Formula and preparation method of washing-free disinfection skin-care hand sanitizer
By combining shell polycan, cinnamin, and black grass seed extract to prepare a kind of free -to -disinfection and skin care handwashing solution, solve the problem of limited effects on skin irritation and sterilization, and achieve good sterilization and disinfection And skin care effect.
Patent Information
- Application Number
- CN202411796826.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-09
- Publication Date
- 2025-01-28
AI Technical Summary
After long-term use, existing hand sanitizer may irritate and damage the skin, and its sterilization effect is limited, making it difficult to meet the multiple needs of skin care and disinfection.
采用壳聚糖、肉桂醛和黑种草籽提取液作为主要成分，通过改性壳聚糖和黑种草籽提取液的结合，制备出一种免洗消毒护肤洗手液。
After use, this hand washing fluid will form a moisturizing skin care film, which has good sterilization and disinfection performance and skin care effect, and the cost is low, practical and efficient.
Smart Images
Figure BDA0005176951490000031 
Figure BDA0005176951490000032 
Figure BDA0005176951490000033
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of hand sanitizers, in particular to a formula and a preparation method of a wash-free disinfecting skin-care hand sanitizer. Background Art
[0002] As a product of market development, hand sanitizer is a new type of hand cleaning product. Traditional hand sanitizers need to be bubbled with water and then rinsed with water during use. However, in the absence of water, the use of traditional hand sanitizers is limited. At this time, the emergence of wash-free hand sanitizers solves the problem of water shortage. It does not require water when used, eliminates the steps of bubbling and rinsing, and has the advantages of convenience, safety, and practicality.
[0003] However, with the maturity of production technology, hand sanitizer is no longer limited to simple cleaning and decontamination. Adding special ingredients to hand sanitizer can make hand sanitizer have multiple functions such as skin care, sterilization and disinfection. Ordinary hand sanitizers use a large amount of ethanol to inhibit bacteria, but long-term use will irritate and damage the skin, making the skin of the hands rough and accompanied by a strong irritating odor. Therefore, how to improve the skin care effect of hand sanitizer is a hot topic of research.
[0004] Chitosan is also known as deacetylated chitin, which is obtained by deacetylation of chitin widely present in nature, and has good biocompatibility, adsorption, antibacterial properties, etc., and is widely used in the fields of biomaterials, pharmaceutical product research and development, antibacterial fiber preparation, etc. Cinnamaldehyde is a natural plant essential oil with excellent physiological activities such as antibacterial, antioxidant, and antiviral, but it is highly volatile, which seriously limits its application in medicine, food, and agricultural production. Nigella sativa seed is a commonly used medicinal material for Xinjiang Uygur and Xishuangbanna Dai, and its nature and flavor are sweet, pungent, and warm, and it has the effects of antioxidation, anticancer, and blood circulation, and it is low in cost, practical and efficient. The present invention uses the antibacterial effect of chitosan, cinnamaldehyde, and Nigella sativa seed, combined with the preparation process of disposable hand sanitizer, to prepare a hand sanitizer for antibacterial and skin care. Summary of the invention
[0005] 1. Technical issues to be resolved
[0006] In view of the deficiencies in the prior art, the present invention provides a formula and a preparation method of a wash-free disinfecting skin-care hand soap, and the prepared hand soap has good bactericidal and disinfecting performance and skin-care performance.
[0007] (II) Technical solution
[0008] A formula of a wash-free disinfecting skin-care hand sanitizer, the formula of the wash-free disinfecting skin-care hand sanitizer consisting of the following components in percentage by mass: 1-5% of carbomer, 2-3% of Tween 80, 2-5% of coconut oil diethanolamide, 1-4% of dodecyl dimethyl betaine, 1-4% of glycerol, 10-20% of alcohol, 2-10% of dicinnamaldehyde-modified chitosan, 5-20% of black cumin seed extract, 0.2-0.8% of citric acid, and the balance being deionized water;
[0009] The preparation method of the wash-free disinfecting skin care hand sanitizer is as follows:
[0010] Carbomer is added to deionized water, stirred and dispersed, Tween 80, coconut acid diethanolamide, dodecyl dimethyl betaine, glycerin and alcohol are added thereto and stirred and mixed evenly, citric acid, dicinnamaldehyde modified chitosan and black cumin seed extract are added thereto, stirred and mixed evenly to obtain a wash-free disinfecting skin care hand soap.
[0011] Further preferably, the preparation method of the black cumin seed extract is as follows:
[0012] (1) Drying and crushing black cumin seeds, placing them in a conical flask, adding 50-70% ethanol, performing ultrasonic extraction in a 150W ultrasonic cleaner for 20-50 minutes, and centrifuging to obtain a filtrate 1 and a residue 1;
[0013] (2) adding the residue 1 to a Soxhlet extractor, adding 80-85% ethanol thereto, reflux at 80° C. for 10-15 h, and filtering with suction to obtain a filtrate 2 and a residue 2;
[0014] (3) Filtrate 1 and filtrate 2 are mixed and dried to obtain a black cumin seed extract.
[0015] Further preferably, the preparation method of the dicinnamaldehyde modified chitosan is as follows:
[0016] S1. Add diethylenetriamine and potassium hydroxide to an ethanol solvent, stir and dissolve, add cinnamaldehyde thereto, react at 55-70°C for 4-7h, and after the reaction is completed, cool to room temperature, filter, wash with ether, and dry to obtain intermediate 1. The reaction route is:
[0017]
[0018] S2, adding intermediate 1 and epichlorohydrin to ethanol solvent, stirring and dispersing, heating to 75-90°C, adding sodium hydroxide, and continuing the reaction for 10-16h. After the reaction is completed, standing and stratifying, the lower layer of liquid is distilled under reduced pressure, recrystallized from ethanol, and dried to obtain intermediate 2. The reaction route is:
[0019]
[0020] S3, adding intermediate 2 and chitosan to isopropanol solvent, stirring and dispersing, reacting at 80-90°C for 10-24h, cooling to room temperature after the reaction, washing with deionized water, vacuum filtering, purifying, and drying to obtain dicinnamaldehyde-modified chitosan, the reaction route is:
[0021]
[0022] Further preferably, in S1, the usage ratio of diethylenetriamine, potassium hydroxide and cinnamaldehyde is 1 mol:(2-2.5) mol:(2.5-3) mol.
[0023] Further preferably, in S2, the usage ratio of intermediate 1, epichlorohydrin and sodium hydroxide is 1 mol:(1-1.5) mol:(1-1.5) mol.
[0024] Further preferably, in S3, the usage ratio of the intermediate 2 and chitosan is 0.05-0.1 mol:1 g.
[0025] (III) Beneficial technical effects
[0026] Reaction mechanism: The present invention extracts black cumin seeds twice to obtain black cumin seeds extract, and the two extractions improve the utilization rate of black cumin seeds. Diethylenetriamine and cinnamaldehyde are condensed by aldehyde amine to obtain intermediate 1, and intermediate 1 is substituted with epichlorohydrin to obtain intermediate 2, which has a novel structure and a simple preparation method. The epoxy group contained in intermediate 2 is used to react with the amino group of chitosan to perform a ring-opening reaction to obtain di-cinnamaldehyde-modified chitosan. Finally, carbomer, di-cinnamaldehyde-modified chitosan, black cumin seeds extract, etc. are added to deionized water, stirred and dispersed, and a wash-free disinfecting skin care hand soap is obtained.
[0027] The cinnamaldehyde used in the present invention is volatile itself, and the present invention grafts it into chitosan to reduce its volatility, and both have good antibacterial properties. The single antibacterial component is limited. The present invention combines the two to produce a good antibacterial synergistic effect. The hand sanitizer prepared thereby will form a thin film on the surface of both hands after use, and has the effect of moisturizing and skin care. The present invention uses low-cost black seed, and obtains black seed extract after two extractions. The wash-free hand sanitizer prepared by the black seed extract and the dicinnamaldehyde modified chitosan has good disinfection and antibacterial effects, and has low irritation, natural skin care, safety and health. The wash-free hand sanitizer prepared by the present invention has good sterilization and disinfection effects and skin care effects. DETAILED DESCRIPTION
[0028] It should be understood that the terms described in the present invention are only for describing special embodiments and are not intended to limit the present invention. In addition, for the numerical range in the present invention, it should be understood that each intermediate value between the upper and lower limits of the scope is also specifically disclosed. Each smaller range between the intermediate value in any stated value or stated range and any other stated value or intermediate value in the described range is also included in the present invention. The upper and lower limits of these smaller ranges can be independently included or excluded in the scope.
[0029] Example 1
[0030] (1) Dry and crush the black cumin seeds, put them into a conical flask, add 50% ethanol, perform ultrasonic extraction in a 150W ultrasonic cleaner for 50 minutes, and centrifuge to obtain a filtrate 1 and a residue 1.
[0031] (2) The residue 1 was added to a Soxhlet extractor, to which 85% ethanol was added, and the mixture was refluxed at 80° C. for 12 h. The mixture was filtered to obtain a filtrate 2 and a residue 2.
[0032] (3) Filtrate 1 and filtrate 2 are mixed and dried to obtain a black cumin seed extract.
[0033] (4) 0.1 mol of diethylenetriamine and 0.24 mol of potassium hydroxide were added to an ethanol solvent and stirred to dissolve. 0.3 mol of cinnamaldehyde was added thereto and reacted at 60° C. for 5 h. After the reaction was completed, the mixture was cooled to room temperature, filtered, washed with ether, and dried to obtain intermediate 1.
[0034] (5) 80 mmol of intermediate 1 and 100 mmol of epichlorohydrin were added to an ethanol solvent, stirred and dispersed, and the temperature was raised to 80° C. 100 mmol of sodium hydroxide was added thereto, and the reaction was continued for 15 h. After the reaction was completed, the mixture was allowed to stand and separate into layers. The lower layer of liquid was distilled under reduced pressure, recrystallized from ethanol, and dried to obtain intermediate 2.
[0035] (6) 0.25 mol of the intermediate 2 and 5 g of chitosan were added to isopropanol solvent, stirred and dispersed, and reacted at 85° C. for 24 h. After the reaction was completed, the mixture was cooled to room temperature, washed with deionized water, vacuum filtered, purified, and dried to obtain dicinnamaldehyde-modified chitosan.
[0036] (7) 3 g of carbomer was added to 61.8 g of deionized water, and the mixture was stirred and dispersed. Then, 3 g of Tween 80, 2 g of coconut oil diethanolamide, 2 g of dodecyl dimethyl betaine, 1 g of glycerol, and 20 g of alcohol were added and mixed evenly. Then, 0.2 g of citric acid, 2 g of dicinnamaldehyde-modified chitosan, and 5 g of black cumin seed extract were added and mixed evenly to obtain a wash-free disinfectant skin care hand soap.
[0037] Example 2
[0038] (1) Dry and crush the black cumin seeds, put them into a conical flask, add 70% ethanol, perform ultrasonic extraction for 30 minutes in a 150W ultrasonic cleaner, and centrifuge to obtain a filtrate 1 and a residue 1.
[0039] (2) The residue 1 was added to a Soxhlet extractor, to which 80% ethanol was added, and the mixture was refluxed at 80° C. for 15 h. The mixture was filtered to obtain a filtrate 2 and a residue 2.
[0040] (3) Filtrate 1 and filtrate 2 are mixed and dried to obtain a black cumin seed extract.
[0041] (4) 0.1 mol of diethylenetriamine and 0.2 mol of potassium hydroxide were added to an ethanol solvent and stirred to dissolve. 0.3 mol of cinnamaldehyde was added thereto and reacted at 60° C. for 7 h. After the reaction was completed, the mixture was cooled to room temperature, filtered, washed with ether, and dried to obtain intermediate 1.
[0042] (5) 80 mmol of intermediate 1 and 80 mmol of epichlorohydrin were added to an ethanol solvent, stirred and dispersed, and the temperature was raised to 75° C. 120 mmol of sodium hydroxide was added thereto, and the reaction was continued for 12 h. After the reaction was completed, the mixture was allowed to stand and the layers were separated. The lower layer of liquid was distilled under reduced pressure, recrystallized from ethanol, and dried to obtain intermediate 2.
[0043] (6) 0.3 mol of the intermediate 2 and 5 g of chitosan were added to isopropanol solvent, stirred and dispersed, and reacted at 90° C. for 10 h. After the reaction was completed, the mixture was cooled to room temperature, washed with deionized water, vacuum filtered, purified, and dried to obtain dicinnamaldehyde-modified chitosan.
[0044] (7) 1 g of carbomer was added to 56.8 g of deionized water, and the mixture was stirred and dispersed. Then, 2 g of Tween 80, 4 g of coconut oil diethanolamide, 4 g of dodecyl dimethyl betaine, 2 g of glycerol, and 15 g of alcohol were added and the mixture was stirred and mixed uniformly. Then, 0.2 g of citric acid, 5 g of dicinnamaldehyde-modified chitosan, and 10 g of black cumin seed extract were added and the mixture was stirred and mixed uniformly to obtain a wash-free disinfecting skin care hand soap.
[0045] Example 3
[0046] (1) Dry and crush the black cumin seeds, put them into a conical flask, add 60% ethanol, perform ultrasonic extraction in a 150W ultrasonic cleaner for 20 minutes, and centrifuge to obtain a filtrate 1 and a residue 1.
[0047] (2) The residue 1 was added to a Soxhlet extractor, to which 80% ethanol was added, and the mixture was refluxed at 80° C. for 12 h. The mixture was filtered to obtain a filtrate 2 and a residue 2.
[0048] (3) Filtrate 1 and filtrate 2 are mixed and dried to obtain a black cumin seed extract.
[0049] (4) 0.1 mol of diethylenetriamine and 0.24 mol of potassium hydroxide were added to an ethanol solvent and stirred to dissolve. 0.25 mol of cinnamaldehyde was added thereto and reacted at 70° C. for 6 h. After the reaction was completed, the mixture was cooled to room temperature, filtered, washed with ether, and dried to obtain intermediate 1.
[0050] (5) 80 mmol of intermediate 1 and 120 mmol of epichlorohydrin were added to an ethanol solvent, stirred and dispersed, and the temperature was raised to 80° C. 100 mmol of sodium hydroxide was added thereto, and the reaction was continued for 10 h. After the reaction was completed, the mixture was allowed to stand and separate into layers. The lower layer of liquid was distilled under reduced pressure, recrystallized from ethanol, and dried to obtain intermediate 2.
[0051] (6) 0.4 mol of the intermediate 2 and 5 g of chitosan were added to isopropanol solvent, stirred and dispersed, and reacted at 85° C. for 12 h. After the reaction was completed, the mixture was cooled to room temperature, washed with deionized water, vacuum filtered, purified, and dried to obtain dicinnamaldehyde-modified chitosan.
[0052] (7) 5 g of carbomer was added to 50.2 g of deionized water, stirred and dispersed, and then 2 g of Tween 80, 5 g of coconut oil diethanolamide, 1 g of dodecyl dimethyl betaine, 3 g of glycerol, and 10 g of alcohol were added thereto and stirred and mixed evenly, and then 0.8 g of citric acid, 8 g of dicinnamaldehyde-modified chitosan, and 15 g of black cumin seed extract were added thereto and stirred and mixed evenly to obtain a wash-free disinfecting skin care hand soap.
[0053] Example 4
[0054] (1) Dry and crush the black cumin seeds, put them into a conical flask, add 60% ethanol, perform ultrasonic extraction in a 150W ultrasonic cleaner for 40 minutes, and centrifuge to obtain a filtrate 1 and a residue 1.
[0055] (2) The residue 1 was added to a Soxhlet extractor, to which 85% ethanol was added, and the mixture was refluxed at 80° C. for 10 h. The mixture was filtered to obtain a filtrate 2 and a residue 2.
[0056] (3) Filtrate 1 and filtrate 2 are mixed and dried to obtain a black cumin seed extract.
[0057] (4) 0.1 mol of diethylenetriamine and 0.25 mol of potassium hydroxide were added to an ethanol solvent and stirred to dissolve. 0.28 mol of cinnamaldehyde was added thereto and reacted at 55° C. for 4 h. After the reaction was completed, the mixture was cooled to room temperature, filtered, washed with ether, and dried to obtain intermediate 1.
[0058] (5) 80 mmol of intermediate 1 and 100 mmol of epichlorohydrin were added to an ethanol solvent, stirred and dispersed, and the temperature was raised to 90° C. 80 mmol of sodium hydroxide was added thereto, and the reaction was continued for 16 hours. After the reaction was completed, the mixture was allowed to stand and separate into layers. The lower layer of liquid was distilled under reduced pressure, recrystallized from ethanol, and dried to obtain intermediate 2.
[0059] (6) 0.5 mol of the intermediate 2 and 5 g of chitosan were added to isopropanol solvent, stirred and dispersed, and reacted at 80° C. for 24 h. After the reaction was completed, the mixture was cooled to room temperature, washed with deionized water, vacuum filtered, purified, and dried to obtain dicinnamaldehyde-modified chitosan.
[0060] (7) 4 g of carbomer was added to 42 g of deionized water, stirred and dispersed, and then 2.5 g of Tween 80, 4 g of coconut oil diethanolamide, 3 g of dodecyl dimethyl betaine, 4 g of glycerol, and 10 g of alcohol were added thereto and stirred and mixed evenly, and then 0.5 g of citric acid, 10 g of dicinnamaldehyde-modified chitosan, and 20 g of black cumin seed extract were added thereto and stirred and mixed evenly to obtain a wash-free disinfecting skin care hand soap.
[0061] Comparative Example 1
[0062] The difference between this comparative example and Example 1 is that in step (7), no dicinnamaldehyde-modified chitosan is contained.
[0063] Comparative Example 2
[0064] The difference between this comparative example and Example 1 is that in step (7), no black cumin seed extract is contained.
[0065] Take a sterile small round filter paper with a diameter of 6 mm, soak it in hand sanitizer, pick out a single clone of Escherichia coli, culture it in LB liquid culture medium for 40 minutes, spread it on a solid culture medium plate, then place the filter paper on the solid culture medium plate, culture it at 37°C for 12 hours, and measure the size of the inhibition zone of the small round piece on the plate.
[0066] Table 1:
[0067]
[0068]
[0069] It can be seen from the table that the hand sanitizer prepared by the present invention has good bactericidal and disinfecting effects.
[0070] 30 healthy people were randomly selected to score various indicators of hand sanitizer. The higher the score, the better the effect.
[0071] Table 2:
[0072] Moisturizing(50) Moisturizing Skin Care(50) Example 1 (average score) 41 45 Example 2 (average score) 43 47 Example 3 (average score) 47 49 Example 4 (average score) 45 46 Comparative Example 1 (average score) 39 40 Comparative Example 2 (average score) 34 38
[0073] It can be seen from the table that the hand washing liquid prepared by the present invention has good moisturizing and skin care effects.
[0074] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions and improvements made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims
1. A formula for a wash-free disinfectant skin care hand soap, characterized in that: The formula of the wash-free disinfecting skin care hand soap is composed of the following components in percentage by mass: 1-5% of carbomer, 2-3% of Tween 80, 2-5% of coconut oil diethanolamide, 1-4% of dodecyl dimethyl betaine, 1-4% of glycerol, 10-20% of alcohol, 2-10% of dicinnamaldehyde modified chitosan, 5-20% of black cumin seed extract, 0.2-0.8% of citric acid, and the balance is deionized water, and the sum of the percentages of the above components is 100%; The preparation method of the wash-free disinfecting skin care hand sanitizer is as follows: Carbomer is added to deionized water, stirred and dispersed, Tween 80, coconut acid diethanolamide, dodecyl dimethyl betaine, glycerin and alcohol are added thereto and stirred and mixed evenly, citric acid, dicinnamaldehyde modified chitosan and black cumin seed extract are added thereto, stirred and mixed evenly to obtain a wash-free disinfecting skin care hand soap.
2. The formula of the wash-free disinfecting skin care hand soap according to claim 1, characterized in that: The preparation method of the black cumin seed extract is as follows: (1) Drying and crushing black cumin seeds, placing them in a conical flask, adding 50-70% ethanol, performing ultrasonic extraction in a 150W ultrasonic cleaner for 20-50 minutes, and centrifuging to obtain a filtrate 1 and a residue 1; (2) adding the residue 1 to a Soxhlet extractor, adding 80-85% ethanol thereto, reflux at 80° C. for 10-15 h, and filtering with suction to obtain a filtrate 2 and a residue 2; (3) Filtrate 1 and filtrate 2 are mixed and dried to obtain a black cumin seed extract.
3. The formula of the wash-free disinfecting skin care hand soap according to claim 1, characterized in that: The preparation method of the dicinnamaldehyde modified chitosan is as follows: S1, adding diethylenetriamine and potassium hydroxide to an ethanol solvent, stirring to dissolve, adding cinnamaldehyde thereto, reacting at 55-70°C for 4-7h, after the reaction is completed, cooling to room temperature, filtering, washing with ether, and drying to obtain intermediate 1; S2, adding intermediate 1 and epichlorohydrin to ethanol solvent, stirring and dispersing, heating to 75-90°C, adding sodium hydroxide thereto, and continuing the reaction for 10-16 hours. After the reaction is completed, standing and stratifying, distilling the lower layer of liquid under reduced pressure, recrystallizing from ethanol, and drying to obtain intermediate 2; S3. Add intermediate 2 and chitosan to isopropanol solvent, stir and disperse, react at 80-90°C for 10-24h. After the reaction is completed, cool to room temperature, wash with deionized water, vacuum filter, purify, and dry to obtain dicinnamaldehyde-modified chitosan.
4. The formula of the wash-free disinfecting skin care hand soap according to claim 3, characterized in that: In the S1, the usage ratio of diethylenetriamine, potassium hydroxide and cinnamaldehyde is 1 mol:(2-2.5) mol:(2.5-3) mol.
5. The formula of the wash-free disinfecting skin care hand soap according to claim 3, characterized in that: In S2, the usage ratio of intermediate 1, epichlorohydrin and sodium hydroxide is 1 mol:(1-1.5) mol:(1-1.5) mol.
6. The formula of the wash-free disinfecting skin care hand soap according to claim 3, characterized in that: In the S3, the usage ratio of the intermediate 2 and chitosan is 0.05-0.1 mol:1 g.