Styrene oligomer diphenyl ketone type photoprimer capable of initiating radiopolymerization and its prepn process

A technology of photoinitiator and benzophenone, which is applied in the field of radiation-initiating polymerization initiators, can solve the problems of limited popularization and application, high price, and limited application range, and achieve wide application prospects, broad absorption spectrum, compatible good sex effect

Inactive Publication Date: 2007-06-06
常州华钛化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the above two photoinitiators have solved the deficiencies of the existing small molecule photoinitiators to a certain extent, these two photoinitiators have not yet reached satisfactory performance indicators and cannot completely replace the existing ones. At the same time, their limited application range and high price also further limit their promotion and application.

Method used

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  • Styrene oligomer diphenyl ketone type photoprimer capable of initiating radiopolymerization and its prepn process
  • Styrene oligomer diphenyl ketone type photoprimer capable of initiating radiopolymerization and its prepn process
  • Styrene oligomer diphenyl ketone type photoprimer capable of initiating radiopolymerization and its prepn process

Examples

Experimental program
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Effect test

Embodiment 1

[0036] Embodiment 1, the preparation of benzoyl polystyrene linear oligomer

[0037] Add 720ml of dichloroethane to a 2L three-neck flask equipped with a stirrer, a separatory funnel with a calcium chloride drying tube, and a reflux condenser connected to an absorption gas device, and then add 40g of benzoyl peroxide while stirring and 200ml of styrene, heated to 80 ° C for about 4 hours to obtain a polystyrene oligomer solution. Cool down to room temperature, add 265 g of anhydrous aluminum trichloride in batches under stirring and raise the temperature to 40°C. Under vigorous stirring, 238 g (200 ml) of benzoyl chloride was added dropwise. After the reaction began to emit hydrogen chloride, the heating was stopped, and benzoyl chloride was added continuously for 4 hours. It was then refluxed for one hour, cooled to room temperature, slowly poured into 5 kg of crushed ice under stirring, and the upper oil layer was separated, washed successively with 5% sodium hydroxide sol...

Embodiment 2

[0038] Embodiment 2,2,4, the preparation of 6-trimethylbenzoyl polystyrene linear oligomer

[0039] Add 720ml of dichloroethane to a 2L three-neck flask equipped with a stirrer, a separatory funnel with a calcium chloride drying tube, and a reflux condenser connected to an absorption gas device, and then add 40g of benzoyl peroxide while stirring and 200ml of styrene, heated to 80 ° C for about 4 hours to obtain a polystyrene oligomer solution. Cool down to room temperature, add 265 g of anhydrous aluminum trichloride in batches under stirring and raise the temperature to 40°C. Under vigorous stirring, 300 g of 2,4,6-trimethylbenzoyl chloride was added dropwise. After the reaction started to release hydrogen chloride, the heating was stopped, and 2,4,6-trimethylbenzoyl chloride was added continuously for 5.5 hours. It was then refluxed for one hour, cooled to room temperature, slowly poured into 5 kg of crushed ice under stirring, and the upper oil layer was separated, washe...

example 3

[0040] Example 3, the preparation of p-methylbenzoyl poly(styrene-methyl methacrylate) linear oligomer

[0041] Add 350ml of carbon disulfide to a 1L three-neck flask equipped with a stirrer, a separatory funnel with a calcium chloride drying tube, and a reflux condenser connected to an absorption gas device, and then add 25g of benzoyl peroxide and 150ml of benzene under stirring. Ethylene and 50ml of methyl methacrylate were heated to 60°C for about 4 hours to obtain a poly(styrene-methyl methacrylate) solution. Cool down to room temperature, add 140 g of anhydrous aluminum trichloride in batches under stirring and raise the temperature to 35°C. Under vigorous stirring, 110 g (93 ml) of p-toluoyl chloride was added dropwise. After the reaction started to release hydrogen chloride, the heating was stopped, and p-toluyl chloride was continued to be added for 3 hours. It was then refluxed for one hour, cooled to room temperature, slowly poured into 3 kg of crushed ice under s...

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Abstract

The present invention is diphenyl ketone type photoprimer as styrene oligomer capable of initiating radiopolymerization. The oligomer is prepared through homopolymerizing or copolymerizing styrene or substituted styrene to form straight chain oligomer, the subsequent reaction with aluminum trichloride and corresponding acylating agent in carbon disulfide, nitrobenzene or other solvent to grafting diarone structure onto the benzene ring of the oligomer, so as to form macromolecule with molecular weight of 400-5000 and possessing radiation initiating characteristic. The macromolecule has the advantages one high initiating efficiency, low volatility, high migration resisting capacity, high environment compatibility, high resin compatibility, etc. and may be used widely in the radiopolymerization of polymer.

Description

technical field [0001] The invention relates to the field of radiation polymerization initiators, in particular to a styrene oligomer benzophenone photoinitiator capable of initiating radiation polymerization and a preparation method thereof. Background technique [0002] Radiation (or photo) initiator is an important component of radiation curing system. In the current industrial photocuring system, photoinitiator is an important factor that determines the curing rate and degree of curing of the system. However, the traditional photoinitiator is a small molecule containing photoactive groups, which has poor compatibility with polymers. Not only that, the photoinitiator and photolytic fragments remaining in the product are easy to migrate and volatilize, making the product aging and yellowing , Odor and toxicity appear, which restricts the application of light curing system in food and drug packaging. Photoinitiators with relatively large molecular weights are an effective ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F2/50C08F12/08
Inventor 董辅隆秦怀德
Owner 常州华钛化学有限公司
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