High-stability sulfur mite-removing liquid soap and preparation method thereof

Abstract

The present application belongs to the cosmetic technical field, and particularly relates to a high-stability sulfur acaricidal liquid soap and a preparation method thereof. The liquid soap comprises the following raw material components in percentage by weight: natural soap base 6-15%, auxiliary surfactant 2-10%, skin conditioner 5-15%, cross-linked cyclodextrin-coated modified sulfur 1-5%, thickening agent 0.05-0.2%, preservative 0.05-0.5%, essence 0.05-0.2%, and the rest is water. The preparation method comprises the following steps: adding the natural soap base, auxiliary surfactant and thickening agent into hot water at 60-80 DEG C to mix uniformly to obtain an aqueous solution; then adding the skin conditioner and cross-linked cyclodextrin-coated modified sulfur to homogenize and emulsify uniformly, and then reducing to normal temperature; adding the preservative and essence to mix uniformly, discharging, and obtaining the high-stability sulfur acaricidal liquid soap. The present application can significantly improve the stability of sulfur acaricidal powder in the liquid soap formula.

Description

Technical Field

[0001] This invention belongs to the field of cosmetic technology, specifically relating to a highly stable sulfur-based anti-mite liquid soap and its preparation method. Background Technology

[0002] Sulfur possesses antibacterial and anti-inflammatory properties, effectively alleviating skin problems such as acne and herpes. It can penetrate the skin, reduce inflammation and redness, and promote the skin's self-repair ability. Simultaneously, sulfur has strong bactericidal capabilities, effectively inhibiting the growth of bacteria and fungi, preventing infection and disease. Therefore, sulfur is frequently used as a functional ingredient in the manufacture of cosmetics and hygiene products.

[0003] For example, Chinese patent CN 107955754 A discloses an antibacterial and anti-mite soap. By adding antibacterial agents and sulfur, the resulting antibacterial and anti-mite soap can achieve both cleaning and antibacterial / anti-mite effects. Chinese patent CN112251302 A discloses a perfumed latex soap that achieves good antibacterial effects by adding sulfur. However, conventional solid soaps require rinsing and rubbing under water before use to wash the skin, and are in direct contact with air and moisture, resulting in poor convenience and hygiene.

[0004] Liquid soaps are gaining popularity due to their ease of squeezing and application, offering both hygiene and convenience. However, unlike solid soaps where the soap base effectively disperses and stabilizes solid sulfur, surfactants in liquid soaps struggle to effectively stabilize insoluble solid sulfur components in the liquid phase, resulting in poor stability. Current methods to improve the dispersibility of solid sulfur in liquid products involve encapsulating it with gum arabic to create colloidal sulfur products. However, gum arabic's high water solubility causes it to dissolve and break the encapsulation during prolonged storage, allowing elemental sulfur to escape and failing to effectively improve storage stability in emulsion products. Chinese patent CN117898953A discloses a triple-encapsulated colloidal sulfur, its preparation method, and its applications. This triple-encapsulation effectively reduces the irritation and odor of sulfur, significantly improving the user experience of colloidal sulfur in cosmetic applications. However, the preparation method for this colloidal sulfur is complex and costly. Summary of the Invention

[0005] The purpose of this invention is to overcome the shortcomings and deficiencies of the prior art and provide a highly stable sulfur-based anti-mite liquid soap and its preparation method.

[0006] The objective of this invention is achieved through the following technical solution:

[0007] A highly stable sulfur-based anti-mite liquid soap comprises the following raw material components in weight percentage:

[0008] Natural soap base 6-15%, auxiliary surfactant 2-10%, skin conditioning agent 5-15%, cross-linked cyclodextrin-coated modified sulfur 1-5%, thickener 0.05-0.2%, preservative 0.05-0.5%, fragrance 0.05-0.2%, balance water;

[0009] The preparation method of the cross-linked cyclodextrin-coated modified sulfur is as follows:

[0010] Cyclodextrin was added to an alkaline aqueous solution and heated to dissolve. Then, pentaerythritol glycidyl ether crosslinking agent and sulfur powder were added and stirred until homogeneous. The etherification and crosslinking reaction was carried out at 40-80℃ with stirring until the epoxy groups were completely reacted. After the reaction was completed, acid was added to neutralize the reaction, and the mixture was cooled to room temperature. Ethanol was added to disperse the reaction mixture, and the mixture was filtered. The solid product was taken, washed, and dried to obtain crosslinked cyclodextrin-coated modified sulfur.

[0011] The preparation principle of cross-linked cyclodextrin-coated modified sulfur in this invention is as follows: The polar hydroxyl groups of cyclodextrin bind with sulfur powder, and the reduced solubility of cyclodextrin in water after cross-linking with pentaerythritol glycidyl ether leads to in-situ precipitation of the cross-linked cyclodextrin on the surface of the sulfur powder after the etherification cross-linking reaction, thereby achieving coating modification of the sulfur powder. The compatibility of the sulfur powder modified with cross-linked cyclodextrin on the surface is significantly improved with surfactants, skin conditioners, and thickeners in liquid soap formulations, thus enhancing dispersion stability. Furthermore, the reduced solubility of the cross-linked cyclodextrin results in better coating stability.

[0012] Furthermore, the natural soap base is one or more of sodium oleate, sodium cocoate, and sodium palmitate.

[0013] Furthermore, the auxiliary surfactant is one or more of the following: cocamidopropyl betaine, fatty alcohol polyoxyethylene ether sulfate, sodium lauroylamphoteric acid, alkyl glycoside, cocoyl glutamate, cocoyl glycinate, lauroyl glutamate, myristoyl glutamate, and lauroyl sarcosine.

[0014] Furthermore, the skin conditioning agent is one or more of glycerin, vegetable oil, plant extract, hydroxystearic acid, ethylene glycol stearate, hydrogenated castor oil hydroxystearate, pentaerythritol tetraisostearate, and cationic starch.

[0015] Furthermore, the thickener is one or both of methyl methacrylate / ethylene glycol dimethacrylate crosspolymer and lauryl methacrylate / ethylene glycol dimethacrylate crosspolymer.

[0016] Furthermore, the preservative is phenoxyethanol.

[0017] Furthermore, in the preparation of the above-mentioned cross-linked cyclodextrin-coated modified sulfur, the cyclodextrin is β-cyclodextrin.

[0018] The alkaline aqueous solution is a sodium hydroxide solution with a pH value of 10 to 13.

[0019] The amount of the pentaerythritol glycidyl ether crosslinking agent added is 0.2% to 2% of the mass of the cyclodextrin.

[0020] The amount of sulfur powder added is 1 to 4 times the mass of cyclodextrin.

[0021] The so-called acid neutralization refers to neutralizing to neutral using hydrochloric acid.

[0022] The preparation method of the above-mentioned highly stable sulfur-based anti-mite liquid soap includes the following steps:

[0023] Natural soap base, auxiliary surfactants and thickeners are added to hot water at 60-80℃ and mixed evenly to obtain an aqueous solution; then skin conditioning agents and cross-linked cyclodextrin-coated modified sulfur are added and homogenized and emulsified evenly, cooled to room temperature, and then preservatives and fragrances are added and mixed evenly, and discharged to obtain a highly stable sulfur anti-mite liquid soap.

[0024] Compared with the prior art, the beneficial effects of the present invention are:

[0025] (1) The present invention uses cross-linked cyclodextrin to surface-coat and modify sulfur powder, which can significantly improve its stability in liquid soap formulation and ensure good anti-mite effect.

[0026] (2) The preparation method of cross-linked cyclodextrin coated modified sulfur of the present invention is simple, does not use toxic and harmful reagents, and is green and environmentally friendly. Detailed Implementation

[0027] The present invention will be further described in detail below with reference to embodiments, but the implementation of the present invention is not limited thereto.

[0028] Example 1

[0029] A highly stable sulfur-based anti-mite liquid soap has the following raw material composition:

[0030] Natural soap base: 10% sodium oleate;

[0031] Auxiliary surfactants: 4% cocamidopropyl betaine, 2% sodium fatty alcohol polyoxyethylene ether sulfate, and 1% sodium lauroyl sarcosinate;

[0032] Skin conditioning agents: 6% glycerin, 1% olive oil, 0.5% aloe vera extract, 0.2% hydrogenated castor oil hydroxystearate;

[0033] Acaricide: 3% cross-linked cyclodextrin-coated modified sulfur;

[0034] Thickener: 0.1% methyl methacrylate / ethylene glycol dimethacrylate crosspolymer;

[0035] Preservative: 0.1% phenoxyethanol;

[0036] Fragrance: 0.1%;

[0037] Water: Balance.

[0038] The preparation method of the cross-linked cyclodextrin-coated modified sulfur is as follows:

[0039] 50g of β-cyclodextrin was added to 500g of sodium hydroxide aqueous solution with pH 12 and heated to 75℃ to dissolve. Then, 0.5g of pentaerythritol glycidyl ether crosslinking agent and 150g of sulfur powder were added and stirred until homogeneous. The etherification crosslinking reaction was carried out at 70℃ with stirring for 4h until the epoxy groups were completely reacted. After the reaction was completed, hydrochloric acid was added to neutralize to neutral, and the mixture was cooled to room temperature. 500g of ethanol was added to disperse the mixture. The mixture was then vacuum filtered, and the solid product was washed with cold water and vacuum dried to obtain crosslinked cyclodextrin-coated modified sulfur.

[0040] The preparation method of the highly stable sulfur-based anti-mite liquid soap is as follows:

[0041] Prepare raw materials according to the mass percentage, add natural soap base, auxiliary surfactant and thickener to 75℃ hot water and mix evenly to obtain an aqueous solution; then add skin conditioning agent and mite remover and homogenize and emulsify evenly, cool to room temperature, then add preservative and fragrance and mix well, discharge to obtain highly stable sulfur mite-removing liquid soap.

[0042] The high-stability sulfur-based anti-mite liquid soap obtained in this embodiment has a viscosity of 3850 mPa·s and no obvious sulfur odor.

[0043] The high-stability sulfur-based anti-mite liquid soap obtained in this embodiment showed no sulfur precipitation in both the centrifugal stability test (centrifuged at 3000 r / min for 30 min) and the accelerated storage stability test (accelerated test in a 42℃ constant temperature chamber for 14 days, followed by centrifugation at 3000 r / min for 30 min), indicating good product stability.

[0044] The high-stability sulfur anti-mite liquid soap obtained in this embodiment was tested for its anti-mite effect (using genuine leather fabric washed with the liquid soap as the test sample and genuine leather fabric washed with distilled water as the control sample, and the anti-mite effect was evaluated with reference to the mite inhibition rate in GB / T 24253-2009). The results showed that the anti-mite inhibition rate was 85%, and the product has a strong anti-mite effect.

[0045] Example 2

[0046] A highly stable sulfur-based anti-mite liquid soap has the following raw material composition:

[0047] Natural soap base: 6% sodium cocoate;

[0048] Auxiliary surfactants: sodium fatty alcohol polyoxyethylene ether sulfate 4%, sodium lauroyl sarcosinate 4%, alkyl glycoside 2%;

[0049] Skin conditioning agents: 8% glycerin, 2% jojoba oil, 0.5% tea tree oil, 0.2% pentaerythritol tetraisostearate;

[0050] Acaricide: 1% cross-linked cyclodextrin-coated modified sulfur;

[0051] Thickener: 0.15% methyl methacrylate / ethylene glycol dimethacrylate crosspolymer;

[0052] Preservative: 0.1% phenoxyethanol;

[0053] Fragrance: 0.1%;

[0054] Water: Balance.

[0055] The preparation method of the cross-linked cyclodextrin-coated modified sulfur is as follows:

[0056] 50g of β-cyclodextrin was added to 500g of sodium hydroxide aqueous solution with pH 12 and heated to 75℃ to dissolve. Then, 0.25g of pentaerythritol glycidyl ether crosslinking agent and 100g of sulfur powder were added and stirred until homogeneous. The etherification and crosslinking reaction was carried out at 70℃ with stirring for 4h until the epoxy groups were completely reacted. After the reaction was completed, hydrochloric acid was added to neutralize to neutral, and the mixture was cooled to room temperature. 500g of ethanol was added to disperse the mixture. The mixture was then vacuum filtered, and the solid product was washed with cold water and vacuum dried to obtain crosslinked cyclodextrin-coated modified sulfur.

[0057] The preparation method of the highly stable sulfur anti-mite liquid soap is the same as that in Example 1.

[0058] The high-stability sulfur-based anti-mite liquid soap obtained in this embodiment has a viscosity of 4120 mPa·s and no obvious sulfur odor.

[0059] The high-stability sulfur-based anti-mite liquid soap obtained in this embodiment showed no sulfur precipitation in both the centrifugal stability test (centrifuged at 3000 r / min for 30 min) and the accelerated storage stability test (accelerated test in a 42℃ constant temperature chamber for 14 days, followed by centrifugation at 3000 r / min for 30 min), indicating good product stability.

[0060] The high-stability sulfur anti-mite liquid soap obtained in this embodiment was tested for its anti-mite effect (using genuine leather fabric washed with the liquid soap as the test sample and genuine leather fabric washed with distilled water as the control sample, and the anti-mite effect was evaluated with reference to the mite inhibition rate in GB / T 24253-2009). The results showed that the anti-mite inhibition rate was 81%, and the product has a strong anti-mite effect.

[0061] Example 3

[0062] A highly stable sulfur-based anti-mite liquid soap has the following raw material composition:

[0063] Natural soap base: 15% sodium palmitate;

[0064] Auxiliary surfactants: 1% sodium cocoyl glutamate, 1% sodium lauroyl sarcosinate;

[0065] Skin conditioning agent: 10% glycerin, 1% jojoba oil, 0.5% lavender essential oil, 0.2% pentaerythritol tetraisostearate;

[0066] Acaricide: 5% cross-linked cyclodextrin-coated modified sulfur;

[0067] Thickener: 0.05% lauryl methacrylate / ethylene glycol dimethacrylate crosspolymer;

[0068] Preservative: 0.1% phenoxyethanol;

[0069] Fragrance: 0.05%;

[0070] Water: Balance.

[0071] The preparation method of the cross-linked cyclodextrin-coated modified sulfur is as follows:

[0072] 50g of β-cyclodextrin was added to 500g of sodium hydroxide aqueous solution with pH 12 and heated to 75℃ to dissolve. Then, 1g of pentaerythritol glycidyl ether crosslinking agent and 200g of sulfur powder were added and stirred until homogeneous. The etherification crosslinking reaction was carried out at 70℃ with stirring for 4h until the epoxy groups were completely reacted. After the reaction was completed, hydrochloric acid was added to neutralize to neutral, and the mixture was cooled to room temperature. 500g of ethanol was added to disperse the mixture. The mixture was then vacuum filtered, and the solid product was washed with cold water and vacuum dried to obtain crosslinked cyclodextrin-coated modified sulfur.

[0073] The preparation method of the highly stable sulfur anti-mite liquid soap is the same as that in Example 1.

[0074] The high-stability sulfur-based anti-mite liquid soap obtained in this embodiment has a viscosity of 3760 mPa·s and no obvious sulfur odor.

[0075] The high-stability sulfur-based anti-mite liquid soap obtained in this embodiment showed no sulfur precipitation in both the centrifugal stability test (centrifuged at 3000 r / min for 30 min) and the accelerated storage stability test (accelerated test in a 42℃ constant temperature chamber for 14 days, followed by centrifugation at 3000 r / min for 30 min), indicating good product stability.

[0076] The high-stability sulfur anti-mite liquid soap obtained in this embodiment was tested for its anti-mite effect (using genuine leather fabric washed with the liquid soap as the test sample and genuine leather fabric washed with distilled water as the control sample, and the anti-mite effect was evaluated with reference to the mite inhibition rate in GB / T 24253-2009). The results showed that the anti-mite inhibition rate was 86%, and the product has a strong anti-mite effect.

[0077] Comparative Example 1

[0078] A sulfur-based anti-mite liquid soap, compared to Example 1, uses unmodified sulfur powder instead of cross-linked cyclodextrin-coated modified sulfur as the anti-mite agent, otherwise the same.

[0079] The sulfur-based anti-mite liquid soap obtained in this comparative example has a viscosity of 3680 mPa·s and a distinct sulfur odor.

[0080] The sulfur-based anti-mite liquid soap obtained in this comparative example showed significant sulfur precipitation in both centrifugal stability tests and accelerated storage stability tests, indicating poor product stability.

[0081] The sulfur-based anti-mite liquid soap obtained in this comparative example showed an anti-mite inhibition rate of 87% in the anti-mite effect test, indicating that the product has a strong anti-mite effect.

[0082] Comparative Example 2

[0083] A sulfur-based anti-mite liquid soap, compared to Example 1, uses cyclodextrin-coated modified sulfur instead of cross-linked cyclodextrin-coated modified sulfur as the anti-mite agent, otherwise remains the same. The preparation method of the cyclodextrin-coated modified sulfur is as follows:

[0084] 50g of β-cyclodextrin was added to 500g of sodium hydroxide aqueous solution with pH 12 and heated to 75℃ to dissolve. Then, 150g of sulfur powder was added and stirred until homogeneous. The adsorption reaction was carried out at 70℃ with stirring for 4h. Then, hydrochloric acid was added to neutralize to neutral, and the mixture was cooled to room temperature. 500g of ethanol was added to disperse the mixture. The mixture was then vacuum filtered, and the solid product was washed with cold water and vacuum dried to obtain cyclodextrin-coated modified sulfur.

[0085] The sulfur-based anti-mite liquid soap obtained in this comparative example has a viscosity of 4200 mPa·s and no obvious sulfur odor.

[0086] The sulfur-containing anti-mite liquid soap obtained in this comparative example showed no sulfur precipitation in the centrifugal stability test, but the accelerated storage stability test showed obvious sulfur precipitation, indicating poor product storage stability.

[0087] The sulfur-based anti-mite liquid soap obtained in this comparative example showed an anti-mite inhibition rate of 85% in the anti-mite effect test, indicating that the product has a strong anti-mite effect.

[0088] Comparative Example 3

[0089] A sulfur-based anti-mite liquid soap, compared to Example 1, uses commercially available colloidal sulfur raw material (sulfur coated with gum arabic) instead of cross-linked cyclodextrin-coated modified sulfur as the anti-mite agent, while the rest are the same.

[0090] The sulfur-containing anti-mite liquid soap obtained in this comparative example showed no sulfur precipitation in the centrifugal stability test, but the accelerated storage stability test showed obvious sulfur precipitation, indicating poor product storage stability.

[0091] The above embodiments are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above embodiments. Any changes, modifications, substitutions, combinations, or simplifications made without departing from the spirit and principle of the present invention shall be considered equivalent substitutions and shall be included within the protection scope of the present invention.

Claims

1. A highly stable sulfur-based anti-mite liquid soap, characterized in that, Includes the following raw material components by weight percentage: Natural soap base 6-15%, auxiliary surfactant 2-10%, skin conditioning agent 5-15%, cross-linked cyclodextrin-coated modified sulfur 1-5%, thickener 0.05-0.2%, preservative 0.05-0.5%, fragrance 0.05-0.2%, balance water; The preparation method of the cross-linked cyclodextrin-coated modified sulfur is as follows: Cyclodextrin was added to an alkaline aqueous solution and heated to dissolve. Then, pentaerythritol glycidyl ether crosslinking agent and sulfur powder were added and stirred until homogeneous. The etherification and crosslinking reaction was carried out at 40-80℃ under stirring conditions until the epoxy groups were completely reacted. After the reaction was completed, acid was added to neutralize, and the mixture was cooled to room temperature. Ethanol was added to disperse the mixture, and the mixture was filtered. The solid product was washed and dried to obtain crosslinked cyclodextrin-coated modified sulfur. The amount of the pentaerythritol glycidyl ether crosslinking agent added is 0.2-2% of the mass of cyclodextrin; the amount of the sulfur powder added is 1-4 times the mass of cyclodextrin.

2. The highly stable sulfur-based anti-mite liquid soap according to claim 1, characterized in that, The natural soap base is one or more of sodium oleate, sodium cocoate, and sodium palmitate; the auxiliary surfactant is one or more of cocamidopropyl betaine, fatty alcohol polyoxyethylene ether sulfate, sodium lauroyl amphoteric acetate, alkyl glycoside, cocoyl glutamate, cocoyl glycinate, lauroyl glutamate, myristoyl glutamate, and lauroyl sarcosine.

3. The highly stable sulfur-based anti-mite liquid soap according to claim 1, characterized in that, The skin conditioning agent is one or more of the following: glycerin, vegetable oil, plant extract, hydroxystearic acid, ethylene glycol stearate, hydrogenated castor oil hydroxystearate, pentaerythritol tetraisostearate, and cationic starch.

4. The highly stable sulfur-based anti-mite liquid soap according to claim 1, characterized in that, The thickener is one or two of methyl methacrylate / ethylene glycol dimethacrylate crosspolymer and lauryl methacrylate / ethylene glycol dimethacrylate crosspolymer; the preservative is phenoxyethanol.

5. The highly stable sulfur-based anti-mite liquid soap according to claim 1, characterized in that, The cyclodextrin is β-cyclodextrin.

6. The highly stable sulfur-based anti-mite liquid soap according to claim 1, characterized in that, The alkaline aqueous solution is a sodium hydroxide solution with a pH value of 10-13.

7. The highly stable sulfur-based anti-mite liquid soap according to claim 1, characterized in that, The so-called acid neutralization refers to neutralizing to neutral using hydrochloric acid.

8. A method for preparing a highly stable sulfur-based anti-mite liquid soap according to any one of claims 1 to 7, characterized in that, Includes the following steps: Natural soap base, auxiliary surfactants and thickeners are added to hot water at 60~80℃ and mixed evenly to obtain an aqueous solution; then skin conditioning agents and cross-linked cyclodextrin-coated modified sulfur are added and homogenized and emulsified evenly, cooled to room temperature, and then preservatives and fragrances are added and mixed evenly, and discharged to obtain a highly stable sulfur anti-mite liquid soap.