CN114276492B - Ultraviolet-resistant thickener, preparation method thereof and disinfection no-wash hand-rubbing gel - Google Patents

Ultraviolet-resistant thickener, preparation method thereof and disinfection no-wash hand-rubbing gel Download PDF

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CN114276492B
CN114276492B CN202210056693.0A CN202210056693A CN114276492B CN 114276492 B CN114276492 B CN 114276492B CN 202210056693 A CN202210056693 A CN 202210056693A CN 114276492 B CN114276492 B CN 114276492B
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parts
thickener
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ultraviolet
monomer
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CN114276492A (en
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马思伟
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Guangdong Star Lion Energy Technology Co ltd
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Guangdong Star Lion Energy Technology Co ltd
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Abstract

The invention belongs to the technical field of polymers, and in particular relates to an ultraviolet-resistant thickener for an alcohol system, which is prepared by reversed-phase suspension polymerization of the following monomers: 80-90 parts by weight of an acrylic monomer; 4-8 parts by weight of C1-C5 alkyl ester monomer of acrylic acid or methacrylic acid; 1-2 parts by weight of acrylamide monomer; 4-8 parts by weight of C1-C5 hydroxyalkyl ester monomer of acrylic acid or methacrylic acid; 1-2 parts by weight of water-soluble chitosan; 0.8-2 parts by weight of a cross-linking agent; the sum of the weights of the monomers is 100 parts by weight. The thickener has two advantages: firstly, a layer of polymer film is formed on the skin surface of a user, the polymer film has certain ultraviolet resistance, and secondly, the thickener can have anti-adhesion performance reduction under sunlight after being used for alcohol gel, and meanwhile, the preparation method of the thickener is also disclosed.

Description

Ultraviolet-resistant thickener, preparation method thereof and disinfection no-wash hand-rubbing gel
Technical Field
The invention belongs to the field of polymers, and particularly relates to an ultraviolet-resistant thickener for an alcohol system, a preparation method thereof and a disinfection hand-washing-free gel.
Background
Powdery acrylic thickeners have been known for decades, which are mainly obtained by copolymerizing acrylic acid, acrylic acid esters and optionally other functional monomers in the presence of a crosslinking agent, and which have a molecular structure containing 52 to 68% of acid groups, so that they have a certain acidity, have hydrophilic properties and are soluble in water, ethanol and glycerol.
During use, wetting, neutralization is required. Since it contains a certain acid group, alkaline neutralization is required during application. The carboxyl of the carbomer resin neutralized by alkalinity is ionized, and the contracted molecular chain is stretched to be in a very large expansion state due to the mutual repulsive action of negative charges, so that the original volume is increased to about 1000 times, and the thickening effect is realized. The common neutralizing agents are sodium hydroxide, potassium bicarbonate, triethanolamine and the like (pH is adjusted to about 7 to obtain crystal clear gel), which is also the reason why carbomers are sensitive to ions.
CN201310122778.5 discloses a preparation method of powdery polyacrylic acid thickener, which comprises the steps of adding organic solvent, polymeric monomer, comonomer, neutralizer and cross-linking agent into a reaction kettle in sequence at room temperature, and then introducing nitrogen to remove oxygen; stirring is started, reactants are uniformly mixed, the temperature is raised to the reaction temperature, an initiator is dissolved in an organic solvent which is the same as a reaction system, dripping is completed within 15-30 min, after the reaction temperature is kept for 3-6 h, cooling, filtering, washing with the organic solvent, removing unreacted raw materials in the product, and vacuum drying a filter cake at 40-50 ℃ for 24-48 h to obtain white powder.
This is a conventional method of preparing powdery thickeners that are common in the art.
At present, consumers are increasingly focusing on personal sanitation and epidemic prevention and control, and have wide demands on alcohol gel. The alcohol gel is smeared on the skin of a consumer, and a very thin polymer film is formed on the skin surface after the alcohol volatilizes.
The technical problem to be solved by the scheme is as follows: how to improve the ultraviolet resistance of the alcohol sterilization gel.
Disclosure of Invention
The invention aims to provide an ultraviolet-resistant thickener for an alcohol system and a preparation method thereof, and the thickener has two advantages: first, a polymer film is formed on the surface of the skin of the user, which has a certain resistance to ultraviolet rays, and second, the thickener can have resistance to decrease in resistance to adhesion under sunlight after being used in alcohol gel.
Meanwhile, the invention also provides a disinfection hands-free gel.
The technical scheme of the invention is as follows:
an ultraviolet resistant thickener for alcohol system is prepared by reversed phase suspension polymerization of the following monomers:
80-90 parts by weight of an acrylic monomer;
4-8 parts by weight of C1-C5 alkyl ester monomer of acrylic acid or methacrylic acid;
1-2 parts by weight of an acrylamide monomer (the acrylamide monomer does not contain acrylamide monomer with crosslinking capability, and is generally selected as acrylamide or methacrylamide);
4-8 parts by weight of C1-C5 hydroxyalkyl ester monomer of acrylic acid or methacrylic acid;
1-2 parts by weight of water-soluble chitosan;
0.8-2 parts by weight of a cross-linking agent;
the sum of the weights of the monomers is 100 parts by weight.
In the ultraviolet resistant thickener for alcohol system, the acrylamide monomer is acrylamide or methacrylamide; the acrylic monomer is acrylic acid or methacrylic acid.
In the ultraviolet resistant thickener for alcohol system, the C1-C5 alkyl ester monomer of acrylic acid or methacrylic acid is at least one of methyl acrylate, ethyl acrylate, butyl acrylate, methyl methacrylate and ethyl methacrylate;
the C1-C5 hydroxyl alkyl ester monomer of the acrylic acid or the methacrylic acid is at least one of hydroxyethyl acrylate, hydroxyethyl methacrylate, hydroxypropyl acrylate, hydroxypropyl methacrylate, hydroxybutyl acrylate and hydroxybutyl methacrylate.
In the ultraviolet resistant thickener for alcohol system, the water-soluble chitosan is carboxymethyl chitosan.
In the ultraviolet resistant thickener for alcohol system, the cross-linking agent is pentaerythritol triallyl ether or N, N-methylene bisacrylamide.
Meanwhile, the invention also discloses a preparation method of the ultraviolet-resistant thickener for the alcohol system, which comprises the following steps:
step 1: adding an organic solvent, a dispersing agent and a monomer into a reactor, and heating to 60-80 ℃ in an inert environment;
step 2: dropwise adding the initiator solution into the reactor for 1-4h, and continuing to react for 1-2h after the dropwise adding of the initiator is completed;
step 3: and (3) adding an initiator solution for eliminating residual monomers at one time, reacting for 0.5-1h, ending the reaction, filtering and drying.
In the preparation method of the ultraviolet resistant thickener for alcohol system, the weight ratio of the organic solvent to the monomer is 2-3:1.
In the preparation method of the ultraviolet resistant thickener for alcohol systems, the dosage of the dispersant is 2.5-4% of the weight of the monomer; the dispersing agent is at least one of polyoxyethylene 30 dipolyhydroxystearate and span-80.
In the preparation method of the ultraviolet resistant thickener for alcohol systems, the initiator is azodiisoheptonitrile or azodiisobutyronitrile, and the initiator is equivalent to 0.25-0.5% of the weight of the monomer.
In addition, the invention also provides a disinfection hand-washing-free gel, which contains 0.2% -1.0% of a thickener, wherein the thickener is any one of the above.
The beneficial effects of the invention are as follows:
the monomer of the invention is composed of acrylic acid monomer, C1-C5 alkyl ester monomer of acrylic acid or methacrylic acid, acrylamide monomer, C1-C5 hydroxy alkyl ester monomer of acrylic acid or methacrylic acid, water-soluble chitosan and cross-linking agent, wherein, as skeleton, acrylic acid monomer and acrylic acid ester monomer are matched with cross-linking agent to be the skeleton structure of common thickener, acrylamide has better affinity with amino in water-soluble chitosan, when acrylamide exists in the system as comonomer, water-soluble chitosan can be stably connected in the cross-linking network system, because chitosan has certain ultraviolet resistance, when the chitosan is stably added into the cross-linking network, the ultraviolet resistance can be exerted to a larger extent, meanwhile, the water-soluble chitosan has carboxyl and a large amount of hydroxyl groups, and the ultraviolet resistance swelling performance in alcohol solution can be improved under the combined action of the water-soluble chitosan and the C1-C5 hydroxy alkyl ester monomer of acrylamide, acrylic acid or methacrylic acid, thus the ultraviolet resistance swelling capacity of the polymer is improved on the other hand.
Detailed Description
The technical scheme of the present invention will be described in further detail below with reference to the specific embodiments, but the present invention is not limited thereto.
Example 1
The preparation method of the ultraviolet-resistant thickener for the alcohol system comprises the following steps:
step 1: adding an organic solvent, a dispersing agent and a monomer into a reactor, and heating to 70 ℃ in an inert environment;
step 2: dropwise adding the initiator solution into the reactor for 2 hours, and continuing to react for 2 hours after the dropwise adding of the initiator is completed;
step 3: and adding an initiator solution for eliminating residual monomers (the initiator in the step accounts for about 10% of the total initiator) at one time, reacting for 1h, ending the reaction, filtering and drying.
A small amount of organic solvent is used in the initiator solution, which has a negligible effect on the concentration of the system.
The amounts of the substances can be found in Table 1 below:
table 1 formulation table
Example 2
The preparation method of the ultraviolet-resistant thickener for the alcohol system comprises the following steps:
step 1: adding an organic solvent, a dispersing agent and a monomer into a reactor, and heating to 70 ℃ in an inert environment;
step 2: dropwise adding the initiator solution into the reactor for 2 hours, and continuing to react for 2 hours after the dropwise adding of the initiator is completed;
step 3: and adding an initiator solution for eliminating residual monomers (the initiator in the step accounts for about 10% of the total initiator) at one time, reacting for 1h, ending the reaction, filtering and drying.
A small amount of organic solvent is used in the initiator solution, which has a negligible effect on the concentration of the system.
The amounts of the substances can be found in Table 2 below:
table 2 formulation table
Example 3
The preparation method of the ultraviolet-resistant thickener for the alcohol system comprises the following steps:
step 1: adding an organic solvent, a dispersing agent and a monomer into a reactor, and heating to 70 ℃ in an inert environment;
step 2: dropwise adding the initiator solution into the reactor for 2 hours, and continuing to react for 2 hours after the dropwise adding of the initiator is completed;
step 3: and adding an initiator solution for eliminating residual monomers (the initiator in the step accounts for about 10% of the total initiator) at one time, reacting for 1h, ending the reaction, filtering and drying.
A small amount of organic solvent is used in the initiator solution, which has a negligible effect on the concentration of the system.
The amounts of the substances can be found in Table 3 below:
table 3 recipe table
Example 4
An ultraviolet resistant thickener for alcohol system was prepared in the same manner as in example 1, and the formulation was as shown in Table 4 below:
table 4 formulation table
Example 5
An ultraviolet resistant thickener for alcohol system was prepared in the same manner as in example 1, and the formulation was as shown in Table 4 below:
table 4 formulation table
Comparative example 1
A thickener for alcohol system was prepared in the same manner as in example 1, and the formulation was as shown in Table 6 below:
table 6 recipe table
Comparative example 2
A thickener for alcohol system was prepared in the same manner as in example 1, and the formulation was as shown in the following Table 7:
performance testing
1. Ultraviolet resistance test, reference QB/T2410-1998 (ultraviolet absorbance method for evaluating sun protection effect of UVB region of sun-protection cosmetic), measuring absorbance of product at wavelength of 280-320 nm; the absorbance at 5 different wavelengths was measured at a test interval of 10nm, and the average value of the absorbance was evaluated.
Sample preparation: dispersing thickener powder into 65vol% ethanol solution, and regulating pH to be neutral to obtain a gel system with the concentration of 0.4%; the samples relate to example 1, example 4, comparative example 1, comparative example 2; wherein in the gel system containing comparative example 1, carboxymethyl chitosan, which is 2% of the weight of the thickener powder, was added to the gel system and the dispersion and dissolution were ensured to be uniform. Samples 1 to 4 were finally obtained (corresponding to example 1, example 4, comparative example 1+2% carboxymethyl chitosan, comparative example 2, respectively, in this order)
Test results refer to Table 8
TABLE 8 average absorbance values
Absorbance of light Sample 1 Sample 2 Sample 3 Sample 4
A 0.975 1.131 0.733 0.751
Through the test, the sample 2 can achieve the moderate ultraviolet light protection effect, and the samples 1, 3 and 4 can only achieve the minimum ultraviolet light protection effect.
2. Solar viscosity change test
Sample preparation: dispersing thickener powder into 65vol% ethanol solution, and regulating pH to be neutral to obtain a gel system with the concentration of 0.4%; the samples relate to example 1, example 4, comparative example 1, comparative example 2; wherein in the gel system containing comparative example 1, carboxymethyl chitosan, which is 2% of the weight of the thickener powder, was added to the gel system and the dispersion and dissolution were ensured to be uniform. Samples 1 to 4 were finally obtained (corresponding to example 1, example 4, comparative example 1+2% carboxymethyl chitosan, comparative example 2, respectively, in this order)
Samples 1 to 4 were tested for primary system viscosity after configuration was completed;
the 4 samples were placed in an outdoor well lit summer daytime environment at 34℃for 3 days. After 3 days, the samples were uniformly placed in a incubator at 25℃and after 1 hour of incubation, the viscosity was measured.
Test results refer to Table 9
TABLE 9 viscosity Change
The test shows that the resistance of the sample 2 to sunlight viscosity reduction is strongest, and the reasons are that the stability of carboxymethyl chitosan in a system can be improved and the performance of the self ultraviolet resistance can be improved in the presence of acrylamide, methylol acrylamide and N, N-methylene bisacrylamide.

Claims (2)

1. The ultraviolet resistant thickener for the alcohol system is characterized in that the preparation method of the ultraviolet resistant thickener comprises the following steps:
step 1: adding an organic solvent, a dispersing agent and a monomer into a reactor, and heating to 70 ℃ in an inert environment;
step 2: dropwise adding the initiator solution into the reactor for 2 hours, and continuing to react for 2 hours after the dropwise adding of the initiator is completed;
step 3: adding an initiator solution for eliminating residual monomers at one time, reacting for 1h, ending the reaction, filtering and drying; the initiator in the step 3 accounts for 10% of the total amount of the initiator;
the monomer consists of the following components in parts by weight:
85 parts of acrylic acid;
2 parts of methyl acrylate;
2 parts of acrylamide;
5 parts of hydroxyethyl acrylate;
2 parts of carboxymethyl chitosan;
0.5 parts of methylol acrylamide;
0.5 part of N, N-methylene bisacrylamide.
2. A disinfecting, leave-on hand gel comprising from 0.2% to 1.0% of a thickener according to claim 1.
CN202210056693.0A 2022-01-19 2022-01-19 Ultraviolet-resistant thickener, preparation method thereof and disinfection no-wash hand-rubbing gel Active CN114276492B (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103450413A (en) * 2013-09-18 2013-12-18 苏州大学 Thickener for printing textiles and preparation method thereof
CN104877455A (en) * 2014-02-27 2015-09-02 真彩文具股份有限公司 A low-viscosity antibacterial gel-ink thickening agent and a preparing method thereof
CN112538132A (en) * 2020-12-08 2021-03-23 南京紫鸿生物科技有限公司 Preparation method of thickening polymer suitable for alcohol system
CN112876596A (en) * 2021-01-06 2021-06-01 广州市东雄化工有限公司 Solution type alcohol disinfection gel thickening agent and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103450413A (en) * 2013-09-18 2013-12-18 苏州大学 Thickener for printing textiles and preparation method thereof
CN104877455A (en) * 2014-02-27 2015-09-02 真彩文具股份有限公司 A low-viscosity antibacterial gel-ink thickening agent and a preparing method thereof
CN112538132A (en) * 2020-12-08 2021-03-23 南京紫鸿生物科技有限公司 Preparation method of thickening polymer suitable for alcohol system
CN112876596A (en) * 2021-01-06 2021-06-01 广州市东雄化工有限公司 Solution type alcohol disinfection gel thickening agent and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
棉织物壳聚糖杂化膜改性及防紫外线性能研究;高大伟等;《纺织导报》(第10期);第104-106页 *

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