Polymerizable macromolecule photoinitiator and preparation method thereof

A photoinitiator and macromolecule technology, applied in the field of macromolecular photoinitiator preparation, can solve the problems of small molecular weight of the initiator, poor initiation effect, low ultraviolet absorption, etc. The effect of simple operating conditions

Inactive Publication Date: 2012-10-24
HANGZHOU INST OF ADVANCED MATERIAL BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Benzophenone photoinitiator is the most widely used free radical type photoinitiator, but its ultraviolet absorption is low, and initiation effect is poor (R.Liska, Journal of Polymer Science PartA: polymerchemistry, 2002 (40): 1504-1518)
[0006] The above methods have the following disadvantages: 1. The molecular weight of the initiator is relatively small, the mobility is large, and free small molecules are easily generated during photolysis; 2. The molecule does not contain double bonds and cannot be polymerized by itself.

Method used

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  • Polymerizable macromolecule photoinitiator and preparation method thereof
  • Polymerizable macromolecule photoinitiator and preparation method thereof
  • Polymerizable macromolecule photoinitiator and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Synthesis of Hydrogen-Substituted Polymerizable Macromolecular Photoinitiators

[0026] Add 10g of 4-hydroxybenzophenone and 4.5g of formaldehyde solution into a three-necked flask, add 0.44g of NaOH, heat and stir to 95°C, and react for 2h; then raise the temperature to 150°C, carry out vacuum filtration reaction for 20min, cool down after the reaction Collect the product at 105°C, pour the product into water to precipitate, and obtain a light yellow macromolecular photoinitiator containing benzophenone after suction filtration. Dissolve the obtained light yellow macromolecular photoinitiator containing benzophenone in 21.2g of dichloromethane, and add 10.21g of triethylamine into the three-necked flask simultaneously for stirring, and dissolve 5.48g of acryloyl chloride in 11g of dichloromethane Slowly add the mixed solution to the three-neck flask dropwise within 3 hours, the reaction temperature is 0-5°C, after the dropwise addition, stir at room temperature for 3 h...

Embodiment 2

[0030] Synthesis of Methyl Substituted Polymerizable Macromolecular Photoinitiators

[0031] Add 10g of 4-hydroxybenzophenone and 4.5g of formaldehyde solution into a three-necked flask, add 0.44g of NaOH, heat and stir to 95°C, and react for 2h; then raise the temperature to 150°C, carry out vacuum filtration reaction for 20min, cool down after the reaction Collect the product at 105°C, pour the product into water to precipitate, and obtain a light yellow macromolecular photoinitiator containing benzophenone after suction filtration. The obtained light yellow macromolecular photoinitiator containing benzophenone was dissolved in 22g of dichloromethane, and 10.21g of triethylamine was added into a three-necked flask simultaneously for stirring, and 6.33g of methacryloyl chloride was dissolved in 13g of dichloromethane In methane, slowly add the mixed solution to the three-neck flask dropwise within 3 hours, the reaction temperature is 0-5°C, after the dropwise addition, stir a...

Embodiment 3

[0035] Synthesis of Methoxyl Substituted Polymerizable Macromolecular Photoinitiators

[0036] Add 10g of 4-hydroxybenzophenone and 4.6g of formaldehyde solution into a three-necked flask, add 0.5g of alkali, heat and stir to 95°C, and react for 2h; Cool to 105°C to collect the product, pour the product into water to precipitate, and obtain a light yellow macromolecular photoinitiator containing benzophenone after suction filtration. The obtained light yellow macromolecular photoinitiator containing benzophenone is dissolved in 21g of dichloromethane, joins in the there-necked flask simultaneously with 10.3g of triethylamine and stirs, and 7.3g of methoxyacryloyl chloride is dissolved in 15g of dichloromethane In methyl chloride, slowly add the mixed solution to the three-necked flask dropwise within 3 hours, the reaction temperature is 0-5°C, after the dropwise addition, stir at room temperature for 3 hours, and let it stand overnight. The yellow liquid obtained above was su...

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Abstract

The present invention relates to a polymerizable macromolecule photoinitiator and a preparation method thereof. The preparation method comprises: adding 4-hydroxybenzophenone and a formaldehyde solution to a three-necked flask filled with an alkali adopted as a catalyst, carrying out heating stirring to a temperature of 95 DEG C, and carrying out a reaction for 2 hours; heating to a temperature of 150 DEG C, carrying out a reaction, and carrying out a reduced pressure suction filtration reaction for 20 minutes; cooling to a temperature of 105 DEG C after completing the reaction, and collecting the product; pouring the product into water to carry out precipitation, and carrying out suction filtration to obtain a benzophenone-containing macromolecule photoinitiator; dissolving the benzophenone-containing macromolecule photoinitiator in an organic solvent, and simultaneously adding the benzophenone-containing macromolecule photoinitiator and a tertiary amine to the three-necked flask to carry out stirring; dissolving acryloyl chloride in an organic solvent, and slowly adding the organic solvent containing the acryloyl chloride to the mixing solution in a dropwise manner, wherein thereaction temperature is 0-5 DEG C; after completing the addition, stirring for 3 hours at a room temperature, and standing overnight; carrying out suction filtration, washing and drying on the resulting solution; and carrying out rotary evaporation to remove the solvent to obtain the polymerizable macromolecule photoinitiator. The photoinitiator prepared by the preparation method of the present invention has characteristics of large molecular weight, relatively small mobility, self-polymerization, and the like.

Description

technical field [0001] The invention belongs to the field of photosensitive molecular materials, and in particular relates to a preparation method of a polymerizable macromolecular photoinitiator containing benzophenone. Background technique [0002] Photopolymerization (also known as photocuring) is irradiated by light (ultraviolet light or visible light) on light-sensitive compounds, causing a series of photophysical and photochemical reactions to generate active fragments, which in turn trigger liquid oligomers. (including monomer) polymerization, and finally the process of instantly converting the liquid coating into a solid polymer material. [0003] The photoinitiator is very important in the photopolymerization system. It is related to whether the oligomer and diluent can quickly change from liquid to solid when the formulation system is irradiated with light. With the continuous development of science and technology and the increasing emphasis on environmental prote...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G8/30C08F2/48
Inventor 马贵平姜苹聂俊徐帅
Owner HANGZHOU INST OF ADVANCED MATERIAL BEIJING UNIV OF CHEM TECH
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