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Method for preparing polymerizable photoinitiators

A technology of polymerization photoinitiator and polymerization inhibitor, which is applied in the field of light curing, can solve the problems of high corrosion, complicated method, high toxicity, etc., and achieve the effect of lowering melting point, increasing compatibility and preventing yellowing

Inactive Publication Date: 2016-08-17
NANCHANG HANGKONG UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Wang Yiheng et al [Synthesis, characterization and application of a hydrophobic polymerizable photoinitiator [J], Synthetic Fiber, 2015, 44(5), 1-5] with 2-hydroxy-4'-(2-hydroxyethyl Oxygen)-2-methylpropiophenone and methacryloyl chloride were used as raw materials to synthesize a hydrophobic polymerizable UV photoinitiator 2-(p-2-hydroxyl-2methylpropiophenone)- Hydroxyethyl methacrylate (HMEM), similar to the application method, but the method has used volatile or toxic, expensive acryloyl chloride (flash point 16, boiling point 75, flammable, highly corrosive, highly toxic , volatile, more expensive), the method adopted is more complicated, and the yield is lower

Method used

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  • Method for preparing polymerizable photoinitiators
  • Method for preparing polymerizable photoinitiators
  • Method for preparing polymerizable photoinitiators

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Take a dried 250mL four-neck flask, respectively install a thermometer, a water separator, a condenser, and flush with nitrogen protection, and add 0.02mol (about 1.72g) of methacrylic acid and 0.01g of p-hydroxybenzoic acid to the flask, respectively. Mix ether and 50mL toluene evenly, add 0.02mol (about 4.48g) 2959, stir to dissolve it completely, add 0.04g catalyst methanesulfonic acid, adjust the reaction temperature to 100°C, and react for 4h. After the reaction, use a rotary evaporator to remove the toluene to obtain a crude product, dissolve the crude product in dichloromethane, and wash it with deionized water and saturated sodium bicarbonate solution several times, dry the washed organic phase with anhydrous magnesium sulfate, and remove it by filtration. Magnesium sulfate, the collected organic phase is further purified through column chromatography, wherein the developer in the silica gel column is a mixed solvent of sherwood oil and ethyl acetate, and its rat...

Embodiment 2

[0022] Take a dried 250mL four-neck flask, respectively install a thermometer, a water separator, a condenser, and flush with nitrogen protection, and add 0.02mol (about 1.72g) of methacrylic acid and 0.01g of p-hydroxybenzoic acid to the flask, respectively. Ether and 50ml of dichloromethane, mix well, add 0.02mol (about 4.48g) 2959, stir to dissolve it completely, add 0.04g catalyst methanesulfonic acid, adjust the reaction temperature to 100°C, and react for 4h. After the reaction, use a rotary evaporator to remove the toluene to obtain a crude product, dissolve the crude product in dichloromethane, and wash it with deionized water and saturated sodium bicarbonate solution several times, dry the washed organic phase with anhydrous magnesium sulfate, and remove it by filtration. Magnesium sulfate, the collected organic phase is further purified through column chromatography, wherein the developer in the silica gel column is a mixed solvent of sherwood oil and ethyl acetate, a...

Embodiment 3

[0024] Take a dried 250mL four-neck flask, respectively install a thermometer, a water separator, a condenser, and flush with nitrogen protection, and add 0.02mol (about 1.72g) of methacrylic acid and 0.01g of p-hydroxybenzoic acid to the flask, respectively. Ether and 50ml of dimethylformamide, mix well, add 0.02mol (about 4.48g) 2959, stir to dissolve it completely, add 0.04g catalyst methanesulfonic acid, adjust the reaction temperature to 100°C, and react for 4h. After the reaction, use a rotary evaporator to remove the toluene to obtain a crude product, dissolve the crude product in dichloromethane, and wash it with deionized water and saturated sodium bicarbonate solution several times, dry the washed organic phase with anhydrous magnesium sulfate, and remove it by filtration. Magnesium sulfate, the collected organic phase is further purified through column chromatography, wherein the developer in the silica gel column is a mixed solvent of sherwood oil and ethyl acetate,...

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Abstract

The invention discloses a method for preparing polymerizable photoinitiators. The polymerizable photoinitiators are prepared from methacrylic acid and 2-hydroxyl-4'-(2'-hydroxyethoxy)-2-methyl propiophenone by the aid of direct esterification processes. The use quantity of polymerization inhibitors in a reaction system accounts for 0.01%-0.5% of the mass of the methacrylic acid, the use quantity of methane sulfonic acid which is a catalyst accounts for 0.1%-2% of the mass of the methacrylic acid, and a molar proportion of the methacrylic acid to the 2-hydroxyl-4'-(2'-hydroxyethoxy)-2-methyl propiophenone is 1:1-1.2. Each polymerization inhibitor is methoxyphenol or hydroquinone or 2-tertiary butylhydroquinone, and a solvent is toluene or dimethylformamide or tetrahydrofuran. The method has the advantages that the polymerizable photoinitiators are excellent in compatibility with monomers and resin in photo-curing systems fragments obtained after the polymerizable photoinitiators are subjected to illumination pyrolysis are low in migration rate in cured films and are anti-yellowing, excellent initiation effects can be realized, and the method can be applied to the field of photo-cured coating, printing ink, adhesive and the like; the method for synthesizing the polymerizable photoinitiators is low in cost, processes for preparing the polymerizable photoinitiators are simple and convenient, and obvious application effects can be realized.

Description

technical field [0001] The invention is a preparation method of a polymerizable photoinitiator, in particular to a polymerizable photoinitiator based on 2-hydroxyl-4'-(2-hydroxyethoxy)-2-methylpropiophenone (2959) The preparation of 2959-MMA belongs to the field of photocuring technology. technical background [0002] Since the 1960s, photocuring technology has attracted the attention of academic and industrial circles due to its advantages of energy saving, environmental protection, and rapidity. In recent years, research and application in this field in my country have also developed rapidly; An important part of the system has always been one of the focuses of people's attention. [0003] The traditional photoinitiator is a small molecule photoinitiator. The study found that although the small molecule photoinitiator can initiate photopolymerization and quickly obtain a photocured film, the solubility of the small molecule photoinitiator in the system is usually small. I...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C69/54
CPCC07C67/08
Inventor 钟荣曾泽张春辉
Owner NANCHANG HANGKONG UNIVERSITY
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