Photo-thermal free radical polymerization preparation method and application of vinyl polymer

A vinyl polymer, free radical technology, applied in the field of materials, can solve the problems of uneven reaction, affecting performance, unfavorable production environment, etc.

Inactive Publication Date: 2019-11-08
成都辉聚光电材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the problems with this scheme are: 1. It is necessary to add a terminator, such as a phenolic chemical reagent, to terminate the reaction at an appropriate degree of reaction, but a slight excess of the terminator will affect the subsequent curing and the performance of the PSA; There is a large amount of unreacted vinyl monomer in the compound that ends the polymerization reaction, which has a strong pungent smell and is extremely unfavorable to the production environment
Chinese invention patents CN 104854140 A and CN101331161 A respectively disclose a method of gap-type bulk polymerization. The former uses a high-energy ionizing radiation source to initiate polymerization, and the latter uses a method of thermal initiation to partially polymerize vinyl monomers and cool down. Then transfer to the second container to add other ingredients and continue the polymerization reaction to completion. Basically, it is a bulk polymerization method without stirring, but the bulk polymerization without stirring makes the reaction uneven and the product has more gels.

Method used

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  • Photo-thermal free radical polymerization preparation method and application of vinyl polymer

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Comparison scheme
Effect test

Embodiment 1

[0071] Solvent-free light / heat-initiated polymerization: soft monomer isononyl acrylate, hard monomer methyl methacrylate and vinyl acetate, functional monomer hydroxypropyl acrylate and acryloyl morpholine, the total amount of the above vinyl monomers is 100g ,Design Tg-40℃, 0.3g photoactive monomer 4-(acryloyloxy)benzophenone, add together with 0.1g photoinitiator TPO, 0.1g thermal initiator AIBN and 0.15g dodecyl mercaptan A 250ml three-neck round bottom flask is equipped with a thermometer, a reflux condenser and a nitrogen inlet, and the nitrogen is connected to a liquid-sealed tube from the top of the reflux condenser. Start stirring, pass 99.999% pure nitrogen for 10 minutes, irradiate the glass bottle with a 15W 365 / 395nm mixed wavelength LED lamp, the temperature will start to rise in about 10 seconds, stop the light when the temperature rises to 65°C, and the temperature in the reactor will continue Rise, there is obvious solvent reflux in the bottle, rise to the hig...

Embodiment 2

[0074] Light / heat initiated polymerization: soft monomer butyl acrylate, hard monomer isobornyl acrylate and vinyl acetate, functional monomer: hydroxypropyl acrylate, N-vinylpyrrolidone, design Tg-13℃, photoinitiator TPO , carry out photopolymerization after stirring and removing oxygen, then turn off the light, add a solution of ethyl acetate dissolved in photoactive monomer 4-(acryloyloxy)fluorenone containing aryl ketone and thermal initiator BPO, and then react for 1h , followed by devolatilization at 120°C and 3kPa, and the rest of the operations were similar to Example 1.

Embodiment 3

[0076] Solvent light / heat initiated polymerization: soft monomer 12 alkyl acrylate, 2(2-ethoxyethoxy) ethyl acrylate, hard monomer methyl methacrylate, cyclohexyl acrylate, functional monomer Hydroxypropyl acrylate, tetrahydrofuryl acrylate, design Tg-54°C, solvent ethyl acetate 10w%, photoinitiator TPO, semi-thermal initiator AIBN, and chain transfer agent mercaptoethanol are mixed to deoxygenate and carry out photopolymerization, and then turn off the light; Subsequently, the solution of ethyl acetate dissolved with the photoactive monomer 4-(2-acryloyloxyethoxy)-benzophenone containing aryl ketone and the other semi-thermal initiator tert-butyl peroxyacetate was exposed to light. Drop in within 15 minutes after stopping, and after another 1 hour of reaction, then add 0.1w% antioxidant 168 of the total amount of polymerization and 0.8w% antioxidant 1010 of the total amount of polymer; then pump into the surface renewal type devolatilization device, and the rest of the operat...

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Abstract

The invention discloses a photo-thermal free radical polymerization preparation method of a vinyl polymer and an application of the polymer. The method uses a photo/thermal composite initiator to initiate polymerization of a vinyl monomer, firstly a photoinitiated polymerization reaction is performed, and a thermal polymerization reaction is performed after the thermal polymerization reaction temperature is achieved. The method for preparing the vinyl polymer provided by the invention can reduce energy consumption, reduce reaction time, and improve production efficiency, and the product has amore uniform structure, better performance, a lower gelation rate or even no gel and a higher conversion rate of the monomer; and the vinyl polymer prepared by the method can be used for coating and photocrosslinking products.

Description

technical field [0001] The invention belongs to the technical field of materials, and in particular relates to a photothermal free radical polymerization preparation method of a vinyl polymer and an application of the polymer. Background technique [0002] The free radical polymerization reaction of vinyl monomer is a chain reaction, which is fast and releases a large amount of heat, which increases the temperature of the material, and the high temperature will further trigger the reaction of more vinyl monomers. If the heat cannot be removed, the reaction temperature will rise rapidly , and may even cause the temperature to rise "instantly", leading to a runaway reaction. Solution polymerization is a technical process in which the heat of polymerization is taken away by solvent boiling. At the same time, the solvent reduces the viscosity of the reaction system and facilitates stirring to make the reaction uniform. However, due to the requirements of energy saving and envir...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F220/18C08F220/14C08F218/08C08F220/20C08F226/06C08F220/30C08F220/28C08F226/10C08F2/50C09J7/38C09J133/08
CPCC08F2/50C08F220/18C09J133/14C09J139/06C09J7/385C09J2301/302
Inventor 王跃川鲜磊
Owner 成都辉聚光电材料有限公司
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