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Photoinitiator for ultraviolet light curing agent and manufacturing method thereof

A manufacturing method and technology of photoinitiator, which are applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as inconsistent test results, and achieve the effects of simple manufacturing method, high yield and good solubility

Active Publication Date: 2013-03-27
TIANJIN JIURI NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] (2) The test result does not meet the requirements of the following formula: ∑(x i / y i -1) <15.0, where:

Method used

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  • Photoinitiator for ultraviolet light curing agent and manufacturing method thereof
  • Photoinitiator for ultraviolet light curing agent and manufacturing method thereof
  • Photoinitiator for ultraviolet light curing agent and manufacturing method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0031] Embodiment 1: the manufacture of 2-(4'-methylbenzoyl) methyl benzoate (concentrated sulfuric acid method)

[0032] In a 250ml four-neck flask equipped with mechanical stirring, add 24.0g 2-(4'-methylbenzoyl)benzoic acid, 72ml toluene and 16.0g methanol, after stirring evenly, slowly add 5.0ml concentrated sulfuric acid dropwise, heat Reflux water separation, TLC or liquid phase monitoring reaction end point, the reaction is complete, cool to room temperature, slowly add 20ml of water dropwise to dilute, separate the lower aqueous phase and discard, and use 5% NaOH aqueous solution (pH about 8) and water respectively for the organic phase. Washed once, dried over anhydrous sodium sulfate, and desolvated under low pressure to obtain 24.0 g of light yellow oil, 21.0 g of white crystals recrystallized with 40 ml of methanol, the yield was 82.7%, and the liquid phase content was 99.0%.

Embodiment 2

[0033] Embodiment 2: the manufacture of 2-(4'-methylbenzoyl) methyl benzoate (SOCl 2 Law)

[0034] In a 250ml four-necked flask equipped with a mechanical stirrer, add 24.0g 2-(4'-methylbenzoyl)benzoic acid, 72ml toluene and 16.0g methanol, after stirring evenly, slowly add 17.8g dropwise under ice bath Thionyl chloride, heated to reflux for water separation, TLC or liquid phase monitoring reaction end point, reaction was complete, cooled to room temperature, slowly added dropwise to 20ml water for dilution, separated the lower aqueous phase and discarded, organic phase with 5% NaOH aqueous solution (pH About 8) was washed with water once, dried over anhydrous sodium sulfate, and desolvated under low pressure to obtain 24.2g of a light yellow oil, and 21.4g of white crystals recrystallized with 40ml of methanol, with a yield of 85.0% and a liquid phase content of 99.0%.

Embodiment 3

[0035] Embodiment 3: the manufacture of 2-(4'-methylbenzoyl) methyl benzoate (p-toluenesulfonic acid method)

[0036] In a 250ml four-neck flask equipped with mechanical stirring, add 24.0g 2-(4'-methylbenzoyl)benzoic acid, 72ml toluene and 16.0g methanol, after stirring evenly, add 5.0g p-toluenesulfonic acid, heat Reflux to separate water, TLC or liquid phase to monitor the reaction end point, the reaction is complete, cool to room temperature, let stand to separate layers, separate the lower layer of water and discard, the organic phase is washed with 80ml of 5% NaOH aqueous solution (pH about 8) and water Once, dried over anhydrous sodium sulfate and desolvated under low pressure to obtain 23.0 g of light yellow oil, 18.4 g of white crystals recrystallized with 20 ml of methanol, yield 72.7%, liquid phase content 99.1%.

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Abstract

The invention relates to an aromatic ester photoinitiator for ultraviolet light-like curing and a manufacturing method thereof. The preparation method of the photoinitiator comprises two ways: a first method is to react aromatic carboxylic acid with alcohol in the presence of a catalyst to prepare the aromatic ester photoinitiator; and a second method is to react in two steps, ensure that the aromatic carboxylic acid and the alkali are acted under a backflow condition to obtain corresponding carboxylate and react the carboxylate with the diethyl sulfate to prepare the aromatic ester photoinitiator at the temperature of 0-50 DEG C. Two manufacturing methods provided by the invention have the advantages of easy operation, rapid reaction, high yield and the like.

Description

technical field [0001] The invention relates to a photoinitiator used in an ultraviolet light curing agent and a manufacturing method thereof. Background technique [0002] Photocuring technology is an efficient, environmentally friendly, energy-saving, high-quality material surface treatment technology, known as a new technology for the green industry in the 21st century. The most common is ultraviolet light curing, which uses ultraviolet light to quickly polymerize and crosslink chemically active liquid materials, and instantly solidify into solid materials. It has been widely used in printing, packaging, advertising, building materials, decoration, electronics, communications, computers, etc. , home appliances, automobiles, aviation, aerospace, instrumentation, sports, health and other industries. UV curing products mainly appear in the form of UV coatings, UV inks, UV adhesives, etc. UV curing products can be seen everywhere in people's daily life, and the use of UV cur...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F2/48C07C67/08C07C69/76
Inventor 赵国锋武瑞张齐徐新元熊高利毛桂红吕振波
Owner TIANJIN JIURI NEW MATERIALS CO LTD
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