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UV cross-linking monomer and preparation method thereof, and application in preparation of fluorine-containing acrylate emulsion

A technology of cross-linking monomer and acrylate, applied to UV cross-linking monomer and its preparation method and application field in the preparation of fluorine-containing acrylate emulsion, can solve the problems of poor adhesion of substrates, increasing process complexity and the like , to achieve the effects of improved hydrophobicity, good emulsion polymerization stability and high conversion rate

Active Publication Date: 2021-07-27
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For the application of crosslinking agent on fabric finishing agent, self-crosslinking application exploration is more, as Chinese invention patent CN111662404 A discloses a kind of preparation method of self-crosslinking long fluorocarbon acrylate polymer emulsion, select diacetone propylene Amides, etc. are used as self-crosslinking agents; while the application of photocrosslinking in fabric finishing agents is less explored
Moreover, the Chinese invention patent CN111662404 A discloses a method for preparing a self-crosslinking long fluorocarbon acrylate polymer emulsion. Long carbon chain fluorine-containing monomers such as dodecafluoroheptyl methacrylate are selected, which are environmentally harmful and bioaccumulative. , secondly, the combination of anionic emulsification system and nonionic emulsification system is selected, which has poor adhesion to the substrate; finally, diacetone acrylamide is selected as a self-crosslinking agent, and a second crosslinking component needs to be added after the reaction Adipic acid dihydrazide, which increases the complexity of the process

Method used

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  • UV cross-linking monomer and preparation method thereof, and application in preparation of fluorine-containing acrylate emulsion
  • UV cross-linking monomer and preparation method thereof, and application in preparation of fluorine-containing acrylate emulsion
  • UV cross-linking monomer and preparation method thereof, and application in preparation of fluorine-containing acrylate emulsion

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0083] A UV crosslinking monomer was prepared by the following methods:

[0084] 1) After the 250 ml of four flasks were raised to 55 ° C, 41.77 g of 1,6-dibromohexane, 12.22 g of 4-hydroxybenzophenone and 51.12 g of 4-hydroxybenzophenone and 51.12 g of potassium carbonate were added, and 60 g was added. Acetone, peripheral temperature is 55 ° C, under mechanical stirring, with tin paper light shielding for 24 hours, yellow light is completely faded, discharged, extracted with dichloromethane, filtrate, chromatography (chromatography, petroleum ether is used The mixture of ethyl acetate, the volume ratio of the petroleum ether and ethyl acetate is 8: 1), spirus and dry, resulting in monochromo substituted diphenyl ketone;

[0085] 2) After the 450ml four-mouth flask is raised to 60 ° C, 6.97 g of monochromo-substituted diphenone, 4.77 g of methyl methacrylic acid, 15.33 g of potassium carbonate, then add 60 g of N, N-dimethyl Cyltamide, drowning with tin paper 24 hours, discharge,...

Embodiment 2

[0088] A UV crosslinking monomer was prepared by the following methods:

[0089] 1) After the 250ml four-mouth flask is raised to 60 ° C, 30.08 g of 1,6-dibromohexane, 12.22 g of 4-hydroxybenzophenone and 51.12 g of anhydrous potassium carbonate were added. Acetone, peripheral temperature of 55 ° C, under mechanical stirring, reacting with tin paper for 20 hours, yellow light fades, discharge, extracted with dichloromethane, filtrate, chromatography (chromatography is petroleum ether) The mixture of ethyl acetate, the volume ratio of the petroleum ether and ethyl acetate is 9: 1), spirus and dry, resulting in monochromo substituting diphenone;

[0090] 2) After the 250ml four-mouth flask is raised to 60 ° C, 6.43 g of monochromo-substituted diphenone, 4.40 g of methacrylic acid, 14.14 g of potassium anhydrous carbonate, then add 60 g of N, N-dimethyl Cyltamide, drowning with tin paper for 20 hours, discharge, filtrate, filtrate, chromatography, chromatography, hydrolytic acid mixt...

Embodiment 3

[0093] A UV crosslinking monomer was prepared by the following methods:

[0094] 1) After the 250ml four-mouth flask is raised to 65 ° C, 75 g 1, 6-dibromohexane, 12.22 g of 4-hydroxybenzophenone and 51.12 g of potassium anhydrous carbonate were added at once, and then 60 g of acetone, peripheral The temperature was 55 ° C, which was mechanically stirred, and the tin paper was allowed to react with tin paper for 24 hours, and the yellow light was completely faded, discharged, extracted with dichloromethane, filtered filtrate, chromatography (chromatography, ethyl acetate) The volume ratio of the mixture and the ethyl ester of petroleum ether and ethyl acetate was 10: 1), sputum and drying, resulting in monochromo substituted diphenyl ketone;

[0095] 2) After 250 ml of four flasks, 6.74 g of mono-bromoate substituted diphenone, 4.62 g of methyl methacrylic acid, 14.83 g of potassium carbonate, add 60 g of N, N-Dia. Cyltamide, with tin paper, it is 30 hours, discharged, filtered th...

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Abstract

The invention discloses a UV cross-linking monomer and a preparation method thereof, and application in preparation of a fluorine-containing acrylate emulsion. The preparation method of the monomer comprises the following steps: uniformly mixing 1, 6-dibromohexane, 4-hydroxybenzophenone, anhydrous potassium carbonate and an organic solvent, and carrying out shading reaction to obtain monobromo-substituted benzophenone; and uniformly mixing monobromo-substituted benzophenone, unsaturated acid, anhydrous potassium carbonate and an organic solvent, and carrying out shading reaction to obtain a reaction solution B, namely the UV cross-linking monomer. According to the invention, the preparation method of the UV cross-linking monomer is simple, efficient, low in cost and easy to industrialize; and the fluorine-containing acrylate emulsion prepared by using the UV cross-linked monomer is small in particle size, narrow in distribution and good in thermal stability, and the used fluorine-containing monomer does not contain C8 or above fluorine-containing alkyl chains, is environment-friendly, and can improve the water resistance of fabrics when being applied to a fabric finishing agent.

Description

Technical field [0001] The present invention belongs to the technical field of acrylate emulsion, and more particularly to a UV crosslinked monomer and a preparation method thereof and a use in the preparation of fluorine-containing acrylate emulsion. Background technique [0002] The fluoropolymer has a number of applications derived from its specific elements and structures. From the elements: Natural world, fluorine atom is the smallest atom except for hydrogen atoms; in addition, the fluorine element has the greatest electrocondolestability, and the CF bond can be much larger than the CH key energy, which has good thermal stability; : On the one hand, the conformational structure containing the fluoropolymer is a helical structure, that is, the fluorine-containing side chain is well wrapped with the main chain to form a fluorine shielding effect, so that the main chain is not damaged, on the other hand, the symmetrical chain structure makes the structure The surface of the fl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/10C07C69/54C07C45/64C07C49/84C08F220/24C08F220/14C08F220/18C08F220/20C08F220/30C08F2/30C08F2/28D06M15/277
CPCC07C67/10C07C69/54C07C45/64C08F220/24C08F2/30C08F2/28D06M15/277C07C49/84C08F220/14C08F220/1818C08F220/20C08F220/302
Inventor 任碧野邝树浓金志利
Owner SOUTH CHINA UNIV OF TECH
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