Synthesis method for ultraviolet photoinitiator XBPO

A synthesis method and initiator technology are applied in the field of environment-friendly high-efficiency ultraviolet photoinitiator XBPO synthesis, which can solve the problems of no phenyl bisulfite, no enterprise production, and difficult synthesis technology.

Inactive Publication Date: 2012-09-19
HUBEI GURUN TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] The full name of the high-efficiency ultraviolet photoinitiator XBPO is: phenylbis(2,4,6-trimethylbenzoyl)phosphine oxide, the synthesis technology is relatively difficult, and the product is exclusively produced by Ciba-Geigy, and the domestic There are not many synthetic studies, there is no suitable process route for phenylbis(2,4,6-trimethylbenzoyl)phosphine oxide, and no enterprise produces

Method used

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  • Synthesis method for ultraviolet photoinitiator XBPO
  • Synthesis method for ultraviolet photoinitiator XBPO
  • Synthesis method for ultraviolet photoinitiator XBPO

Examples

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Embodiment 1

[0023] Under an inert atmosphere, put 24g (0.5mol) of 50% sodium hydrogen (sodium hydride) and 300ml of benzene into a four-necked reaction flask (1000ml) equipped with a dropping funnel, a stirrer, and a thermometer, and slowly add phenyl dichloride dropwise. Phosphine 90g (0.5mol), the dropping temperature is controlled at 30-50°C, and the dropping time is 2-2.5 hours. After dropping, keep at this temperature for 0.5-1 hour, then cool down to 10°C in ice water. Add 101g (1.0mol) of triethylamine, then slowly add 200g (1.1mol) of 2,4,6-trimethylbenzoyl chloride dropwise, the dropwise temperature is controlled at 10-20°C, and the dropwise time is 3-3.5 hours. After dripping, keep at this temperature for 3 hours, and then slowly add 50ml of pure water dropwise after the heat preservation is over, the dropping temperature is controlled at 20-30°C, and the dropping time is 0.5-1.0 hours. After dripping, keep at this temperature for 0.5 hours, then slowly add 120g of 30% hydrogen...

Embodiment 2

[0025] Under an inert atmosphere, put 24g (0.5mol) of 50% sodium hydrogen (sodium hydride) and 500ml of toluene into a 1000ml four-necked reaction flask equipped with a dropping funnel, a stirrer, and a thermometer, and slowly add phenylphosphine dichloride dropwise. 90g (0.55mol), the dropping temperature is controlled at 30-50°C, and the dropping time is 2-2.5 hours. After dropping, keep at this temperature for 0.5-1 hour, then cool down to 10°C in ice water. Add 110g (1.09mol) of triethylamine, then slowly add 185g (1.0mol) of 2,4,6-trimethylbenzoyl chloride dropwise, the dropwise addition temperature is controlled at 10-20°C, and the dropwise addition time is 3-3.5 hours. After dripping, keep at this temperature for 3 hours, and then slowly add 50ml of pure water dropwise after the heat preservation is over, the dropping temperature is controlled at 20-30°C, and the dropping time is 0.5-1.0 hours. After dripping, keep at this temperature for 0.5 hours, then slowly add 120...

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Abstract

The invention provides a synthesis method for ultraviolet photoinitiator XBPO, which comprises the following steps of: putting sodium hydride and solvent benzene into a stirring reaction kettle, dropwise adding dichlorophenyl phosphine, putting catalyst organic base, dropwise adding 2, 4, 6-trimethyl benzoyl chloride, slowly dropwise adding pure water, slowly dropwise adding oxidant, dropwise adding 2% sodium hydroxide, washing with water, concentrating, crystallizing, filtering, and drying to obtain the ultraviolet photoinitiator. The synthesis method has the advantages that the photolytic product of the ultraviolet photoinitiator XBPO has two trimethyl benzoyl chloride and one phenyl phosphine acyl free radical, which are higher in initiation activity, compared with the photo initiation activity of TPO. The wide wave band has light sensitivity, so that the GR-XBPO not only can be independently used, but also can be used in cooperation with the other ultraviolet absorbers.

Description

technical field [0001] The invention relates to the field of synthesis method of environment-friendly high-efficiency ultraviolet photoinitiator XBPO. Background technique [0002] The full name of the high-efficiency ultraviolet photoinitiator XBPO is: phenylbis(2,4,6-trimethylbenzoyl)phosphine oxide, the synthesis technology is relatively difficult, and the product is exclusively produced by Ciba-Geigy, and the domestic There are not many synthetic studies, and there is no suitable process route for phenylbis(2,4,6-trimethylbenzoyl)phosphine oxide, and no enterprise produces it. Contents of the invention [0003] The present invention is aimed at phenylbis(2,4,6-trimethylbenzoyl)phosphine oxide, and the synthesis technology is relatively difficult. The product is exclusively produced by Ciba-Geigy, and there are not many domestic synthesis studies. There is no suitable process route for the production of phenylbis(2,4,6-trimethylbenzoyl)phosphine oxide, and there is no ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/40
Inventor 邹应全
Owner HUBEI GURUN TECH CO LTD
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