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Preparation method of benzophenone photoinitiator

A technology of benzophenones and photoinitiators, applied in the direction of organic chemistry, can solve the problems of easy volatilization, low initiating activity, easy migration, etc., and achieve the effect of low volatility, high initiating activity and good stability

Pending Publication Date: 2021-07-23
优缔贸易(上海)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to solve the problem that the activity of benzophenone photoinitiator in the prior art is not high, and it is easy to migrate and volatilize in the curing process, and the preparation of a kind of benzophenone photoinitiator proposed method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] A kind of preparation method of benzophenone photoinitiator that the present invention proposes comprises the following steps:

[0022] S1. According to the mass ratio of 1:3, diphenylmethane was dissolved in ethanol to prepare a mixed solution for later use, and 4-(N-formyl-N-methyl)aminobenzoyl chloride was added to the reaction kettle with tetrahydrofuran, while stirring Add the mixed solution dropwise at a rate of 3ml / min. After the dropwise addition, stir the reaction for 1h, pour the reaction solution into ice water, filter and dry it with suction to obtain the intermediate product I, wherein, 4-(N-formyl-N -The mass ratio of methyl) aminobenzoyl chloride, tetrahydrofuran and mixed solution is 2:1.8:1;

[0023] S2. Add the intermediate product I into a reaction kettle equipped with acetonitrile, stir and dissolve, add 3-dimethoxycinnamic acid, and react for 1 hour at a temperature of 50°C. After the reaction is completed, add water and sodium hydroxide, Continue ...

Embodiment 2

[0026] A kind of preparation method of benzophenone photoinitiator that the present invention proposes comprises the following steps:

[0027] S1. According to the mass ratio of 1:3.2, diphenylmethane was dissolved in diethyl ether to prepare a mixed solution for later use, and 4-(N-formyl-N-methyl)aminobenzoyl chloride was added to the reaction kettle with tetrahydrofuran, while stirring Add the mixed solution dropwise at a rate of 3.ml / min. After the dropwise addition, stir and react for 1.2h, pour the reaction solution into ice water, filter and dry to obtain the intermediate product I, wherein 4-(N-formazol The mass ratio of acyl-N-methyl)aminobenzoyl chloride, tetrahydrofuran and mixed solution is 2:2:1.2;

[0028] S2. Add the intermediate product I to the reaction kettle equipped with acetonitrile, stir and dissolve, add 3-dimethoxycinnamic acid, and react at a temperature of 502°C for 1.5h. After the reaction is completed, add water and sodium hydroxide , continue to s...

Embodiment 3

[0031] A kind of preparation method of benzophenone photoinitiator that the present invention proposes comprises the following steps:

[0032] S1. According to the mass ratio of 1:3.4, diphenylmethane was dissolved in chloroform to prepare a mixed solution for later use, and 4-(N-formyl-N-methyl)aminobenzoyl chloride was added to the reaction kettle containing tetrahydrofuran, while stirring Add the mixed solution dropwise at a rate of 4ml / min. After the dropwise addition, stir the reaction for 1-2h, pour the reaction solution into ice water, filter and dry it with suction to obtain the intermediate product I, wherein 4-(N-formyl The mass ratio of -N-methyl) aminobenzoyl chloride, tetrahydrofuran and mixed solution is 2:2.5:1.1;

[0033] S2. Add the intermediate product I into a reaction kettle equipped with acetonitrile, stir and dissolve, add 3-dimethoxycinnamic acid, and react for 2 hours at a temperature of 55°C. After the reaction is completed, add water and sodium hydrox...

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Abstract

The invention belongs to the technical field of photoinitiator materials, in particular relates to a preparation method of a benzophenone photoinitiator, and solves the problems that in the prior art, the initiation activity of the benzophenone photoinitiator is not high, and the benzophenone photoinitiator is easy to migrate and volatilize in the curing process. The preparation method of the benzophenone photoinitiator comprises the following steps: reacting diphenylmethane with 4-(N-formyl-N-methyl) aminobenzoyl chloride to obtain an intermediate product I; reacting the intermediate product I with 3-dimethoxycinnamic acid, adding water and sodium hydroxide, and reacting to obtain an intermediate product II; the intermediate product II, 5-hydroxyindole-2-ethyl formate and 2-phenoxy ethyl acrylate are subjected to a reaction, and a final product is obtained. The molecular structure of the obtained photoinitiator is modified by introducing the methoxy group and the indole group, and the obtained benzophenone photoinitiator is low in volatilization, low in yellowing, low in migration, good in stability and high in initiation activity.

Description

technical field [0001] The invention relates to the technical field of photoinitiator materials, in particular to a preparation method of a benzophenone photoinitiator. Background technique [0002] Photopolymerization is essentially a reaction in which monomers are polymerized using light energy. Compared with traditional polymerization methods, photopolymerization has the characteristics of low energy required, environmental friendliness, reaction, and easy formation of scale. In recent years, photopolymerization has attracted more and more attention, and it has a wide range of applications in dental materials, 3D printing, inks, photoresists and other fields. The general photopolymerization system mainly includes the following three components: (1) oligomers (or prepolymers, prepolymerized monomers), which endow materials with basic physical and chemical properties; (2) monomers, also known as reactive diluents. (3) photoinitiator, which is used to generate active speci...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F2/48C07D209/42
CPCC08F2/48C07D209/42
Inventor 陈莉
Owner 优缔贸易(上海)有限公司
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