more of arginine, serine, methionine, glutamic acid, glycine, proline, aspartic acid, and cysteine.

[0014] Furthermore, it also includes: an auxiliary agent.

[0015] Furthermore, the auxiliary agent is selected from one or more of a chelating agent, a fragrance, a pH regulator, and a solubilizer.

[0016] Furthermore, the cationic surfactant is selected from one or more of a single-long straight-chain quaternary ammonium salt, a dilong straight-chain quaternary ammonium salt, a benzyl quaternary ammonium salt, a hydroxyalkyl quaternary ammonium salt, a fatty amide propyl hydroxyalkyl quaternary ammonium salt, and a polyquaternary ammonium salt obtained by copolymerization of vinyl pyrrolidone, an unsaturated amide or an unsaturated quaternary ammonium salt.

[0017] Furthermore, the squalane is of plant origin.

[0018] Preferably, the method for preparing squalane comprises the following steps:

[0019] L1. Extraction of squalene:

[0020] Take 30g of olive oil, 6g of KOH, and 60mL of 95% ethanol and add them to a three-necked flask. React with nitrogen as the protective gas while stirring continuously. Reflux in a water bath at 100°C for 10 hours. After stopping the reaction, quickly add 200mL of distilled water. Extract the unsaponifiable matter with 250mL of petroleum ether in five steps. Wash the ether phase with HCl and a 5% NaCl aqueous solution, and finally wash with water until the washing liquid is neutral. Add an appropriate amount of anhydrous Na2SO4 to absorb the residual water in the ether phase. Remove the solvent by rotary evaporation at 60°C to obtain the unsaponifiable matter of olive oil.

[0021] The unsaponifiable matter of olive oil was fed into a primary molecular distillation apparatus, and the primary molecular distillation was carried out at 100° C., a system pressure of 0.001 mbar, a feed rate of 1 mL / min, and a scraping speed of 150 rpm. The distillate was collected for secondary molecular distillation; the secondary molecular distillation was carried out at 150° C., a system pressure of 0.001 mbar, a feed rate of 1 mL / min, and a scraping speed of 200 rpm. The distillate under the corresponding conditions was collected to obtain crude squalene.

[0022] Weigh 30g of silica gel (200-300 mesh), activate it at high temperature in an oven for 3-5h, cool it to room temperature in a desiccator, add 30mL of n-hexane, stir it, and wet-pack it into a column using n-hexane as the eluent. Add 1g of crude squalene. Use 100mL of n-hexane, 100mL of 1% ethyl acetate-n-hexane, 200mL of 5% ethyl acetate-n-hexane, and 200mL of 10% ethyl acetate-n-hexane as the mobile phases, respectively. Use an automatic fraction collector to collect 20ml of each fraction, evaporate and remove the solvent, and combine the same fractions after chromatographic detection to obtain purified squalene.

[0023] L2. Hydrogenation of squalene:

[0024] 100 g of squalene and 1 g of nickel catalyst Ni9910 were added to a reactor, hydrogen was introduced, and the reaction was carried out at 2 MPa and 190° C. for 5 h to obtain squalane.

[0025] Another object of the present invention is to provide a method for preparing the above-mentioned shampoo containing plant squalane small molecule oil, wherein the method for preparing the shampoo containing plant squalane small molecule oil comprises the following steps:

[0026] S1. Squalene, sodium methacrylate, methacrylic acid, an emulsifier and an initiator were mixed and heated under a nitrogen atmosphere to obtain modified squalene;

[0027] S2. Add fatty alcohol polyoxyethylene ether, cocamidopropyl betaine, sodium fatty alcohol polyoxyethylene ether carboxylate, and cationic surfactant to the solvent, heat and stir, then add the modified squalene, squalane and amino acid, stir evenly, and obtain a shampoo containing plant squalane small molecule oil.

[0028] Furthermore, in step S1, the temperature of the heating reaction is 50-90°C.

[0029] Furthermore, in step S2, the temperature of the heating and stirring is 40-80°C.

[0030] Compared with the prior art, the present invention has the following beneficial effects:

[0031] The invention discloses a shampoo containing plant squalane small molecule oil. The shampoo contains multiple components such as squalane, a surfactant, and modified squalene. The modified squalene is obtained by copolymerizing squalene with acrylic acid and sodium acrylate. On the one hand, the component contains lipophilic squalene segments and hydrophilic acrylic acid and acrylate segments, and thus has amphiphilic properties, which is beneficial for improving the stability of the shampoo emulsion and enhancing the washing and decontamination effects. On the other hand, squalene has similar polarity to squalane and has good affinity, and thus can promote the dispersion effect of hydrophobic components such as squalane, so that the product has a more stable and uniform system, thereby improving the user experience.

[0032] Furthermore, the modified squalene copolymer forms a network structure, resulting in improved film-forming properties. This facilitates the film formation of surfactants and active ingredients on the hair, achieving enhanced hair care and nourishment results. Furthermore, the network polymer provides stability to the formula, further stabilizing cationic and anionic surfactants, and preventing delamination or precipitation under high and low temperature testing. DETAILED DESCRIPTION

[0033] In order to more clearly illustrate the technical solution of the present invention, the following embodiments are listed, but the present invention is not limited thereto.

[0034] Unless otherwise specified, the experimental methods used in the following examples are conventional methods; the reagents, materials, etc. used in the following examples are all commercially available unless otherwise specified.

[0035] The fatty alcohol polyoxyethylene ether in the embodiment of the present invention is AEO-9;

[0036] The cocamidopropyl betaine in the embodiment of the present invention is CAB-35;

[0037] The sodium fatty alcohol polyoxyethylene ether carboxylate in the embodiment of the present invention is AEC-9Na;

[0038] The cationic surfactant in the embodiment of the present invention is polyquaternium-11;

[0039] The amino acids in the embodiment of the present invention are arginine, serine, aspartic acid, glutamic acid and cysteine ​​in a mass ratio of 1:1:1:1:1.

[0040] The pH regulator in the embodiment of the present invention is citric acid.

[0041] The emulsifier in the embodiment of the present invention is OP-10 (dodecylphenol polyoxyethylene ether); the initiator is potassium persulfate.

[0042] The “parts” in the embodiments of the present invention refer to parts by mass.

[0043] Example 1

[0044] A shampoo containing plant squalane small molecule oil, comprising the following components in parts by mass:

[0045]

[0046] The preparation method of the shampoo containing plant squalane small molecule oil comprises the following steps:

[0047] S1. Using water as a solvent, squalene, sodium methacrylate, and methacrylic acid were mixed in a molar ratio of 1:0.5:0.8, and then 4% of the mass of the reactants and 1% of the mass of the initiator were added. The reaction was carried out at 70 ° C under a nitrogen atmosphere for 6 hours, and the solvent was removed and dried to obtain modified squalene;

[0048] S2. Add fatty alcohol polyoxyethylene ether, cocamidopropyl betaine, sodium fatty alcohol polyoxyethylene ether carboxylate, and cationic surfactant to water according to the above-mentioned mass fractions, heat and stir at 60°C for 2 minutes, then add the modified squalene, squalane and amino acid, stir evenly, and add a pH adjuster to obtain a shampoo containing plant squalane small molecule oil.

[0049] Example 2

[0050] A shampoo containing plant squalane small molecule oil, comprising the following components in parts by mass:

[0051]

[0052]

[0053] The preparation method of the shampoo containing plant squalane small molecule oil comprises the following steps:

[0054] S1. Using water as a solvent, squalene, sodium methacrylate, and methacrylic acid were mixed in a molar ratio of 1:0.5:0.5, and then 4% of the mass of the reactants and 1% of the mass of the initiator were added. The reaction was carried out at 70 ° C under a nitrogen atmosphere for 6 hours, and the solvent was removed and dried to obtain modified squalene;

[0055] S2. Add fatty alcohol polyoxyethylene ether, cocamidopropyl betaine, sodium fatty alcohol polyoxyethylene ether carboxylate, and cationic surfactant to water according to the above-mentioned mass fractions, heat and stir at 60°C for 2 minutes, then add the modified squalene, squalane and amino acid, stir evenly, and add a pH adjuster to obtain a shampoo containing plant squalane small molecule oil.

[0056] Example 3

[0057] A shampoo containing plant squalane small molecule oil, comprising the following components in parts by mass:

[0058]

[0059] The preparation method of the shampoo containing plant squalane small molecule oil comprises the following steps:

[0060] S1. Using water as a solvent, squalene, sodium methacrylate, and methacrylic acid were mixed in a molar ratio of 1:0.5:0.8, and then 4% of the mass of the reactants and 1% of the mass of the initiator were added. The reaction was carried out at 70 ° C under a nitrogen atmosphere for 6 hours, and the solvent was removed and dried to obtain modified squalene;

[0061] S2. Add fatty alcohol polyoxyethylene ether, cocamidopropyl betaine, sodium fatty alcohol polyoxyethylene ether carboxylate, and cationic surfactant to water according to the above-mentioned mass fractions, heat and stir at 60°C for 2 minutes, then add the modified squalene, squalane and amino acid, stir evenly, and add a pH adjuster to obtain a shampoo containing plant squalane small molecule oil.

[0062] Comparative Example 1

[0063] A shampoo containing plant squalane small molecule oil. The difference between this comparative example and Example 1 is that squalene in step S1 is replaced by butyl acrylate, and other ingredients and preparation methods are the same as those in Example 1.

[0064] Comparative Example 2

[0065] A shampoo containing plant squalane small molecule oil. The difference between this comparative example and Example 1 is that step S1 is deleted, and the modified squalene is replaced by unmodified squalene. Other ingredients and preparation methods are the same as those in Example 1.

[0066] Test Example 1

[0067] Stability testing

[0068] The shampoos containing plant squalane small molecule oil of Examples 1-3 and Comparative Examples 1-2 were selected for stability testing, and the testing method was as follows:

[0069] High temperature stability: Take 200 ml of each of the above samples, put them into transparent small bottles and seal them, place them in an environment of 45℃±1℃, keep the constant temperature for 1 month, then return to room temperature of 25℃ and observe their appearance.

[0070] Low temperature stability: Take 200 ml of each of the above samples, put them into transparent small bottles and seal them, place them in an environment of 0℃±2℃, keep them at constant temperature for 1 month, and observe their appearance.

[0071] The test results are shown in Table 1.

[0072] Table 1 Stability test

[0073] sample High temperature stability Low temperature stability Example 1 The product is uniform, without stratification or precipitation The product is uniform, without stratification or precipitation Example 2 The product is uniform, without stratification or precipitation The product is uniform, without stratification or precipitation Example 3 The product is uniform, without stratification or precipitation The product is uniform, without stratification or precipitation Comparative Example 1 The product is uniform, without stratification or precipitation Obvious stratification Comparative Example 2 Obvious stratification Obvious stratification

[0074] The above test results demonstrate that the shampoo samples of Examples 1-3 exhibit excellent high- and low-temperature stability, maintaining uniform and stable dispersion of multiple components under diverse extreme conditions, avoiding precipitation and stratification. However, the substitution of modified squalene in Comparative Examples 1 and 2 resulted in reduced compatibility between components, significantly diminishing the stability and uniformity of the shampoo formulations and failing to meet practical application requirements.

[0075] Test Example 2

[0076] Efficacy test

[0077] The shampoos containing plant squalane small molecule oil of Example 1 and Comparative Examples 1-2 were selected for efficacy testing, and the testing method was as follows:

[0078] One hundred female volunteers aged 20-30 were randomly divided into five groups of 20 participants each. Each group was assigned to a trial of 5-7 g of the shampoo samples of Examples 1-3 and Comparative Examples 1-2, using them once daily for one week. The shampoo samples were evenly applied to the hair and scalp, gently applied for approximately 2 minutes, then quickly rinsed with water and air-dried. After air-drying, the effects on hair quality and scalp itching were evaluated and scored, with the results averaged across the groups.

[0079] The scoring range is 1-5 points, and the standards for each score are as follows:

[0080] 1 point: no improvement; 2 points: slight improvement; 3 points: some improvement; 4 points: significant improvement; 5 points: significant improvement.

[0081] The test results are shown in Table 2.

[0082] Table 2 Usage effect test

[0083] sample Improved hair quality Improved itching Example 1 3.70 4.05 Example 2 3.80 4.10 Example 3 3.55 3.90 Comparative Example 1 3.15 3.35 Comparative Example 2 3.30 3.55

[0084] The above test results demonstrate that the various components of the shampoos containing plant squalane small molecule oil prepared in Examples 1-3 are uniformly dispersed, promoting film formation and adhesion, thereby ensuring that the multiple active ingredients improve hair quality and scalp health, demonstrating excellent efficacy in improving hair quality and pruritus. However, Comparative Examples 1-2, which replaced the modified squalene ingredient, exhibited reduced formulation uniformity and decreased absorption into the hair and scalp, ultimately resulting in less than ideal improvements in hair quality and scalp quality.

[0085] 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 embodied in other specific forms without departing from the spirit or essential characteristics of the invention. Therefore, the embodiments should be considered in all respects as illustrative and non-restrictive, and the scope of the invention is defined by the appended claims rather than the foregoing description, and it is intended that all variations that come within the meaning and range of equivalents of the claims be embraced therein.

[0086] In addition, it should be understood that although this specification is described in terms of implementation methods, not every implementation method contains only one independent technical solution. This narrative method of the specification is only for the sake of clarity. Those skilled in the art should regard the specification as a whole. The technical solutions in each embodiment can also be appropriately combined to form other implementation methods that can be understood by those skilled in the art.

Claims

1. A shampoo containing plant squalane small molecule oil, characterized in that: The shampoo containing plant squalane small molecule oil includes the following components in parts by mass: solvents; The modified squalene is a product obtained by copolymerization of squalene, sodium methacrylate and methacrylic acid.

2. The shampoo containing plant squalane small molecule oil according to claim 1, characterized in that: The molar ratio of squalene, sodium methacrylate and methacrylic acid is 1:1:1-1:0.3:0.

3.

3. The shampoo containing plant squalane small molecule oil according to claim 1, characterized in that: The amino acids are selected from one or more of arginine, serine, methionine, glutamic acid, glycine, proline, aspartic acid, and cysteine.

4. The shampoo containing plant squalane small molecule oil according to claim 1, characterized in that: Also includes: Additives.

5. The shampoo containing plant squalane small molecule oil according to claim 4, characterized in that: The auxiliary agent is selected from one or more of a chelating agent, a fragrance, a pH regulator, and a solubilizer.

6. The shampoo containing plant squalane small molecule oil according to claim 1, characterized in that: The cationic surfactant is selected from one or more of single-long linear quaternary ammonium salts, double-long linear quaternary ammonium salts, benzyl quaternary ammonium salts, hydroxyalkyl quaternary ammonium salts, fatty amide propyl hydroxyalkyl quaternary ammonium salts, and polyquaternary ammonium salts obtained by copolymerization of vinyl pyrrolidone, unsaturated amide or unsaturated quaternary ammonium salt.

7. The shampoo containing plant squalane small molecule oil according to claim 1, characterized in that: The squalane is of plant origin.

8. The method for preparing the shampoo containing plant squalane small molecule oil according to any one of claims 1 to 7, characterized in that: The preparation method of the shampoo containing plant squalane small molecule oil comprises the following steps: S1. Squalene, sodium methacrylate, methacrylic acid, an emulsifier and an initiator were mixed and heated under a nitrogen atmosphere to obtain modified squalene; S2. Add fatty alcohol polyoxyethylene ether, cocamidopropyl betaine, sodium fatty alcohol polyoxyethylene ether carboxylate, and cationic surfactant to the solvent, heat and stir, then add the modified squalene, squalane and amino acid, stir evenly, and obtain a shampoo containing plant squalane small molecule oil.

9. The method for preparing the shampoo containing plant squalane small molecule oil according to claim 8, characterized in that: In step S1, the temperature of the heating reaction is 50-90°C.

10. The method for preparing the shampoo containing plant squalane small molecule oil according to claim 8, characterized in that: In step S2, the temperature of the heating and stirring is 40-80°C.

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