CN111329786B - Multifunctional hand sanitizer containing aminopropanesulfonic acid inner salt type amphoteric structure and preparation method thereof - Google Patents
Multifunctional hand sanitizer containing aminopropanesulfonic acid inner salt type amphoteric structure and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a multifunctional hand sanitizer containing aminopropanesulfonic acid inner salt type amphoteric structure and a preparation method thereof, wherein starch is subjected to enzymatic degradation to prepare degraded starch, then N, N-dimethyl (methacryloyloxyethyl) aminopropanesulfonic acid inner salt is used for grafting modified starch under the action of horseradish peroxidase, and then acrylic acid and N, N-dimethyl (methacryloyloxyethyl) aminopropanesulfonic acid inner salt and allyl alcohol polyoxyethylene ether are prepared into a copolymer, animal oleic acid and polyethylene glycol monomethyl ether are used for reacting to prepare animal oleic acid polyethylene glycol monomethyl ether, and the prepared grafted modified starch, copolymer and animal oleic acid polyethylene glycol ester are compounded with dodecyl sodium sulfate, acrylic acid, sodium methacrylate, sodium tripolyphosphate, tritolyglycoside, isothiazolinone, citric acid, essence, pigment and the like to prepare the ecological hand sanitizer containing aminopropanesulfonate inner salt type structure.
Description
Technical Field
The invention relates to a detergent, in particular to a multifunctional hand sanitizer containing an amino propane sulfonic acid inner salt type amphoteric structure and a preparation method thereof.
Background
The most effective and simple method for controlling the spread of diseases and preventing infection is to wash hands frequently, and has good preventive effect on diseases spread by digestive tracts and diseases spread by respiratory tracts. The atypical epidemic situation in 2003 leads people to generally improve the self-protection consciousness in daily life, the most common self-protection habit is to carry out the hand washing and hand washing, and the spreading of the epidemic situation of the new coronal pneumonia before and after the spring festival in 2020 reminds people to improve the consciousness and the behavior of the self-protection from the habit of daily life again, wherein the hand washing and the hand washing become the living habit that individuals must stand against the epidemic situation of the new coronal pneumonia. The hand is the part which is most contacted with the outside and is easy to infect, and is the main way for causing people to infect diseases, one of the methods for washing hands is to select and use the hand sanitizer, the time that the hand sanitizer contacts with the hand in the washing process is shorter, and the hand sanitizer with the sterilization and disinfection function must be selected correctly for achieving the sterilization and disinfection function.
The antibacterial components of the common commercial antibacterial hand sanitizer at present mainly comprise o-phenylphenol (OPP), trichlorohydroxydiphenyl ether (DP 300), 4-chloro-3, 5-xylenol (PCMX), trichlorperanilide (TCC) and the novel Jieling disinfectant. The use of the antibacterial agents has great influence on human bodies and the environment, and secondary pollution is easy to generate. Therefore, the novel hand sanitizer with good decontamination effect, safety, low stimulation, antibacterial and bactericidal capacity, environmental friendliness and low cost is developed.
Researchers in 1935 found that quaternary ammonium salts have strong bactericidal properties, and subsequent studies of quaternary ammonium salts as antibacterial agents have attracted great attention. At present, quaternary ammonium type cationic betaine, secerzamide and the like are applied to daily hand washing liquid for sterilization and disinfection. However, these cationic quaternary ammonium salts have small molecules, are easily lost, and have short contact time with hands. Furthermore, quaternary ammonium cations have a certain irritation and cannot meet the use requirements of the quaternary ammonium cations as washing products for cleaning human skin and the like.
Disclosure of Invention
The invention aims to provide a multifunctional hand sanitizer containing an amino propane sulfonic acid inner salt type amphoteric structure and a preparation method thereof, wherein introduced quaternary ammonium salt cations and adjacent anions are of an inner salt type structure and neutral, so that the irritation of the quaternary ammonium salt and the influence on the system stability are reduced, and the prepared hand sanitizer is environment-friendly, has small irritation to human skin and the like and has strong sterilizing and decontamination capacities.
In order to achieve the above purpose, the invention adopts the following technical scheme:
a preparation method of a multifunctional hand sanitizer containing an amino propane sulfonic acid inner salt type amphoteric structure comprises the following steps:
step one, mixing 20 to 25 parts of starch with 100 to 130 parts of deionized water and 0.2 to 0.3 part of high-temperature alpha-amylase according to parts by weight, heating to 90 to 95 ℃, and carrying out degradation reaction for 2.5 to 3.5 hours at a temperature to obtain a degraded starch solution;
adding 10-12 parts of N, N-dimethyl (methacryloyloxyethyl) aminopropanesulfonic acid inner salt and 6-8 parts of acrylamide into the degraded starch solution prepared in the step one, stirring and heating to 40-45 ℃, adding 4-6 parts of buffer solution to adjust the pH value of a system to 6.3-6.5, simultaneously dropwise adding 5-8 parts of horseradish peroxidase solution with the mass fraction of 0.09-0.15% and 8-10 parts of hydrogen peroxide solution with the mass fraction of 30%, controlling the dropwise adding time to 2.0-2.5 hours, and continuously preserving heat for reacting for 4.5-5.5 hours after the dropwise adding is finished to obtain modified starch;
step three, adding 25 to 30 parts of polyether macromonomer, 15 to 18 parts of N, N-dimethyl (methacryloyloxyethyl) aminopropanesulfonic acid inner salt and 250 to 282 parts of water into a reactor, uniformly stirring, keeping the temperature in the system at 40 to 50 ℃, and then adding 0.45 to 0.53 part of persulfate and uniformly stirring; then, dropwise adding a mixture of 44-52 parts of acrylic acid, 9-11 parts of sodium methacrylate, 0.36-0.42 part of vitamin C, 0.35-0.41 part of mercaptoethanol and 102-130 parts of water for 2.5-3 hours, continuing stirring and reacting for 2-3 hours after the dropwise adding, and regulating the pH value to 6.0-6.5 by using sodium hydroxide with the mass fraction of 40%, wherein the obtained product is an aminopropanesulfonic acid inner salt type amphoteric polymer;
mixing 26-30 parts of animal oleic acid, 30-35 parts of polyethylene glycol monomethyl ether and 0.6-0.8 part of p-toluenesulfonic acid in a reactor, stirring and heating to 110-120 ℃, preserving heat for 3-3.5 hours, and cooling to room temperature to obtain animal oleic acid polyethylene glycol monomethyl ether ester;
and step five, sequentially adding 46 to 53 parts of modified starch prepared in the step two, 19 to 23 parts of aminopropanesulfonic acid inner salt type amphoteric polymer prepared in the step three, 4 to 5 parts of sodium dodecyl sulfate, 5 to 6 parts of animal oleic acid polyethylene glycol monomethyl ether ester prepared in the step four, 2 to 3 parts of sodium tripolyphosphate, 0.7 to 0.9 part of citric acid, 0.05 to 0.08 part of triterpenoid saponin, 0.01 to 0.03 part of isothiazolinone, 0.1 to 0.3 part of essence, 2.5 to 3.2 parts of pigment and 55 to 74 parts of deionized water into a mixing container, and stirring for 0.5 to 1 hour to obtain the multifunctional hand sanitizer containing the aminopropanesulfonic acid inner salt type amphoteric structure.
Further, the buffer solution is prepared by dissolving 6.7-7.1 parts of sodium dihydrogen phosphate and 7.3-7.6 parts of disodium hydrogen phosphate in 100-120 parts of deionized water, and the pH value is 6.5-7.0.
Further, the polyether macromonomer is one or a mixture of several of allyl alcohol polyoxyethylene ether, methyl allyl alcohol polyoxyethylene ether and isopentenyl alcohol polyoxyethylene ether, the molecular weight is 2000-2400, the water content is less than or equal to 1%, the hydroxyl value is 2500-2800 mgKOH/g, the unsaturation degree is 0.5-0.63 mmol, and the pH value of a 1% aqueous solution is 5.0-7.0.
Further, the average relative molecular weight of the polyethylene glycol monomethyl ether is 2100 to 2200.
Further, the enzyme activity of the horseradish peroxidase is 330u/mg, and 0.05-0.08 part of horseradish peroxidase is dissolved in 50-60 parts of deionized water to prepare a horseradish peroxidase solution with the mass fraction of 0.09-0.15%.
Further, the animal oleic acid is light yellow transparent oily liquid, the acid value is 190-205 mgKOH/g, the saponification value is 192-215 mgKOH/g, the iodine value is 80-g I/100 g, the freezing point is less than 4 ℃, and the water content is less than 0.5%.
Further, the number average molecular weight of the modified starch is 6.8-9.6 ten thousand, and the number average molecular weight of the aminopropanesulfonic acid inner salt type amphoteric polymer is 8.9-12.4 ten thousand.
Further, the modified starch prepared in the second step has a molecular structural formula of
Wherein a, b and c are the number of structural units.
Further, the molecular structural formula of the aminopropanesulfonic acid inner salt type amphoteric polymer prepared in the step three is
Wherein a, b, c, d is the number of structural units.
The multifunctional hand sanitizer containing the aminopropanesulfonic acid inner salt type amphoteric structure has the pH value of 6.0-6.5, the viscosity of 810-480 Pa.s, the foam height of 480-560 mm, and the sterilization rates of 99.50-99.99% and 99.98-100% on escherichia coli and staphylococcus aureus respectively.
Compared with the prior art, the invention has the beneficial effects that:
(1) The inner salt type amphoteric monomer N, N-dimethyl (methacryloyloxyethyl) aminopropanesulfonic acid inner salt is selected as a component with sterilization and disinfection, the appearance shows neutrality, when the inner salt structure encounters negative substances such as bacterial viruses, the quaternary ammonium cations can be released to realize the blocking and killing of the bacterial viruses, the inner salt type amphoteric structure has the characteristics of mild and non-irritating effects on skin, strong sterilization and disinfection capability and the like, and the inner salt type amphoteric sterilization disinfectant formed by the quaternary ammonium salts and the sulfonate has novelty and innovation.
(2) The selected inner salt type amphoteric disinfectant contains double bonds capable of undergoing free radical polymerization, and inner salt type cationic monomers are respectively grafted on degraded starch and polymerized with acrylic acid, polyether macromonomer and the like to form a water-based polymer with larger viscosity, so that on one hand, the contact time of the inner salt type disinfectant with hands during hand washing is improved, the sterilization and disinfection effects are improved, on the other hand, the inner salt type disinfectant is combined with natural polymer material starch, the ecological degradation effects of the hand sanitizer after use are improved, the pollution of amphoteric substances to a water system after use is reduced, and therefore, the inner salt type disinfectant has very strong innovation in use of the amphoteric disinfectant.
(3) The selected inner salt type amphoteric disinfectant, acrylic acid, sodium methacrylate sulfonate and polyether macromonomer are subjected to free radical copolymerization to prepare macromolecules with larger molecular weight, introduced quaternary ammonium salt cations are of an inner salt type structure, instability of the quaternary ammonium salt to a system is reduced, contact time of the disinfectant and hands is prolonged, a disinfecting effect is improved, meanwhile, the polymer has functions of thickening, resisting hard water, foaming, stabilizing foam, lubricating and the like, use comfort of the hand washing liquid is improved, and innovativeness in the aspect of a using effect is improved.
(4) The animal oleic acid polyethylene glycol ester is prepared, has the effect of moistening skin on hands during hand washing, has the effects of foaming and stabilizing foam, and also has innovativeness.
(5) The hand sanitizer is viscous liquid, the content of the hand sanitizer is 20% -21%, the pH value is 6.0-6.5, the viscosity is 810-480 Pa.s, the foam height is 480-560 mm, the hand sanitizer has the functions of sterilization and disinfection, has good inhibition effects on escherichia coli and staphylococcus aureus, the sterilization rates of the escherichia coli and the staphylococcus aureus respectively reach 99.50-99.99% and 99.98-100%, the hand sanitizer has the functions of skin care and skin moistening, and has rich and rapid bubbles, rapid defoaming and good practicability.
(6) The preparation process is scientific and reasonable, pollution-free, high in cost performance and good in market application prospect.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but is not limited thereto.
The invention relates to a preparation method of multifunctional hand sanitizer containing an amino propane sulfonic acid inner salt type amphoteric structure, which specifically comprises the following steps:
step one, mixing 20 to 25 parts of starch with 100 to 130 parts of deionized water and 0.2 to 0.3 part of high-temperature alpha-amylase according to parts by weight, heating to 90 to 95 ℃, and carrying out degradation reaction for 2.5 to 3.5 hours at a temperature to obtain a degraded starch solution;
adding 10-12 parts of N, N-dimethyl (methacryloyloxyethyl) aminopropanesulfonic acid inner salt and 6-8 parts of acrylamide into the degraded starch solution, stirring and heating to 40-45 ℃, adding 4-6 parts of buffer solution to adjust the pH value of a system to 6.3-6.5, simultaneously dropwise adding 5-8 parts of horseradish peroxidase solution with the mass fraction of 0.09-0.15% and 8-10 parts of hydrogen peroxide solution with the mass fraction of 30%, controlling the dropwise adding time to be 2.0-2.5 hours, and continuing to perform heat preservation reaction for 4.5-5.5 hours after dropwise adding to obtain modified starch;
the reaction equation for preparing the aminopropanesulfonic inner salt grafted modified starch is as follows:
step three, adding 25 to 30 parts of polyether macromonomer, 15 to 18 parts of N, N-dimethyl (methacryloyloxyethyl) amino propane sulfonic acid inner salt and 250 to 282 parts of water into a reactor, uniformly stirring, keeping the temperature in the system at 40 to 50 ℃, and then adding 0.45 to 0.53 part of persulfate and uniformly stirring. Then, 44 to 52 parts of acrylic acid, 9 to 11 parts of sodium methacrylate, 0.36 to 0.42 part of vitamin C, 0.35 to 0.41 part of mercaptoethanol and a mixture of 102 to 130 parts of water are dripped for 2.5 to 3 hours, the reaction is continued to be stirred for 2 to 3 hours after the dripping is finished, the product obtained in sodium hydroxide with the mass fraction of 40 percent is used for regulating and controlling the pH value to be 6.0 to 6.5, and the obtained product is the aminopropanesulfonic acid inner salt type amphoteric polymer, and has the effects of thickening, stabilizing foam, improving smooth feeling and the like.
The reaction equation for preparing the aminopropanesulfonic inner salt type amphoteric polymer is as follows:
and fourthly, mixing 26-30 parts of animal oleic acid, 30-35 parts of polyethylene glycol monomethyl ether and 0.6-0.8 part of p-toluenesulfonic acid in a dry and anhydrous reactor, stirring and heating to 110-120 ℃, preserving heat for 3-3.5 hours, and cooling to room temperature to obtain the animal oleic acid polyethylene glycol monomethyl ether ester.
And fifthly, sequentially adding 46-53 parts of modified starch, 19-23 parts of aminopropanesulfonic inner salt type amphoteric polymer, 4-5 parts of sodium dodecyl sulfate, 5-6 parts of animal oleic acid polyethylene glycol ester, 2-3 parts of sodium tripolyphosphate, 0.7-0.9 part of citric acid, 0.05-0.08 part of triterpenoid saponin, 0.01-0.03 part of isothiazolinone, 0.1-0.3 part of essence, 2.5-3.2 parts of pigment and 55-74 parts of deionized water into a mixing container, and stirring for 0.5-1 hour to obtain the multifunctional hand sanitizer for ecological skin care and sterilization.
The starch is corn starch, potato starch or sweet potato starch, and the moisture content of the starch is less than 1%.
The activity unit of the high temperature alpha-amylase is 20000U/mL, the effective temperature range is 85-105 ℃, and the effective pH value range is 5.0-7.0.
The buffer solution is prepared by dissolving 6.7-7.1 parts of sodium dihydrogen phosphate and 7.3-7.6 parts of disodium hydrogen phosphate in 100-120 parts of deionized water, and the pH value is 6.5-7.0.
The enzyme activity of the horseradish peroxidase is 330u/mg, and 0.05-0.08 part of horseradish peroxidase is dissolved in 50-60 parts of deionized water to prepare a horseradish peroxidase solution with the mass fraction of 0.09-0.15%.
The polyether macromonomer is one or a mixture of several of allyl alcohol polyoxyethylene ether, methyl allyl alcohol polyoxyethylene ether and isopentenyl alcohol polyoxyethylene ether, the molecular weight is 2000-2400, the moisture content is less than 1%, the hydroxyl value is 2500-2800 mgKOH/g, the unsaturation degree is 0.5-0.63 mmol, and the pH value of a 1% aqueous solution is 5.0-7.0.
The content of the acrylic acid, the sodium methacrylate sulfonate, the N, N-dimethyl (methacryloyloxyethyl) amino propane sulfonate, the acrylamide, the vitamin C and the mercaptoethanol is more than 99 percent.
The persulfate is ammonium persulfate, sodium persulfate and potassium persulfate, and the content of the persulfate is more than 99%.
The animal oleic acid has the appearance of light yellow transparent oily liquid, the acid value of 190-205 mgKOH/g, the saponification value of 192-215 mgKOH/g and the iodine value of 80-g I 2 100g, freezing point less than 4 ℃ and water content less than 0.5%.
The average relative molecular mass of the polyethylene glycol monomethyl ether is 2100-2200.
The contents of the sodium dodecyl sulfate, the sodium tripolyphosphate, the citric acid and the triterpenoid saponin are all more than 98 percent.
The isothiazolinone bactericide is light amber liquid, and the effective matter content is 2.5%.
The essence is food-grade essence, the appearance is transparent liquid, the content of effective matters is more than 98%, and the fragrance type can be selected from flower fragrance type, fruit fragrance type, compound fragrance type, chocolate type and the like according to the needs.
The pigment is natural colorant, powder, and has effective matter content greater than 99%, and the pigment can be orange, light green, pink, light blue, grape purple, etc.
Embodiment one:
step one, mixing 20 parts of starch with 100 parts of deionized water and 0.2 part of high-temperature alpha-amylase according to parts by weight, heating to 90 ℃, and carrying out degradation reaction for 2.5 hours at a temperature to obtain a degraded starch solution;
adding 10 parts of N, N-dimethyl (methacryloyloxyethyl) aminopropanesulfonic acid inner salt and 6 parts of acrylamide into the degraded starch solution, stirring and heating to 40 ℃, adding 4 parts of buffer solution to adjust the pH value of a system to 6.3, simultaneously dropwise adding 5 parts of horseradish peroxidase solution with the mass fraction of 0.09% and 8 parts of hydrogen peroxide solution with the mass fraction of 30%, controlling the dropwise adding time to be 2.0 hours, and continuing to perform heat preservation reaction for 4.5 hours after the dropwise adding is finished to obtain modified starch;
and thirdly, adding 25 parts of polyether macromonomer, 15 parts of N, N-dimethyl (methacryloyloxyethyl) amino propane sulfonic acid inner salt and 250 parts of water into a reactor, uniformly stirring, keeping the temperature in the system at 40 ℃, and then adding 0.45 part of persulfate and uniformly stirring. Then, 44 parts of acrylic acid, 9 parts of sodium methacrylate sulfonate, 0.36 part of vitamin C, 0.35 part of mercaptoethanol and a mixture with 102 parts of water are dropwise added for 2.5 hours, stirring reaction is continued for 2 hours after the dropwise addition, and the pH value is regulated to 6.0 by using a product obtained in 40% sodium hydroxide by mass fraction, so that the obtained product is an aminopropanesulfonic acid inner salt type amphoteric polymer, and has the effects of thickening, stabilizing foam, improving slip feeling and the like.
The molecular structural formula of the prepared aminopropanesulfonic inner salt type amphoteric polymer is as follows:
and step four, mixing 26 parts of animal oleic acid, 30 parts of polyethylene glycol monomethyl ether and 0.6 part of p-toluenesulfonic acid in a dry and anhydrous reactor, stirring and heating to 110 ℃, preserving heat for 3 hours, and cooling to room temperature to obtain the animal oleic acid polyethylene glycol monomethyl ether ester.
And step five, sequentially adding 46 parts of grafted modified starch, 19 parts of aminopropanesulfonic inner salt type amphoteric polymer, 4 parts of sodium dodecyl sulfate, 5 parts of animal oleic acid polyethylene glycol ester, 2 parts of sodium tripolyphosphate, 0.7 part of citric acid, 0.05 part of triterpenoid saponin, 0.01 part of isothiazolinone, 0.1 part of essence, 2.5 parts of pigment and 55 parts of deionized water into a mixing container, and stirring for 0.5 hour to obtain the ecological skin care sterilizing multifunctional hand sanitizer.
The number average molecular weight of the prepared grafted modified starch is 8.8 ten thousand, the number average molecular weight of the aminopropanesulfonic acid inner salt type amphoteric polymer is 10.6 ten thousand, the yield of animal oleic acid polyethylene glycol monomethyl ether ester is 99.1%, the hand cleanser is viscous liquid, the content is 20%, the pH value is 6.0, the viscosity is 850 Pa.s, the foam height is 510mm, the grafted modified starch has good inhibition effect on escherichia coli and staphylococcus aureus, the sterilization rate on escherichia coli and staphylococcus aureus reaches 99.60% and 99.85%, and meanwhile, the hand skin is moistened and protected.
Embodiment two:
step one, mixing 23 parts of starch with 120 parts of deionized water and 0.25 part of high-temperature alpha-amylase according to parts by mass, heating to 95 ℃, and carrying out degradation reaction for 3.5 hours at a temperature to obtain a degraded starch solution;
adding 12 parts of N, N-dimethyl (methacryloyloxyethyl) aminopropanesulfonic acid inner salt and 8 parts of acrylamide into the degraded starch solution, stirring and heating to 45 ℃, adding 6 parts of buffer solution to adjust the pH value of a system to 6.5, simultaneously dropwise adding 7 parts of horseradish peroxidase solution with the mass fraction of 0.12% and 9 parts of hydrogen peroxide solution with the mass fraction of 30%, controlling the dropwise adding time to be 2.5 hours, and continuing to perform heat preservation reaction for 5.5 hours after the dropwise adding is finished to obtain modified starch;
and thirdly, adding 30 parts of polyether macromonomer, 18 parts of N, N-dimethyl (methacryloyloxyethyl) amino propane sulfonic acid inner salt and 282 parts of water into a reactor, uniformly stirring, keeping the temperature in the system at 50 ℃, and then adding 0.53 part of persulfate and uniformly stirring. Then 52 parts of acrylic acid, 11 parts of sodium methacrylate sulfonate, 0.42 part of vitamin C, 0.41 part of mercaptoethanol and 130 parts of water are added dropwise for 3 hours, stirring reaction is continued for 3 hours after the dripping is finished, the pH value is regulated to 6.5 by using a product obtained from 40% sodium hydroxide by mass, and the obtained product is an aminopropanesulfonic acid inner salt type amphoteric polymer, and has the effects of thickening, stabilizing foam, improving smoothness and the like.
And step four, mixing 28 parts of animal oleic acid, 33 parts of polyethylene glycol monomethyl ether and 0.7 part of p-toluenesulfonic acid in a dry and anhydrous reactor, stirring and heating to 120 ℃, preserving heat for 3 hours, and cooling to room temperature to obtain the animal oleic acid polyethylene glycol monomethyl ether ester.
And fifthly, sequentially adding 50 parts of modified starch, 20 parts of aminopropanesulfonic inner salt type amphoteric polymer, 4.5 parts of sodium dodecyl sulfate, 5.5 parts of animal oleic acid polyethylene glycol ester, 2.5 parts of sodium tripolyphosphate, 0.8 part of citric acid, 0.07 part of triterpenoid saponin, 0.02 part of isothiazolinone, 0.2 part of essence, 2.9 parts of pigment and 65 parts of deionized water into a mixing container, and stirring for 0.8 hour to obtain the ecological skin care sterilizing multifunctional hand sanitizer.
The number average molecular weight of the prepared grafted modified starch is 6.8 ten thousand, the number average molecular weight of the aminopropanesulfonic acid inner salt type amphoteric polymer is 8.9 ten thousand, the yield of animal oleic acid polyethylene glycol monomethyl ether ester is 98.5%, the hand cleanser is viscous liquid, the content is 20%, the pH value is 6.0, the viscosity is 810mPa.s, the foam height is 480mm, the grafted modified starch has good inhibition effect on escherichia coli and staphylococcus aureus, the sterilization rate on escherichia coli and staphylococcus aureus reaches 99.95% and 99.98%, and meanwhile, the hand skin is moistened and protected.
Embodiment III:
step one, mixing 25 parts of starch with 130 parts of deionized water and 0.3 part of high-temperature alpha-amylase according to parts by mass, heating to 95 ℃, and carrying out degradation reaction for 3.5 hours at a temperature to obtain a degraded starch solution;
adding 11 parts of N, N-dimethyl (methacryloyloxyethyl) aminopropanesulfonic acid inner salt and 7 parts of acrylamide into the degraded starch solution, stirring and heating to 45 ℃, adding 6 parts of buffer solution to adjust the pH value of a system to 6.5, simultaneously dropwise adding 8 parts of horseradish peroxidase solution with the mass fraction of 0.15% and 10 parts of hydrogen peroxide solution with the mass fraction of 30%, controlling the dropwise adding time to be 2.5 hours, and continuing to perform heat preservation reaction for 5.5 hours after the dropwise adding is finished to obtain modified starch;
and thirdly, adding 30 parts of polyether macromonomer, 18 parts of N, N-dimethyl (methacryloyloxyethyl) amino propane sulfonic acid inner salt and 282 parts of water into a reactor, uniformly stirring, keeping the temperature in the system at 50 ℃, and then adding 0.53 part of persulfate and uniformly stirring. Then, 49 parts of acrylic acid, 11 parts of sodium methacrylate sulfonate, 0.42 part of vitamin C, 0.41 part of mercaptoethanol and 130 parts of water are added dropwise for 3 hours, stirring reaction is continued for 3 hours after the dripping is finished, and the pH value is regulated to 6.5 by using a product obtained from 40% sodium hydroxide by mass, so that the obtained product is an aminopropanesulfonic acid inner salt type amphoteric polymer, and the effects of thickening, stabilizing foam, improving smoothness and the like are achieved.
And step four, mixing 30 parts of animal oleic acid, 35 parts of polyethylene glycol monomethyl ether and 0.8 part of p-toluenesulfonic acid in a dry and anhydrous reactor, stirring and heating to 120 ℃, preserving heat for 3.5 hours, and cooling to room temperature to obtain the animal oleic acid polyethylene glycol monomethyl ether ester.
53 parts of modified starch, 23 parts of aminopropanesulfonic acid inner salt type amphoteric polymer, 5 parts of sodium dodecyl sulfate, 6 parts of animal oleic acid polyethylene glycol ester, 3 parts of sodium tripolyphosphate, 0.9 part of citric acid, 0.08 part of tritolysaccharide, 0.03 part of isothiazolinone, 0.3 part of essence, 3.2 parts of pigment and 74 parts of deionized water are sequentially added into a mixing container, and stirring is carried out for 1 hour, so that the preparation method of the ecological skin care sterilizing multifunctional hand sanitizer is obtained.
The number average molecular weight of the prepared grafted modified starch is 9.6 ten thousand, the number average molecular weight of the aminopropanesulfonic acid inner salt type amphoteric polymer is 12.4 ten thousand, the yield of animal oleic acid polyethylene glycol monomethyl ether ester is 99.6%, the hand cleanser is viscous liquid, the content is 21%, the pH value is 6.5, the viscosity is 480 Pa.s, the foam height is 560mm, the grafted modified starch has good inhibition effect on escherichia coli and staphylococcus aureus, the sterilization rate on escherichia coli and staphylococcus aureus reaches 99.99% and 100%, and meanwhile, the hand skin is moistened and protected.
Embodiment four:
step one, mixing 22 parts of starch with 110 parts of deionized water and 0.3 part of high-temperature alpha-amylase according to parts by mass, heating to 92 ℃, and carrying out degradation reaction for 3 hours at a temperature to obtain a degraded starch solution;
adding 11 parts of N, N-dimethyl (methacryloyloxyethyl) aminopropanesulfonic acid inner salt and 7 parts of acrylamide into the degraded starch solution, stirring and heating to 42 ℃, adding 5 parts of buffer solution to adjust the pH value of a system to 6.4, simultaneously dropwise adding 8 parts of horseradish peroxidase solution with the mass fraction of 0.15% and 10 parts of hydrogen peroxide solution with the mass fraction of 30%, controlling the dropwise adding time to be 2.2 hours, and continuing to perform heat preservation reaction for 5.0 hours after the dropwise adding is finished to obtain modified starch;
and thirdly, adding 27 parts of polyether macromonomer, 17 parts of N, N-dimethyl (methacryloyloxyethyl) amino propane sulfonic acid inner salt and 260 parts of water into a reactor, uniformly stirring, keeping the temperature in the system at 45 ℃, and then adding 0.50 part of persulfate and uniformly stirring. Then, 49 parts of acrylic acid, 10 parts of sodium methacrylate sulfonate, 0.40 part of vitamin C, 0.40 part of mercaptoethanol and a mixture of 110 parts of water are dropwise added for 2.8 hours, stirring reaction is continued for 2.5 hours after the dropwise addition is finished, a product obtained by using 40% sodium hydroxide by mass fraction is used for regulating the pH value to be 6.2, and the obtained product is an aminopropanesulfonic acid inner salt type amphoteric polymer, and has the effects of thickening, stabilizing foam, improving smoothness and the like.
And step four, mixing 30 parts of animal oleic acid, 35 parts of polyethylene glycol monomethyl ether and 0.8 part of p-toluenesulfonic acid in a dry and anhydrous reactor, stirring and heating to 115 ℃, preserving heat for 3.2 hours, and cooling to room temperature to obtain the animal oleic acid polyethylene glycol monomethyl ether ester.
53 parts of modified starch, 23 parts of aminopropanesulfonic acid inner salt type amphoteric polymer, 5 parts of sodium dodecyl sulfate, 6 parts of animal oleic acid polyethylene glycol ester, 3 parts of sodium tripolyphosphate, 0.9 part of citric acid, 0.08 part of tritolysaccharide, 0.03 part of isothiazolinone, 0.3 part of essence, 3.2 parts of pigment and 74 parts of deionized water are sequentially added into a mixing container, and stirring is carried out for 1 hour, so that the preparation method of the ecological skin care sterilizing multifunctional hand sanitizer is obtained.
Finally, it should be noted that: the above embodiments are only for illustrating the technical aspects of the present invention and not for limiting the same, and although the present invention has been described in detail with reference to the above embodiments, it should be understood by those of ordinary skill in the art that: modifications and equivalents may be made to the specific embodiments of the invention without departing from the spirit and scope of the invention, which are intended to be covered by the scope of the claims.
Claims (10)
1. The preparation method of the multifunctional hand sanitizer containing the aminopropanesulfonic inner salt type amphoteric structure is characterized by comprising the following steps of:
step one, mixing 20 to 25 parts of starch with 100 to 130 parts of deionized water and 0.2 to 0.3 part of high-temperature alpha-amylase according to parts by weight, heating to 90 to 95 ℃, and carrying out degradation reaction for 2.5 to 3.5 hours at a temperature to obtain a degraded starch solution;
adding 10-12 parts of N, N-dimethyl (methacryloyloxyethyl) aminopropanesulfonic acid inner salt and 6-8 parts of acrylamide into the degraded starch solution prepared in the step one, stirring and heating to 40-45 ℃, adding 4-6 parts of buffer solution to adjust the pH value of a system to 6.3-6.5, simultaneously dropwise adding 5-8 parts of horseradish peroxidase solution with the mass fraction of 0.09-0.15% and 8-10 parts of hydrogen peroxide solution with the mass fraction of 30%, controlling the dropwise adding time to 2.0-2.5 hours, and continuously preserving heat for reacting for 4.5-5.5 hours after the dropwise adding is finished to obtain modified starch;
step three, adding 25 to 30 parts of polyether macromonomer, 15 to 18 parts of N, N-dimethyl (methacryloyloxyethyl) aminopropanesulfonic acid inner salt and 250 to 282 parts of water into a reactor, uniformly stirring, keeping the temperature in the system at 40 to 50 ℃, and then adding 0.45 to 0.53 part of persulfate and uniformly stirring; then, dropwise adding a mixture of 44-52 parts of acrylic acid, 9-11 parts of sodium methacrylate, 0.36-0.42 part of vitamin C, 0.35-0.41 part of mercaptoethanol and 102-130 parts of water for 2.5-3 hours, continuing stirring and reacting for 2-3 hours after the dropwise adding, and regulating the pH value to 6.0-6.5 by using sodium hydroxide with the mass fraction of 40%, wherein the obtained product is an aminopropanesulfonic acid inner salt type amphoteric polymer;
mixing 26-30 parts of animal oleic acid, 30-35 parts of polyethylene glycol monomethyl ether and 0.6-0.8 part of p-toluenesulfonic acid in a reactor, stirring and heating to 110-120 ℃, preserving heat for 3-3.5 hours, and cooling to room temperature to obtain animal oleic acid polyethylene glycol monomethyl ether ester;
and step five, sequentially adding 46 to 53 parts of modified starch prepared in the step two, 19 to 23 parts of aminopropanesulfonic acid inner salt type amphoteric polymer prepared in the step three, 4 to 5 parts of sodium dodecyl sulfate, 5 to 6 parts of animal oleic acid polyethylene glycol monomethyl ether ester prepared in the step four, 2 to 3 parts of sodium tripolyphosphate, 0.7 to 0.9 part of citric acid, 0.05 to 0.08 part of triterpenoid saponin, 0.01 to 0.03 part of isothiazolinone, 0.1 to 0.3 part of essence, 2.5 to 3.2 parts of pigment and 55 to 74 parts of deionized water into a mixing container, and stirring for 0.5 to 1 hour to obtain the multifunctional hand sanitizer containing the aminopropanesulfonic acid inner salt type amphoteric structure.
2. The method for preparing the multifunctional hand sanitizer containing the aminopropanesulfonic inner salt type amphoteric structure according to claim 1, which is characterized in that: the buffer solution is prepared by dissolving 6.7-7.1 parts of sodium dihydrogen phosphate and 7.3-7.6 parts of disodium hydrogen phosphate in 100-120 parts of deionized water, and the pH value is 6.5-7.0.
3. The method for preparing the multifunctional hand sanitizer containing the aminopropanesulfonic inner salt type amphoteric structure according to claim 1, which is characterized in that: the polyether macromonomer is one or a mixture of several of allyl alcohol polyoxyethylene ether, methyl allyl alcohol polyoxyethylene ether and isopentenyl alcohol polyoxyethylene ether, the molecular weight is 2000-2400, the water content is less than or equal to 1%, the hydroxyl value is 2500-2800 mgKOH/g, the unsaturation degree is 0.5-0.63 mmol, and the pH value of a 1% aqueous solution is 5.0-7.0.
4. The method for preparing the multifunctional hand sanitizer containing the aminopropanesulfonic inner salt type amphoteric structure according to claim 1, which is characterized in that: the average relative molecular mass of the polyethylene glycol monomethyl ether is 2100-2200.
5. The method for preparing the multifunctional hand sanitizer containing the aminopropanesulfonic inner salt type amphoteric structure according to claim 1, which is characterized in that: the enzyme activity of the horseradish peroxidase is 330u/mg, and 0.05-0.08 part of horseradish peroxidase is dissolved in 50-60 parts of deionized water to prepare a horseradish peroxidase solution with the mass fraction of 0.09-0.15%.
6. The method for preparing the multifunctional hand sanitizer containing the aminopropanesulfonic inner salt type amphoteric structure according to claim 1, which is characterized in that: the animal oleic acid is light yellow transparent oily liquid, the acid value is 190-205 mgKOH/g, the saponification value is 192-215 mgKOH/g, the iodine value is 80-g I2/100g, the freezing point is less than 4 ℃, and the water content is less than 0.5%.
7. The method for preparing the multifunctional hand sanitizer containing the aminopropanesulfonic inner salt type amphoteric structure according to claim 1, which is characterized in that: the number average molecular weight of the modified starch is 6.8-9.6 ten thousand, and the number average molecular weight of the aminopropanesulfonic acid inner salt type amphoteric polymer is 8.9-12.4 ten thousand.
8. The method for preparing the multifunctional hand sanitizer containing the aminopropanesulfonic inner salt type amphoteric structure according to claim 1, which is characterized in that: the molecular structural formula of the modified starch prepared in the second step is
Wherein a, b and c are the number of structural units.
9. The method for preparing the multifunctional hand sanitizer containing the aminopropanesulfonic inner salt type amphoteric structure according to claim 1, which is characterized in that: the molecular structural formula of the aminopropanesulfonic acid inner salt type amphoteric polymer prepared in the step three is
Wherein a, b, c, d is the number of structural units.
10. The multifunctional hand sanitizer containing the aminopropanesulfonic inner salt type amphoteric structure prepared by the preparation method according to the claims 1-9, which is characterized in that: the pH value is 6.0-6.5, the viscosity is 810-980mPa.s, the foam height is 480-560 mm, and the sterilization rates for escherichia coli and staphylococcus aureus are 99.50-99.99% and 99.98-100%, respectively.
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