High-stability sulfur mite-killing liquid soap and preparation method thereof
By surface-coating sulfur powder with cross-linked cyclodextrin, the problem of poor sulfur stability in liquid soap is solved, and liquid soap with high stability and anti-mite effect is achieved, which simplifies the preparation process and reduces costs.
Patent Information
- Application Number
- CN202510810743.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-06-17
- Publication Date
- 2025-09-19
- Estimated Expiration
- 2045-06-17
AI Technical Summary
The stability of the solid sulfur component in liquid soap is poor. Existing methods are costly and complex, making it difficult to achieve sulfur coating and modification stability in liquid soap.
Cross-linked cyclodextrin is used to modify the surface of sulfur powder by coating it. By performing an etherification cross-linking reaction on the surface of the sulfur powder, cross-linked cyclodextrin-coated modified sulfur is formed, thereby improving its stability in liquid soap formula.
The dispersion stability and anti-mite effect of sulfur in liquid soap are significantly improved. At the same time, the process is simple, environmentally friendly, reduces sulfur odor, and has low cost.
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of cosmetics, and particularly relates to a high-stability sulfur mite-removing liquid soap and a preparation method thereof. Background Art
[0002] Sulfur has certain antibacterial and anti-inflammatory properties, effectively alleviating skin problems such as acne and herpes. It can penetrate the skin, reduce inflammation, reduce redness and swelling, and promote the skin's self-repair ability. Sulfur also has strong bactericidal properties, effectively inhibiting the growth of bacteria and fungi, preventing infection and disease. Therefore, sulfur is often used as a functional ingredient in the manufacture of cosmetics and cleaning and hygiene products.
[0003] For example, Chinese patent CN 107955754 A discloses an antibacterial and mite-removing soap. By adding an antibacterial agent and sulfur, the resulting soap not only has a cleansing effect but also has antibacterial and mite-removing properties. Chinese patent CN 112251302 A discloses a perfume-type latex soap that achieves excellent antibacterial effects by adding sulfur. However, conventional solid soaps require rinsing underwater and rubbing before washing the skin, and are directly exposed to air and moisture, resulting in poor ease of use and hygiene.
[0004] Liquid soap is becoming increasingly popular with consumers because it is easier to squeeze and apply, is both hygienic and convenient. However, unlike the dispersing and stabilizing effect of soap bases on solid sulfur in solid soaps, the surfactants in liquid soaps are difficult to effectively stabilize the insoluble solid sulfur components in the liquid phase, resulting in poor stability. The existing method for improving the dispersibility of solid sulfur in liquid products is to use gum arabic for encapsulation to prepare colloidal sulfur products. However, gum arabic is highly water-soluble and easily dissolves and opens the inclusions during long-term storage of the product, causing the sulfur element to overflow, and is unable to effectively improve the storage stability in emulsion products. Chinese patent CN117898953A discloses a triple-encapsulated colloidal sulfur and its preparation method and application. By triple-encapsulating colloidal sulfur, the irritation and odor of sulfur itself can be effectively reduced, significantly improving the user experience of colloidal sulfur in cosmetic applications. However, the preparation method of this colloidal sulfur is relatively complex and costly. Summary of the Invention
[0005] The purpose of the present invention is to solve the shortcomings and deficiencies in the above-mentioned prior art and to provide a high-stability sulfur mite-removing liquid soap and a preparation method thereof.
[0006] The purpose of the present invention is achieved through the following technical solutions:
[0007] A high-stability sulfur mite-removing liquid soap comprises the following raw material components in percentage by weight:
[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%, and the balance is water;
[0009] The preparation method of the cross-linked cyclodextrin-coated modified sulfur is as follows:
[0010] Cyclodextrin is added to an alkaline aqueous solution and heated to dissolve, and then pentaerythritol glycidyl ether cross-linking agent and sulfur powder are added and stirred to mix evenly, and an etherification cross-linking reaction is carried out at a temperature of 40 to 80° C. and under stirring conditions until the epoxy groups react completely. After the reaction is completed, acid is added for neutralization, and the mixture is cooled to room temperature, and ethanol is added for dispersion. The solid phase product is filtered, washed, and dried to obtain cross-linked cyclodextrin-coated modified sulfur.
[0011] The preparation principle of the cross-linked cyclodextrin-coated modified sulfur of the present invention is to utilize the binding effect of the polar hydroxyl groups of cyclodextrin with sulfur powder and the reduced solubility of the cyclodextrin in water after cross-linking with pentaerythritol glycidyl ether. After the etherification and cross-linking reaction, the cross-linked cyclodextrin is precipitated in situ on the surface of the sulfur powder, thereby achieving the coating modification of the sulfur powder. The surface-modified sulfur powder significantly improves its compatibility with surfactants, skin conditioners, and thickeners in liquid soap formulations, thereby enhancing dispersion stability. Furthermore, the solubility of the cross-linked cyclodextrin is reduced, thereby achieving better coating stability.
[0012] Furthermore, the natural soap base is one or more of sodium olivetate, sodium cocoate, and sodium palmitate.
[0013] Furthermore, the auxiliary surfactant is one or more of cocamidopropyl betaine, fatty alcohol polyoxyethylene ether sulfate, sodium lauroylamphoacetate, alkyl glucoside, cocoyl glutamate, cocoyl glycinate, lauroyl glutamate, myristoyl glutamate, and lauroyl sarcosinate.
[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 cross-linked polymer and lauryl methacrylate / ethylene glycol dimethacrylate cross-linked polymer.
[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 added amount of the pentaerythritol glycidyl ether cross-linking agent is 0.2-2% of the mass of the cyclodextrin.
[0020] The added amount of the sulfur powder is 1 to 4 times the mass of the cyclodextrin.
[0021] The acid-adding neutralization refers to neutralization to neutrality with hydrochloric acid.
[0022] The preparation method of the above-mentioned high-stability sulfur mite-removing liquid soap comprises the following steps:
[0023] Add natural soap base, auxiliary surfactant and thickener into hot water at 60-80°C and mix evenly to obtain an aqueous phase solution; then add skin conditioner and cross-linked cyclodextrin-coated modified sulfur and homogenize and emulsify evenly, cool to room temperature, add preservative and fragrance and mix evenly, and discharge to obtain a high-stability sulfur mite-removing liquid soap.
[0024] Compared with the prior art, the present invention has the following beneficial effects:
[0025] (1) The present invention uses cross-linked cyclodextrin to carry out surface coating modification on sulfur powder, which can significantly improve its stability in liquid soap formula and ensure good anti-mite effect.
[0026] (2) The preparation method of the cross-linked cyclodextrin-coated modified sulfur of the present invention is simple in process, does not use toxic or harmful reagents, and is green and environmentally friendly. DETAILED DESCRIPTION
[0027] The present invention will be further described in detail below with reference to examples, but the embodiments of the present invention are not limited thereto.
[0028] Example 1
[0029] A high-stability sulfur mite-removing liquid soap, the raw material composition ratio of which is as follows:
[0030] Natural soap base: sodium olivetate 10%;
[0031] Auxiliary surfactants: cocamidopropyl betaine 4%, sodium fatty alcohol polyoxyethylene ether sulfate 2%, sodium lauroyl sarcosinate 1%;
[0032] Skin Conditioning Agents: Glycerin 6%, Olive Oil 1%, Aloe Vera Extract 0.5%, Hydrogenated Castor Oil Hydroxystearate 0.2%;
[0033] Mite remover: cross-linked cyclodextrin coated modified sulfur 3%;
[0034] Thickener: Methyl methacrylate / ethylene glycol dimethacrylate crosspolymer 0.1%;
[0035] Preservative: Phenoxyethanol 0.1%;
[0036] Fragrance: 0.1%;
[0037] Water: Balance.
[0038] The preparation method of the cross-linked cyclodextrin-coated modified sulfur is as follows:
[0039] 50 g of β-cyclodextrin was added to 500 g of sodium hydroxide aqueous solution with a pH value of 12 and heated to 75° C. to dissolve. Then, 0.5 g of pentaerythritol glycidyl ether crosslinking agent and 150 g of sulfur powder were added and stirred to mix evenly. The etherification crosslinking reaction was carried out at 70° C. with stirring for 4 h until the epoxy groups reacted completely. After the reaction was completed, hydrochloric acid was added to neutralize the mixture, and the mixture was cooled to room temperature. 500 g of ethanol was added to disperse the mixture, and vacuum filtered. The solid phase product was washed with cold water and vacuum dried to obtain cross-linked cyclodextrin-coated modified sulfur.
[0040] The preparation method of the high-stability sulfur mite-removing liquid soap is as follows:
[0041] Prepare raw materials according to the percentage by mass, add natural soap base, auxiliary surfactant and thickener into 75°C hot water and mix evenly to obtain an aqueous phase solution; then add skin conditioner and mite remover and homogenize and emulsify evenly, cool to room temperature, then add preservative and fragrance and mix evenly, discharge the material to obtain a high-stability sulfur mite remover liquid soap.
[0042] The high-stability sulfur mite-removing liquid soap obtained in this example has a viscosity of 3850 mPa·s and has no obvious sulfur odor.
[0043] The high-stability sulfur mite-removing liquid soap obtained in this embodiment was subjected to a centrifugal stability test (centrifuged in a centrifuge at 3000 r / min for 30 minutes) and an accelerated storage stability test (accelerated test in a 42°C constant temperature box for 14 days, followed by centrifugation in a centrifuge at 3000 r / min for 30 minutes). The results showed that there was no sulfur precipitation, and the product stability was good.
[0044] The high-stability sulfur mite-removing liquid soap obtained in this example was tested for its anti-mite effect (using leather fabric washed with liquid soap as a test sample, and leather fabric washed with distilled water as a control sample, and evaluating the anti-mite effect with reference to the mite inhibition rate in GB / T 24253-2009). The results showed that the anti-mite inhibition rate was 85%, indicating that the product has a strong anti-mite effect.
[0045] Example 2
[0046] A high-stability sulfur mite-removing liquid soap, the raw material composition ratio of which is as follows:
[0047] Natural soap base: sodium cocoate 6%;
[0048] Auxiliary surfactants: sodium fatty alcohol polyoxyethylene ether sulfate 4%, sodium lauroyl sarcosinate 4%, alkyl glycoside 2%;
[0049] Skin Conditioning Agents: Glycerin 8%, Jojoba Oil 2%, Tea Tree Oil 0.5%, Pentaerythrityl Tetraisostearate 0.2%;
[0050] Mite remover: cross-linked cyclodextrin coated modified sulfur 1%;
[0051] Thickener: Methyl methacrylate / ethylene glycol dimethacrylate crosspolymer 0.15%;
[0052] Preservative: Phenoxyethanol 0.1%;
[0053] Fragrance: 0.1%;
[0054] Water: Balance.
[0055] The preparation method of the cross-linked cyclodextrin-coated modified sulfur is as follows:
[0056] 50 g of β-cyclodextrin was added to 500 g of sodium hydroxide aqueous solution with a pH value of 12 and heated to 75° C. to dissolve. Then, 0.25 g of pentaerythritol glycidyl ether crosslinking agent and 100 g of sulfur powder were added and stirred to mix evenly. The etherification crosslinking reaction was carried out at 70° C. with stirring for 4 h until the epoxy groups reacted completely. After the reaction was completed, hydrochloric acid was added to neutralize the mixture, and the mixture was cooled to room temperature. 500 g of ethanol was added to disperse the mixture, and vacuum filtration was performed. The solid phase product was washed with cold water and vacuum dried to obtain cross-linked cyclodextrin-coated modified sulfur.
[0057] The preparation method of the high-stability sulfur mite-removing liquid soap is the same as that in Example 1.
[0058] The high-stability sulfur mite-killing liquid soap obtained in this example has a viscosity of 4120 mPa·s and has no obvious sulfur odor.
[0059] The high-stability sulfur mite-removing liquid soap obtained in this embodiment was subjected to a centrifugal stability test (centrifuged in a centrifuge at 3000 r / min for 30 minutes) and an accelerated storage stability test (accelerated test in a 42°C constant temperature box for 14 days, followed by centrifugation in a centrifuge at 3000 r / min for 30 minutes). The results showed that there was no sulfur precipitation, and the product stability was good.
[0060] The high-stability sulfur mite-removing liquid soap obtained in this example was tested for its anti-mite effect (using leather fabric washed with liquid soap as a test sample, and leather fabric washed with distilled water as a control sample, and evaluating the anti-mite effect with reference to the mite inhibition rate in GB / T 24253-2009). The results showed that the anti-mite inhibition rate was 81%, indicating that the product has a strong anti-mite effect.
[0061] Example 3
[0062] A high-stability sulfur mite-removing liquid soap, the raw material composition ratio of which is as follows:
[0063] Natural soap base: sodium palmitate 15%;
[0064] Auxiliary surfactants: sodium cocoyl glutamate 1%, sodium lauroyl sarcosinate 1%;
[0065] Skin Conditioning Agents: Glycerin 10%, Jojoba Oil 1%, Lavender Essential Oil 0.5%, Pentaerythrityl Tetraisostearate 0.2%;
[0066] Mite remover: cross-linked cyclodextrin coated modified sulfur 5%;
[0067] Thickener: Lauryl Methacrylate / Ethylene Glycol Dimethacrylate Crosspolymer 0.05%;
[0068] Preservative: Phenoxyethanol 0.1%;
[0069] Fragrance: 0.05%;
[0070] Water: Balance.
[0071] The preparation method of the cross-linked cyclodextrin-coated modified sulfur is as follows:
[0072] 50 g of β-cyclodextrin was added to 500 g of sodium hydroxide aqueous solution with a pH value of 12 and heated to 75° C. to dissolve. Then, 1 g of pentaerythritol glycidyl ether crosslinking agent and 200 g of sulfur powder were added and stirred to mix evenly. The etherification crosslinking reaction was carried out at 70° C. with stirring for 4 h until the epoxy groups reacted completely. After the reaction was completed, hydrochloric acid was added to neutralize the mixture, and the mixture was cooled to room temperature. 500 g of ethanol was added to disperse the mixture, and vacuum filtered. The solid phase product was washed with cold water and vacuum dried to obtain cross-linked cyclodextrin-coated modified sulfur.
[0073] The preparation method of the high-stability sulfur mite-removing liquid soap is the same as that in Example 1.
[0074] The high-stability sulfur mite-killing liquid soap obtained in this example has a viscosity of 3760 mPa·s and has no obvious sulfur odor.
[0075] The high-stability sulfur mite-removing liquid soap obtained in this embodiment was subjected to a centrifugal stability test (centrifuged in a centrifuge at 3000 r / min for 30 minutes) and an accelerated storage stability test (accelerated test in a 42°C constant temperature box for 14 days, followed by centrifugation in a centrifuge at 3000 r / min for 30 minutes). The results showed that there was no sulfur precipitation, and the product stability was good.
[0076] The high-stability sulfur mite-removing liquid soap obtained in this example was tested for its anti-mite effect (using leather fabric washed with liquid soap as a test sample, and leather fabric washed with distilled water as a control sample, and evaluating the anti-mite effect with reference to the mite inhibition rate in GB / T 24253-2009). The results showed that the anti-mite inhibition rate was 86%, indicating that the product has a strong anti-mite effect.
[0077] Comparative Example 1
[0078] A sulfur mite-removing liquid soap is disclosed. Compared with Example 1, the mite-removing agent uses unmodified sulfur powder instead of cross-linked cyclodextrin-coated modified sulfur, and the rest is the same.
[0079] The sulfur mite-killing liquid soap obtained in this comparative example has a viscosity of 3680 mPa·s and a noticeable sulfur odor.
[0080] The sulfur mite-killing liquid soap obtained in this comparative example produced obvious sulfur precipitation in the centrifugal stability test and the accelerated storage stability test, and the product stability was poor.
[0081] The anti-mite effect test results of the sulfur anti-mite liquid soap obtained in this comparative example showed that the anti-mite inhibition rate was 87%, and the product had a strong anti-mite effect.
[0082] Comparative Example 2
[0083] A sulfur mite-removing liquid soap, compared with Example 1, uses cyclodextrin-coated modified sulfur instead of cross-linked cyclodextrin-coated modified sulfur, and the rest is the same. The preparation method of the cyclodextrin-coated modified sulfur is as follows:
[0084] 50 g of β-cyclodextrin was added to 500 g of sodium hydroxide aqueous solution with a pH value of 12 and heated to 75° C. to dissolve. Then, 150 g of sulfur powder was added and stirred to mix evenly. The adsorption reaction was carried out at 70° C. under stirring conditions for 4 hours. Then, hydrochloric acid was added to neutralize it, and the mixture was cooled to room temperature. 500 g of ethanol was added to disperse it, and vacuum filtration was performed. The solid phase product was washed with cold water and vacuum dried to obtain cyclodextrin-coated modified sulfur.
[0085] The sulfur mite-killing liquid soap obtained in this comparative example has a viscosity of 4200 mPa·s and has no obvious sulfur odor.
[0086] The sulfur mite-removing liquid soap obtained in this comparative example showed no sulfur precipitation after centrifugal stability test, but showed obvious sulfur precipitation in the accelerated storage stability test, indicating that the product had poor storage stability.
[0087] The anti-mite effect test results of the sulfur anti-mite liquid soap obtained in this comparative example showed that the anti-mite inhibition rate was 85%, and the product had a strong anti-mite effect.
[0088] Comparative Example 3
[0089] A sulfur mite-removing liquid soap is disclosed. Compared with Example 1, the mite-removing agent uses colloidal sulfur raw material (sulfur wrapped in gum arabic) on the market instead of cross-linked cyclodextrin-coated modified sulfur, and the rest is the same.
[0090] The sulfur mite-removing liquid soap obtained in this comparative example showed no sulfur precipitation after centrifugal stability test, but showed obvious sulfur precipitation in the accelerated storage stability test, indicating that the product had poor storage stability.
[0091] The above embodiments are preferred implementations of the present invention, but the implementations of the present invention are not limited to the above embodiments. Any other changes, modifications, substitutions, combinations, and simplifications that do not deviate from the spirit and principles of the present invention should be considered as equivalent replacement methods and are included in the scope of protection of the present invention.
Claims
1. A high-stability sulfur mite-removing liquid soap, characterized in that: The raw material components include the following percentages by weight: 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%, and the balance is water; The preparation method of the cross-linked cyclodextrin-coated modified sulfur is as follows: Cyclodextrin is added to an alkaline aqueous solution and heated to dissolve, and then pentaerythritol glycidyl ether cross-linking agent and sulfur powder are added and stirred to mix evenly, and an etherification cross-linking reaction is carried out at a temperature of 40 to 80° C. and under stirring conditions until the epoxy groups react completely. After the reaction is completed, acid is added for neutralization, and the mixture is cooled to room temperature, and ethanol is added for dispersion. The solid phase product is filtered, washed, and dried to obtain cross-linked cyclodextrin-coated modified sulfur.
2. A high-stability sulfur mite-removing liquid soap according to claim 1, characterized in that: The natural soap base is one or more of sodium olivetate, sodium cocoate, and sodium palmitate; the auxiliary surfactant is one or more of cocamidopropyl betaine, fatty alcohol polyoxyethylene ether sulfate, sodium lauroylamphoacetate, alkyl glucoside, cocoyl glutamate, cocoyl glycinate, lauroyl glutamate, myristoyl glutamate, and lauroyl sarcosinate.
3. A high-stability sulfur mite-removing liquid soap according to claim 1, characterized in that: 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.
4. A high-stability sulfur mite-removing liquid soap according to claim 1, characterized in that: The thickener is one or two of methyl methacrylate / ethylene glycol dimethacrylate cross-linked polymer and lauryl methacrylate / ethylene glycol dimethacrylate cross-linked polymer; and the preservative is phenoxyethanol.
5. A high-stability sulfur mite-killing liquid soap according to claim 1, characterized in that: The cyclodextrin is β-cyclodextrin.
6. A high-stability sulfur mite-killing liquid soap according to claim 1, characterized in that: The alkaline aqueous solution is a sodium hydroxide solution with a pH value of 10 to 13.
7. A high-stability sulfur mite-killing liquid soap according to claim 1, characterized in that: The added amount of the pentaerythritol glycidyl ether cross-linking agent is 0.2-2% of the mass of the cyclodextrin.
8. The high-stability sulfur mite-killing liquid soap according to claim 1, characterized in that: The added amount of the sulfur powder is 1 to 4 times the mass of the cyclodextrin.
9. The high-stability sulfur mite-killing liquid soap according to claim 1, characterized in that: The acid-adding neutralization refers to neutralization to neutrality with hydrochloric acid.
10. The method for preparing a high-stability sulfur mite-killing liquid soap according to any one of claims 1 to 9, characterized in that: The steps include: Add natural soap base, auxiliary surfactant and thickener into hot water at 60-80°C and mix evenly to obtain an aqueous phase solution; then add skin conditioner and cross-linked cyclodextrin-coated modified sulfur and homogenize and emulsify evenly, cool to room temperature, add preservative and fragrance and mix evenly, and discharge to obtain a high-stability sulfur mite-removing liquid soap.
Citation Information
Patent Citations
Method for preparing highly-dispersed insoluble sulphur by water-soluble polymer material coating
CN102732064A
Mite-killing liquid soap and preparation method thereof
CN115645324A