Bacteriostatic hand sanitizer and preparation method thereof

Abstract

The invention belongs to the technical field of washing and care, and particularly relates to a bacteriostatic hand sanitizer and a preparation method thereof. The hand sanitizer is prepared from the following raw materials in parts by weight: 4 to 9 parts of modified nano attapulgite, 1 to 5 parts of hail vegetable polysaccharide, 1 to 5 parts of plant essential oil, 15 to 22 parts of a surfactant, 10 to 17 parts of a humectant, 0.1 to 0.3 part of a pH regulator, 1 to 3 parts of a thickening agent and 90 to 100 parts of deionized water. The preparation process of the modified nano attapulgite comprises the following steps: S1, adding pretreated nano attapulgite into an ethanol water solution, then adding gamma-aminopropyltriethoxysilane, and stirring for reaction to obtain aminated nano attapulgite; and S2, adding the aminated attapulgite into a solvent, then adding gallic acid and triethylamine, and carrying out heating and stirring reaction to obtain the modified nano attapulgite. And the modified attapulgite can improve the stability of gallic acid in the product and reduce the irritation to skin, and has good antibacterial activity when being matched with the hail vegetable polysaccharide.

Description

Technical Field

[0001] The invention belongs to the technical field of washing and care, and particularly relates to an antibacterial hand soap and a preparation method thereof. Background Art

[0002] In daily life and medical environments, hand cleaning and disinfection are key measures to prevent cross-infection and disease transmission. Antibacterial hand sanitizers have become an indispensable personal care product due to their convenience and efficiency. However, the antibacterial properties of many commercially available antibacterial hand sanitizers will gradually decrease during long-term storage or use, affecting the use effect of the product. Therefore, the development of an antibacterial hand sanitizer with long-lasting antibacterial properties, high safety and stability has become a hot topic in current research.

[0003] At present, there are many types of antibacterial hand sanitizers on the market, and the main ingredients include surfactants, antibacterial agents, moisturizers, fragrances, etc. Among them, antibacterial agents are the key factor in determining the antibacterial effect. However, these antibacterial agents have the following problems during use: the antibacterial components in hand sanitizers may degrade under the influence of environmental factors such as temperature, resulting in a decrease in antibacterial performance. In addition, some antibacterial agents are highly irritating to the skin, and long-term use may cause skin problems.

[0004] Gallic acid is a natural antibacterial agent with a broad antibacterial spectrum, showing good inhibitory effects on a variety of bacteria, fungi and viruses. However, gallic acid itself is somewhat irritating and may cause discomfort to the skin.

[0005] The main component of attapulgite is magnesium aluminum silicate, a natural inorganic mineral. It not only has a unique chain layered structure, but also has a very high specific surface area (9.6~36m² / g) and porosity. The surface can absorb a large amount of water and other molecules, and has a good adsorption effect on heavy metal ions and organic pollutants. After attapulgite is prepared into nanoscale, the surface area of ​​the particles increases, the surface energy increases, the particles are in an unstable state, and the particle "agglomeration" phenomenon is easy to occur. This will affect its dispersibility and uniformity in other media.

[0006] Based on the above background technology, the present invention provides an antibacterial hand sanitizer and a preparation method thereof to solve the above-mentioned problems. Summary of the invention

[0007] In order to overcome the deficiencies of the prior art, the primary purpose of the present invention is to provide an antibacterial hand sanitizer.

[0008] The purpose of the present invention is achieved through the following technical solutions: An antibacterial hand soap comprises the following raw materials in parts by weight: 4-9 parts of modified nano-attapulgite, 1-5 parts of sea hail polysaccharide, 1-5 parts of plant essential oil, 15-22 parts of surfactant, 10-17 parts of moisturizer, 0.1-0.3 parts of pH regulator, 1-3 parts of thickener, and 90-100 parts of deionized water; The preparation process of the modified nano-attapulgite is as follows: S1. The pretreated nano-attapulgite is added to an ethanol aqueous solution, and then γ-aminopropyltriethoxysilane is added and stirred to react to obtain an amino-modified nano-attapulgite; S2. Add the aminated nano-attapulgite into a solvent, then add gallic acid and triethylamine, heat and stir to react, and obtain modified nano-attapulgite.

[0009] Furthermore, the mass ratio of the pretreated nano-attapulgite, γ-aminopropyltriethoxysilane, and ethanol aqueous solution in S1 is 1 g: (0.1-0.2) g: (10-15) mL.

[0010] Furthermore, the mass ratio of the amino nano-attapulgite, gallic acid and triethylamine in S2 is 1:(0.2-0.4):(0.5-0.9).

[0011] Furthermore, the temperature of the heating and stirring in S2 is 80-90° C., and the time is 1-2 h.

[0012] Furthermore, the ethanol aqueous solution described in S1 is obtained by mixing ethanol and water in a volume ratio of (3-5):1; and the solvent described in S2 is DMF.

[0013] Furthermore, the pretreatment process of the nano attapulgite in S1 is as follows: the nano attapulgite is calcined at 150-230° C. for 30 min-90 min.

[0014] Furthermore, the plant essential oil is lavender essential oil or orange essential oil; the moisturizer is any one of glycerin, propylene glycol, and polyethylene glycol; the thickener is xanthan gum or carbomer; the surfactant is cocamidopropyl betaine or dodecyl glucoside; and the pH adjuster is sodium citrate.

[0015] Another object of the present invention is to provide a method for preparing an antibacterial hand sanitizer.

[0016] The purpose of the present invention is achieved through the following technical solutions: A method for preparing an antibacterial hand sanitizer comprises the following steps: adding a surfactant and a moisturizer into water according to the weight ratio, heating and stirring, and then adding modified nano-attapulgite, salvia polysaccharide, plant essential oil, a thickener and a pH regulator and stirring evenly.

[0017] The present invention has the following effects compared with the prior art: 1. The present invention calcines the nano-attapulgite to enlarge its internal pores, then adds γ-aminopropyltriethoxysilane for amination, and then reacts it with gallic acid. The amino groups on the attapulgite react with the carboxyl groups of the gallic acid to connect the gallic acid to the amination nano-attapulgite, thereby improving the stability of the gallic acid and the dispersion uniformity of the nano-attapulgite.

[0018] 2. The present invention has proved through experiments that the combined use of modified attapulgite and sea hail polysaccharide not only improves the stability of gallic acid and reduces the irritation of gallic acid, but also enhances the antibacterial stability of hand sanitizer, providing consumers with a safer, more effective and environmentally friendly hand cleaning product.

[0019] 3. The present invention provides a method for preparing an antibacterial hand sanitizer, which is easy to operate and can be applied to industrial production. DETAILED DESCRIPTION

[0020] The present invention will be described in further detail below in conjunction with the examples, but the embodiments of the present invention are not limited thereto. Unless otherwise specified, the reagents, methods and equipment used in the present invention are conventional reagents, methods and equipment in the art. The test methods for which specific experimental conditions are not specified in the following examples are usually carried out according to conventional experimental conditions or according to the experimental conditions recommended by the manufacturer. Unless otherwise specified, the reagents and raw materials used in the present invention can be obtained commercially.

[0021] Example 1 An antibacterial hand soap comprises the following raw materials in parts by weight: 6 parts of modified nano-attapulgite, 3 parts of hyacinthus annuus polysaccharide, 3 parts of orange essential oil, 18 parts of cocamidopropyl betaine, 15 parts of glycerol, 2 parts of xanthan gum, 0.2 parts of sodium citrate, and 95 parts of deionized water; The preparation process of the modified nano-attapulgite is as follows: S1. calcining the nano-attapulgite at 200°C for 60 minutes to obtain pretreated nano-attapulgite; adding the pretreated nano-attapulgite to an ethanol aqueous solution (ethanol and water are mixed in a volume ratio of 4:1), and then adding γ-aminopropyltriethoxysilane, wherein the amount ratio of the pretreated nano-attapulgite, γ-aminopropyltriethoxysilane, and the ethanol aqueous solution is 1g:0.15g:12mL; stirring the reaction at room temperature for 2h to obtain amino-modified nano-attapulgite; S2. Add the aminated nano-attapulgite to DMF, and then add gallic acid and triethylamine, wherein the mass ratio of aminated nano-attapulgite, gallic acid and triethylamine is 1:0.2:0.8, stir and react at 85°C for 1.5h, and then filter, wash and dry to obtain modified nano-attapulgite.

[0022] The preparation process of Haihaicai polysaccharide is as follows: The seaweed is dried and then crushed, and the mixture is passed through a 50-mesh sieve to obtain seaweed powder. The seaweed powder is placed in a steam explosion instrument and subjected to a pressure treatment at 2 MPa for 1 minute to obtain treated seaweed powder. 10 times the amount of pure water is added to the treated seaweed powder, and the mixture is refluxed at 100°C for extraction for 50 minutes. After filtration, 5 times the amount of pure water is added to the filter residue, and the mixture is refluxed at 100°C for extraction for 50 minutes. The mixture is filtered again, and the filtrates obtained twice are combined. The filtrates are evaporated using a rotary evaporator and the concentrated solution is collected. Ethanol is added to the concentrated solution until the ethanol concentration is 85%, and the concentrated solution is subjected to alcohol precipitation treatment for 24 hours. The concentrated solution is centrifuged at 5000 rpm for 20 minutes, and the precipitate is crude seaweed polysaccharide. Sevage reagent is added to the crude seaweed polysaccharide for deproteinization, and the mixture is centrifuged at 5500 rpm for 15 minutes. This is repeated twice, and the mixture is concentrated and freeze-dried to obtain the obtained product.

[0023] A method for preparing an antibacterial hand sanitizer comprises the following steps: According to the above weight ratio, cocamidopropyl betaine and glycerin are added to water, heated to 50°C and stirred to mix, and modified nano-attapulgite, salvia polysaccharide, orange essential oil, xanthan gum and sodium citrate are added under heating at 50°C, and the antibacterial hand sanitizer is obtained after mixing evenly.

[0024] Example 2 An antibacterial hand soap comprises the following raw materials in parts by weight: 4 parts of modified nano-attapulgite, 1 part of salvia polysaccharide, 1 part of lavender essential oil, 15 parts of dodecyl glucoside, 10 parts of propylene glycol, 1 part of carbomer, 0.1 part of sodium citrate, and 90 parts of deionized water; The preparation process of the modified nano-attapulgite is as follows: S1. calcining the nano-attapulgite at 150°C for 90 minutes to obtain pretreated nano-attapulgite; adding the pretreated nano-attapulgite to an ethanol aqueous solution (ethanol and water are mixed in a volume ratio of 4:1), and then adding γ-aminopropyltriethoxysilane, wherein the amount of the pretreated nano-attapulgite, γ-aminopropyltriethoxysilane, and the ethanol aqueous solution is 1g:0.1g:10mL; stirring the reaction at room temperature for 2h to obtain amino-modified nano-attapulgite; S2. Add the aminated nano-attapulgite to DMF, and then add gallic acid and triethylamine, wherein the mass ratio of the aminated nano-attapulgite, gallic acid and triethylamine is 1:0.3:0.5; stir the reaction at 80°C for 2h, and then filter, wash and dry to obtain modified nano-attapulgite.

[0025] The preparation process of the polysaccharide of Aquilegia salsa is the same as that in Example 1.

[0026] A method for preparing an antibacterial hand sanitizer comprises the following steps: According to the above weight ratio, dodecyl glucoside and propylene glycol are added to water, heated to 50°C and stirred to mix, and modified nano-attapulgite, salvia polysaccharide, lavender essential oil, carbomer and sodium citrate are added under heating at 50°C, and the antibacterial hand sanitizer is obtained after mixing evenly.

[0027] Example 3 An antibacterial hand soap comprises the following raw materials in parts by weight: 9 parts of modified nano-attapulgite, 5 parts of sea hail polysaccharide, 5 parts of orange essential oil, 22 parts of cocamidopropyl betaine, 17 parts of polyethylene glycol, 3 parts of xanthan gum, 0.3 parts of sodium citrate, and 100 parts of deionized water; The preparation process of the modified nano-attapulgite is as follows: S1. calcining the nano-attapulgite at 230°C for 30 min to obtain pretreated nano-attapulgite; adding the pretreated nano-attapulgite to an ethanol aqueous solution (ethanol and water are mixed in a volume ratio of 4:1), and then adding γ-aminopropyltriethoxysilane, wherein the amount ratio of the pretreated nano-attapulgite, γ-aminopropyltriethoxysilane, and the ethanol aqueous solution is 1g:0.2g:15mL; stirring the reaction at room temperature for 2h to obtain amino-modified nano-attapulgite; S2. Add the aminated nano-attapulgite to DMF, and then add gallic acid and triethylamine, wherein the mass ratio of the aminated nano-attapulgite, gallic acid and triethylamine is 1:0.4:0.9; stir the reaction at 90°C for 1h, and then filter, wash and dry to obtain modified nano-attapulgite.

[0028] The preparation process of the polysaccharide of the sea hail is the same as that of Example 1 A method for preparing an antibacterial hand sanitizer comprises the following steps: According to the above weight ratio, cocamidopropyl betaine and polyethylene glycol are added to water, heated to 50°C and stirred to mix, and modified nano-attapulgite, salvia polysaccharide, orange essential oil, xanthan gum and sodium citrate are added under heating at 50°C, and the antibacterial hand sanitizer is obtained after mixing evenly.

[0029] Comparative Example 1 A hand soap comprises the following raw materials in parts by weight: 6 parts of nano-attapulgite, 3 parts of salvia polysaccharide, 3 parts of orange essential oil, 18 parts of cocamidopropyl betaine, 15 parts of glycerol, 2 parts of xanthan gum, 0.1 part of sodium citrate, and 95 parts of deionized water; other parts are consistent with those in Example 1.

[0030] Comparative Example 2 A hand soap comprises the following raw materials in parts by weight: 5 parts of nano-attapulgite, 1 part of gallic acid, 3 parts of physalis polysaccharide, 3 parts of orange essential oil, 18 parts of cocamidopropyl betaine, 15 parts of glycerol, 2 parts of xanthan gum, 0.1 part of sodium citrate, and 95 parts of deionized water; the rest is consistent with Example 1.

[0031] Comparative Example 3 A hand soap comprises the following raw materials in parts by weight: 6 parts of modified nano-attapulgite, 3 parts of orange essential oil, 18 parts of cocamidopropyl betaine, 15 parts of glycerol, 2 parts of xanthan gum, 0.1 parts of sodium citrate, and 95 parts of deionized water; the rest is consistent with Example 1.

[0032] Test example Test Example 1 1. Antibacterial test: The test strains were Escherichia coli and Staphylococcus aureus, and the concentrations of Escherichia coli suspension and Staphylococcus aureus suspension were adjusted to 3.0×10 6 CFU / mL. Take 10mL of the hand sanitizer prepared in Example 1-3 and Comparative Example 1-3, sterilize and add to a sterile test tube, add 100µL of Escherichia coli suspension and 100µL of Staphylococcus aureus suspension to the sterile test tube, culture for 2 minutes, use a sterile pipette to draw 0.5mL of the liquid in the above sterile test tube and add it to 4.5mL of neutralizer (add 1g of sodium thiosulfate to 100mL of 0.03mol / L phosphate buffer, steam sterilize at 121°C for 20min) and mix evenly, after 10 minutes, draw 200µL and inoculate it on the culture medium, spread it evenly with an applicator, and then invert and culture at 37°C for 48h, count the number of live bacterial colonies, calculate the antibacterial rate data, replace the hand sanitizer with double distilled water and perform the same treatment as the blank control group.

[0033] Inhibition rate = (average colony count of blank control group - average colony count of experimental group) / average colony count of blank control group × 100%; 3 parallel experiments were performed in each group, and the inhibition rate value was the average value of 3 parallel experiments. The results are shown in Table 1.

[0034] Table 1 It can be seen from the test data in Table 1 that the hand sanitizers of Examples 1 to 3 of the present invention have good antibacterial properties. Compared with Example 1, the antibacterial rates of Comparative Examples 1 and 3 are reduced, indicating that the use of modified attapulgite and salvia polysaccharide can improve the antibacterial properties of hand sanitizers.

[0035] 2. Antibacterial stability test: 10 mL of the hand sanitizer of the above Examples 1-3 and Comparative Examples 1-3 was placed at 54° C. and 75% relative humidity for 14 days. The antibacterial rate of each group of hand sanitizers was tested with reference to the operating steps of the above antibacterial test. The results are shown in Table 2.

[0036] Table 2 It can be seen from the test data in Table 2 that the hand sanitizers of Examples 1-3 still have a good antibacterial rate after being placed under the conditions of 54° C. and 75% relative humidity for two weeks.

[0037] Compared with Example 1, Comparative Example 2 directly mixed nano-attapulgite and gallic acid, Comparative Example 1 replaced modified nano-attapulgite with nano-attapulgite, and Comparative Example 3 omitted the polysaccharide of sea hail. The antibacterial rates of the three groups decreased to varying degrees. Analysis shows that after the amino-treated attapulgite is grafted with gallic acid, the stability of gallic acid in the hand sanitizer can be improved, so that gallic acid can be stably distributed in the hand sanitizer, thereby achieving a long-term antibacterial effect and reducing its irritation to the skin. On the other hand, modified attapulgite can be used in combination with sea hail polysaccharide to jointly improve the antibacterial activity and antibacterial stability of the hand sanitizer.

[0038] Test Example 2 The stability of the hand sanitizers obtained in Examples 1-3 and Comparative Examples 1-3 was tested according to the test standard of "Special Hand Sanitizer GB19877.1-2005", and the specific steps are as follows: Take 10 mL of the hand sanitizer of the above Examples 1-3 and Comparative Examples 1-3, place them at -5°C and 40°C for 24 hours, then take them out, and when they return to room temperature, observe whether they have stratification or the like. The results are shown in Table 3.

[0039] Table 3 From the test data in Table 3, it can be seen that the antibacterial hand sanitizer of the present invention has good stability, and no stratification, turbidity, etc. occur after being placed at 40°C and -5°C for 24 hours. Compared with Example 1, Comparative Example 3 omits the polysaccharide of the sea hail, and the hand sanitizer shows stratification to varying degrees under hot and cold environments. These phenomena indicate that the stability of the antibacterial hand sanitizer is poor, and the polysaccharide of the sea hail can be used in combination with modified attapulgite to jointly improve the stability of the hand sanitizer.

[0040] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit them. The basic principles and main features of the present invention have been described above with specific implementation schemes. On the basis of the present invention, some modifications or replacements may be made thereto, but these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the scope of protection claimed by the present invention.

Claims

1. An antibacterial hand soap, characterized in that: The invention comprises the following raw materials in parts by weight: 4-9 parts of modified nano-attapulgite, 1-5 parts of sea hail polysaccharide, 1-5 parts of plant essential oil, 15-22 parts of surfactant, 10-17 parts of moisturizing agent, 0.1-0.3 parts of pH adjusting agent, 1-3 parts of thickener, and 90-100 parts of deionized water; The preparation process of the modified nano-attapulgite is as follows: S1. The pretreated nano-attapulgite is added to an ethanol aqueous solution, and then γ-aminopropyltriethoxysilane is added and stirred to react to obtain an amino-modified nano-attapulgite; S2. Add the aminated nano-attapulgite into a solvent, then add gallic acid and triethylamine, heat and stir to react, and obtain modified nano-attapulgite.

2. An antibacterial hand sanitizer according to claim 1, characterized in that: The mass ratio of the pretreated nano-attapulgite, γ-aminopropyltriethoxysilane, and ethanol aqueous solution in S1 is 1 g: (0.1-0.2) g: (10-15) mL.

3. The antibacterial hand sanitizer according to claim 1, characterized in that: The mass ratio of the amino nano-attapulgite, gallic acid and triethylamine in S2 is 1:(0.2-0.4):(0.5-0.9).

4. The antibacterial hand sanitizer according to claim 1, characterized in that: The temperature of the heating and stirring in S2 is 80-90°C and the time is 1-2h.

5. The antibacterial hand sanitizer according to claim 1, characterized in that: The ethanol aqueous solution described in S1 is obtained by mixing ethanol and water in a volume ratio of (3-5):1; the solvent described in S2 is DMF.

6. The antibacterial hand sanitizer according to claim 1, characterized in that: The pretreatment process of the nano attapulgite in S1 is as follows: the nano attapulgite is calcined at 150-230° C. for 30 min-90 min.

7. The antibacterial hand sanitizer according to claim 1, characterized in that: The plant essential oil is lavender essential oil or orange essential oil; the moisturizer is any one of glycerin, propylene glycol, and polyethylene glycol; the thickener is xanthan gum or carbomer; the surfactant is cocamidopropyl betaine or dodecyl glucoside; and the pH adjuster is sodium citrate.

8. A method for preparing the antibacterial hand sanitizer according to any one of claims 1 to 7, characterized in that: The steps include: According to the weight ratio, the surfactant and the moisturizer are added into water, heated and stirred, and then the modified nano-attapulgite, the polysaccharide of the sea hail, the plant essential oil, the thickener and the pH adjuster are added and stirred evenly to obtain the product.

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