CN114276492A - Anti-ultraviolet thickening agent, preparation method thereof and disinfection washing-free hand rubbing gel - Google Patents
Anti-ultraviolet thickening agent, preparation method thereof and disinfection washing-free hand rubbing gel Download PDFInfo
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- 239000002562 thickening agent Substances 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000004659 sterilization and disinfection Methods 0.000 title description 6
- 239000000178 monomer Substances 0.000 claims abstract description 51
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 39
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 33
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229920001661 Chitosan Polymers 0.000 claims abstract description 20
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical group NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims abstract description 14
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims abstract description 14
- -1 hydroxyalkyl ester Chemical class 0.000 claims abstract description 11
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 9
- 229920000642 polymer Polymers 0.000 claims abstract description 6
- 238000010557 suspension polymerization reaction Methods 0.000 claims abstract description 3
- 239000003999 initiator Substances 0.000 claims description 31
- 239000003960 organic solvent Substances 0.000 claims description 14
- 239000002270 dispersing agent Substances 0.000 claims description 10
- 125000002057 carboxymethyl group Chemical group [H]OC(=O)C([H])([H])[*] 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 125000006724 (C1-C5) alkyl ester group Chemical group 0.000 claims description 4
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 4
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 claims description 4
- 239000011837 N,N-methylenebisacrylamide Substances 0.000 claims description 3
- FQPSGWSUVKBHSU-UHFFFAOYSA-N methacrylamide Chemical compound CC(=C)C(N)=O FQPSGWSUVKBHSU-UHFFFAOYSA-N 0.000 claims description 3
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 claims description 3
- 229920002818 (Hydroxyethyl)methacrylate Polymers 0.000 claims description 2
- IEVADDDOVGMCSI-UHFFFAOYSA-N 2-hydroxybutyl 2-methylprop-2-enoate Chemical compound CCC(O)COC(=O)C(C)=C IEVADDDOVGMCSI-UHFFFAOYSA-N 0.000 claims description 2
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 claims description 2
- GNSFRPWPOGYVLO-UHFFFAOYSA-N 3-hydroxypropyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCCCO GNSFRPWPOGYVLO-UHFFFAOYSA-N 0.000 claims description 2
- QZPSOSOOLFHYRR-UHFFFAOYSA-N 3-hydroxypropyl prop-2-enoate Chemical compound OCCCOC(=O)C=C QZPSOSOOLFHYRR-UHFFFAOYSA-N 0.000 claims description 2
- FYRWKWGEFZTOQI-UHFFFAOYSA-N 3-prop-2-enoxy-2,2-bis(prop-2-enoxymethyl)propan-1-ol Chemical group C=CCOCC(CO)(COCC=C)COCC=C FYRWKWGEFZTOQI-UHFFFAOYSA-N 0.000 claims description 2
- NDWUBGAGUCISDV-UHFFFAOYSA-N 4-hydroxybutyl prop-2-enoate Chemical compound OCCCCOC(=O)C=C NDWUBGAGUCISDV-UHFFFAOYSA-N 0.000 claims description 2
- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 claims description 2
- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical compound CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 claims description 2
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 2
- CNCOEDDPFOAUMB-UHFFFAOYSA-N N-Methylolacrylamide Chemical compound OCNC(=O)C=C CNCOEDDPFOAUMB-UHFFFAOYSA-N 0.000 claims description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 2
- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 claims description 2
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims description 2
- SUPCQIBBMFXVTL-UHFFFAOYSA-N ethyl 2-methylprop-2-enoate Chemical compound CCOC(=O)C(C)=C SUPCQIBBMFXVTL-UHFFFAOYSA-N 0.000 claims description 2
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 239000012074 organic phase Substances 0.000 claims 3
- CERQOIWHTDAKMF-UHFFFAOYSA-M Methacrylate Chemical compound CC(=C)C([O-])=O CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 claims 1
- 125000005233 alkylalcohol group Chemical group 0.000 claims 1
- 230000000249 desinfective effect Effects 0.000 claims 1
- 239000011261 inert gas Substances 0.000 claims 1
- 230000000977 initiatory effect Effects 0.000 claims 1
- 229940051841 polyoxyethylene ether Drugs 0.000 claims 1
- 229920000056 polyoxyethylene ether Polymers 0.000 claims 1
- 230000006750 UV protection Effects 0.000 abstract description 8
- 229920006254 polymer film Polymers 0.000 abstract description 5
- 230000009467 reduction Effects 0.000 abstract description 3
- 239000000499 gel Substances 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 12
- 238000012360 testing method Methods 0.000 description 7
- 238000002835 absorbance Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 229920002125 Sokalan® Polymers 0.000 description 4
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 229960001631 carbomer Drugs 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 230000000475 sunscreen effect Effects 0.000 description 2
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
- 125000005396 acrylic acid ester group Chemical group 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 229910000028 potassium bicarbonate Inorganic materials 0.000 description 1
- 235000015497 potassium bicarbonate Nutrition 0.000 description 1
- 239000011736 potassium bicarbonate Substances 0.000 description 1
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000516 sunscreening agent Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
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- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention belongs to the technical field of polymers, and particularly relates to an anti-ultraviolet thickening agent for an alcohol system, which is obtained by performing inverse suspension polymerization on the following monomers: 80-90 parts by weight of acrylic monomers; 4-8 parts of acrylic acid or methacrylic acid C1-C5 alkyl ester monomer; 1-2 parts of acrylamide monomer; 4-8 parts of acrylic acid or methacrylic acid C1-C5 hydroxyalkyl ester monomer; 1-2 parts of water-soluble chitosan; 0.8-2 parts of a crosslinking agent; the sum of the weights of the monomers is 100 parts by weight. The thickener has two advantages: firstly, a polymer film is formed on the skin surface of a user, the polymer film has certain ultraviolet resistance, secondly, the thickener has the performance of resisting the reduction of viscosity under the sunlight after being used for alcohol gel, and simultaneously, a preparation method of the thickener is also disclosed.
Description
Technical Field
The invention belongs to the field of polymers, and particularly relates to an anti-ultraviolet thickening agent for an alcohol system, a preparation method of the anti-ultraviolet thickening agent, and a disinfection wash-free hand-rubbing gel.
Background
The powdery acrylic acid thickener has been obtained for decades, is mainly obtained by copolymerizing acrylic acid, acrylic ester and optional other functional monomers in the presence of a cross-linking agent, and has a molecular structure containing 52-68% of acid groups, so that the powdery acrylic acid thickener has certain acidity and hydrophilic performance, and can be dissolved in water, ethanol and glycerol.
During use, wetting and neutralization are required. Since it contains certain acid groups, basic neutralization is required during application. The carboxyl of the alkali neutralized carbomer resin is ionized, and a coiled molecular chain stretches into a greatly expanded state due to the mutual repulsion of negative charges, so that the original volume is increased to about 1000 times, and the carbomer resin has the function of thickening. The commonly used neutralizing agents include sodium hydroxide, potassium bicarbonate, triethanolamine and the like (the pH value is adjusted to about 7, thus obtaining a crystal clear gel), which is also the reason why carbomer is sensitive to ions.
CN201310122778.5 discloses a preparation method of a powdery polyacrylic acid thickener, which comprises the steps of sequentially adding an organic solvent, a polymeric monomer, a comonomer, a neutralizer and a cross-linking agent into a reaction kettle at room temperature, and then introducing nitrogen to remove oxygen; starting stirring to uniformly mix reactants, heating to reaction temperature, dissolving an initiator in an organic solvent with the same reaction system, dropwise adding within 15-30 min, keeping the reaction temperature for 3-6 h, cooling, filtering, washing with the organic solvent, removing unreacted raw materials in the product, and vacuum-drying the filter cake at 40-50 ℃ for 24-48 h to obtain white powder.
This is a conventional method of preparation of powdered thickeners common in the art.
Consumers pay more and more attention to personal hygiene and epidemic prevention and control at present, and the alcohol gel has wide demand. Alcohol gels are applied to the skin of the consumer and, after evaporation of the alcohol, form a very thin polymer film on the skin.
The technical problem that the present scheme will solve is: how to improve the ultraviolet resistance of the alcohol sterilization gel.
Disclosure of Invention
The invention aims to provide an anti-ultraviolet thickening agent for an alcohol system and a preparation method thereof, and the thickening agent has the advantages of two aspects: firstly, a polymer film is formed on the skin surface of a user, the polymer film has certain ultraviolet resistance, and secondly, the thickening agent has the performance of resisting the reduction of viscosity under sunlight after being used for alcohol gel.
Meanwhile, the invention also provides a disinfection wash-free hand-rubbing gel.
The technical scheme of the invention is as follows:
an anti-ultraviolet thickening agent for alcohol systems is obtained by carrying out reversed phase suspension polymerization on the following monomers:
80-90 parts by weight of acrylic monomers;
4-8 parts of acrylic acid or methacrylic acid C1-C5 alkyl ester monomer;
1-2 parts by weight of acrylamide monomer (the monomer does not contain acrylamide monomer with crosslinking capacity, and is generally selected to be acrylamide or methacrylamide);
4-8 parts of acrylic acid or methacrylic acid C1-C5 hydroxyalkyl ester monomer;
1-2 parts of water-soluble chitosan;
0.8-2 parts of a crosslinking agent;
the sum of the weights of the monomers is 100 parts by weight.
In the above mentioned ultraviolet resistant thickener for alcohol system, the acrylamide monomer is acrylamide or methacrylamide; the acrylic monomer is acrylic acid or methacrylic acid.
In the above mentioned 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 hydroxyalkyl acrylate monomer of acrylic acid or methacrylic acid is at least one of hydroxyethyl acrylate, hydroxyethyl methacrylate, hydroxypropyl acrylate, hydroxypropyl methacrylate, hydroxybutyl acrylate and hydroxybutyl methacrylate.
In the above anti-ultraviolet thickener for alcohol system, the water-soluble chitosan is carboxymethyl chitosan.
In the above mentioned anti-ultraviolet 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 thickening agent for the alcohol system, which comprises the following steps:
step 1: adding an organic solvent, a dispersant and a monomer into a reactor, and heating to 60-80 ℃ under 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 finished;
and step 3: adding initiator solution for eliminating residual monomer at one time, reacting for 0.5-1 hr, filtering, and drying.
In the above preparation method of the anti-ultraviolet thickener for alcohol systems, the weight ratio of the organic solvent to the monomer is 2-3: 1.
In the above preparation method of the anti-ultraviolet thickener for alcohol system, the amount 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 above preparation method of the anti-ultraviolet thickener for alcohol systems, the initiator is azobisisoheptonitrile or azobisisobutyronitrile, and the initiator is 0.25-0.5% of the weight of the monomer.
In addition, the invention also provides a disinfection wash-free hand-rubbing gel which contains 0.2-1.0% of the thickening agent, wherein the thickening agent is as described in any one of the above.
The invention has the following beneficial effects:
the monomer of the invention consists of acrylic acid monomer, C1-C5 alkyl ester monomer of acrylic acid or methacrylic acid, acrylamide monomer, C1-C5 hydroxyalkyl ester monomer of acrylic acid or methacrylic acid, water-soluble chitosan and cross-linking agent, wherein, as a framework, the acrylic acid monomer and the acrylic acid ester monomer are matched with the cross-linking agent to be a framework structure of a common thickening agent, acrylamide and amino in the water-soluble chitosan have better affinity, when the acrylamide exists in a system as a comonomer, the water-soluble chitosan can be stably connected in a cross-linked network system, and as the chitosan has certain anti-ultraviolet capability, the anti-ultraviolet capability of the chitosan can be exerted to a greater extent after the chitosan is stably added into the cross-linked network, and simultaneously, the water-soluble chitosan has carboxyl and a large amount of hydroxyl, the swelling performance of the polymer in alcohol solution can be improved by the combined action of the polymer and C1-C5 hydroxyalkyl ester monomers of acrylamide, acrylic acid or methacrylic acid, and the ultraviolet resistance of the polymer is improved on the other hand.
Detailed Description
The technical solution of the present invention will be described in further detail with reference to the following embodiments, but the present invention is not limited thereto.
Example 1
A method for preparing an anti-ultraviolet thickening agent for an alcohol system comprises the following steps:
step 1: adding an organic solvent, a dispersant and a monomer into a reactor, and heating to 70 ℃ under an inert environment;
step 2: dropwise adding the initiator solution into the reactor for 2h, and continuing to react for 2h after the dropwise addition of the initiator is finished;
and step 3: adding initiator solution (the initiator in the step accounts for about 10% of the total initiator) for removing residual monomers at one time, reacting for 1h, finishing 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 seen in table 1 below:
table 1 formula table
Example 2
A method for preparing an anti-ultraviolet thickening agent for an alcohol system comprises the following steps:
step 1: adding an organic solvent, a dispersant and a monomer into a reactor, and heating to 70 ℃ under an inert environment;
step 2: dropwise adding the initiator solution into the reactor for 2h, and continuing to react for 2h after the dropwise addition of the initiator is finished;
and step 3: adding initiator solution (the initiator in the step accounts for about 10% of the total initiator) for removing residual monomers at one time, reacting for 1h, finishing 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 seen in table 2 below:
table 2 formula table
Example 3
A method for preparing an anti-ultraviolet thickening agent for an alcohol system comprises the following steps:
step 1: adding an organic solvent, a dispersant and a monomer into a reactor, and heating to 70 ℃ under an inert environment;
step 2: dropwise adding the initiator solution into the reactor for 2h, and continuing to react for 2h after the dropwise addition of the initiator is finished;
and step 3: adding initiator solution (the initiator in the step accounts for about 10% of the total initiator) for removing residual monomers at one time, reacting for 1h, finishing 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 seen in table 3 below:
table 3 formula table
Example 4
An anti-UV thickener for alcohol systems is prepared in the same manner as in example 1, with reference to the following Table 4:
table 4 formula table
Example 5
An anti-UV thickener for alcohol systems is prepared in the same manner as in example 1, with reference to the following Table 4:
table 4 formula table
Comparative example 1
A thickener for alcohol systems is prepared in the same manner as in example 1, with reference to the following Table 6:
table 6 formula table
Comparative example 2
A thickener for alcohol systems is prepared in the same manner as in example 1, with reference to the following Table 7:
performance testing
1. An ultraviolet resistance test, which refers to QB/T2410-1998 (ultraviolet absorbance method for evaluating the sunscreen effect in the UVB region of sunscreen cosmetics), and measures the absorbance of the product at a wavelength of 280-320 nm; the absorbance at 5 different wavelengths was measured at 10nm intervals and the average value of the absorbance was evaluated.
Sample preparation: dispersing the thickener powder into 65 vol% ethanol solution, and adjusting pH to be neutral to obtain 0.4% gel system; the samples relate to example 1, example 4, comparative example 1, comparative example 2; wherein in the gel system containing the comparative example 1, carboxymethyl chitosan which is 2 percent of the weight of the thickener powder is added into the gel system and the uniform dispersion and dissolution are ensured. Finally, samples 1 to 4 were 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 the solution | Sample 1 | Sample 2 | Sample 3 | Sample No. 4 |
| A | 0.975 | 1.131 | 0.733 | 0.751 |
Through the tests, the sample 2 can achieve the medium ultraviolet protection effect, and the samples 1, 3 and 4 can only achieve the minimum ultraviolet protection effect.
2. Sunshine viscosity change test
Sample preparation: dispersing the thickener powder into 65 vol% ethanol solution, and adjusting pH to be neutral to obtain 0.4% gel system; the samples relate to example 1, example 4, comparative example 1, comparative example 2; wherein in the gel system containing the comparative example 1, carboxymethyl chitosan which is 2 percent of the weight of the thickener powder is added into the gel system and the uniform dispersion and dissolution are ensured. Finally, samples 1 to 4 were obtained (corresponding to example 1, example 4, comparative example 1+ 2% carboxymethyl chitosan, comparative example 2, respectively in this order)
Samples 1 to 4 tested the viscosity of the primary system after the preparation was completed;
the 4 samples were placed in a summer daytime environment with good outdoor lighting at an ambient temperature of 34 ℃ for 3 days. After 3 days, the samples were placed in a 25 ℃ incubator at a constant temperature for 1 hour to measure the viscosity.
Test results refer to Table 9
TABLE 9 Change in viscosity
The reason why the resistance of sample 2 to sunlight viscosity reduction is the strongest is found through the test is that the stability of carboxymethyl chitosan in the system can be improved and the exertion of the ultraviolet resistance of carboxymethyl chitosan can be improved in the presence of acrylamide, hydroxymethyl acrylamide and N, N-methylene bisacrylamide.
Claims (10)
1. An anti-ultraviolet thickening agent for alcohol systems, characterized by comprising the following steps:
step 1: dissolving a monomer and a dispersant in an organic solvent to obtain an organic phase;
step 2: placing 60-70 wt% of organic phase in a reactor, introducing inert gas, heating to an initiation temperature, and dropwise adding the rest organic phase and an initiator; the dripping time is maintained for 4 to 6 hours;
and step 3: adding an initiator for eliminating residual monomers, reacting for 0.5-1h, and finishing the reaction;
the monomer comprises C1-C5 alkyl ester of acrylic acid, acrylic acid or methacrylic acid, C10-C20 alkyl ester of acrylic acid or methacrylic acid, and long-chain alkyl alcohol polyoxyethylene ether methacrylate
The polymer is obtained by inverse suspension polymerization of the following monomers:
acrylic monomer 80-90 weight parts
4-8 parts by weight of acrylic acid or methacrylic acid C1-C5 alkyl ester monomer
1-2 parts by weight of acrylamide monomer
4-8 parts by weight of C1-C5 hydroxyalkyl acrylate monomer of acrylic acid or methacrylic acid
1-2 parts of water-soluble chitosan;
0.8-2 parts of a crosslinking agent;
the sum of the weights of the monomers is 100 parts by weight.
2. The UV-resistant thickener for alcohol systems as claimed in claim 1, wherein the acrylamide-based monomer is acrylamide or methacrylamide; the acrylic monomer is acrylic acid or methacrylic acid.
3. The UV resistant thickener for alcohol system as claimed in claim 1, wherein 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 hydroxyalkyl acrylate monomer of acrylic acid or methacrylic acid is at least one of hydroxyethyl acrylate, hydroxyethyl methacrylate, hydroxypropyl acrylate, hydroxypropyl methacrylate, hydroxybutyl acrylate and hydroxybutyl methacrylate.
4. The UV resistant thickener for alcohol systems as claimed in claim 1, wherein the water soluble chitosan is carboxymethyl chitosan.
5. The UV resistant thickener for alcohol systems as claimed in claim 1, wherein the cross-linking agent is pentaerythritol triallyl ether or N, N-methylenebisacrylamide or methylol acrylamide.
6. A preparation method of an anti-ultraviolet thickening agent for an alcohol system is characterized by comprising the following steps:
step 1: adding an organic solvent, a dispersant and a monomer into a reactor, and heating to 60-80 ℃ under 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 finished;
and step 3: adding initiator solution for eliminating residual monomer at one time, reacting for 0.5-1 hr, filtering, and drying.
7. The method of claim 6, wherein the weight ratio of the organic solvent to the monomer is 2-3: 1.
8. The method for preparing an anti-UV thickener for alcohol systems according to claim 6, wherein the amount of the dispersant is 2.5 to 4% by weight based on the monomer; the dispersing agent is at least one of polyoxyethylene 30 dipolyhydroxystearate and span-80.
9. The method of claim 6, wherein the initiator is azobisisoheptonitrile or azobisisobutyronitrile, and the initiator is 0.25-0.5% by weight of the monomer.
10. A disinfecting wash-free hand rub gel comprising from 0.2% to 1.0% of a thickening agent, said thickening agent being as claimed in any one of claims 1 to 5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210056693.0A CN114276492B (en) | 2022-01-19 | 2022-01-19 | Ultraviolet-resistant thickener, preparation method thereof and disinfection no-wash hand-rubbing gel |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210056693.0A CN114276492B (en) | 2022-01-19 | 2022-01-19 | Ultraviolet-resistant thickener, preparation method thereof and disinfection no-wash hand-rubbing gel |
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| CN114276492A true CN114276492A (en) | 2022-04-05 |
| CN114276492B CN114276492B (en) | 2023-11-28 |
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| CN115466346A (en) * | 2022-09-29 | 2022-12-13 | 中国天辰工程有限公司 | Preparation method of polymer thickener in polar solvent |
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| 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 |
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| 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 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115466346A (en) * | 2022-09-29 | 2022-12-13 | 中国天辰工程有限公司 | Preparation method of polymer thickener in polar solvent |
| CN115466346B (en) * | 2022-09-29 | 2024-05-07 | 中国天辰工程有限公司 | Preparation method of polymer thickener in polar solvent |
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