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Preparation method for phenyl bis(2,4,6-trimethylbenzoyl)phosphine oxide

A technology of trimethylbenzoyl and phenylbis, which is applied in the field of preparation of phenylbis(2,4,6-trimethylbenzoyl)phosphine oxide (819), can solve the problem of phenylbis(2) , 4,6-trimethylbenzoyl) technical scheme disclosure of phosphine oxide and other problems, to achieve the effects of environmental friendliness, low cost and easy industrialization

Active Publication Date: 2016-02-24
内蒙古久日新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The inventors of the present application have found that there is no technical scheme for the preparation of phenylbis(2,4,6-trimethylbenzoyl)phosphine oxide using triphenylphosphine as a starting material.

Method used

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  • Preparation method for phenyl bis(2,4,6-trimethylbenzoyl)phosphine oxide
  • Preparation method for phenyl bis(2,4,6-trimethylbenzoyl)phosphine oxide

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Embodiment 1

[0032] The preparation method of embodiment 1 phenyl bis (2,4,6-trimethylbenzoyl) phosphine oxide

[0033] 1) Under the protection of nitrogen, suspend metal sodium block (13.8g, 0.6mol) in 120ml toluene, heat until reflux, and stir vigorously to form a suspension of powdery sodium, then add triphenylphosphine dropwise under vigorous stirring (13.1g, 0.05mol), after dropping, add 6ml of tert-butanol and heat to reflux for reaction. After the reaction of triphenylphosphine is complete, cool down to room temperature, add phosphorus trichloride (13.7g, 0.1mol) dropwise, and Vigorously stir the reaction during the addition process, and heat to 100°C for the reaction after dropping, and monitor the reaction by TLC;

[0034] 2) Cool the mixture obtained in step 1) to 80°C, add 2,4,6-trimethylbenzoyl chloride (54.8g, 0.3mol) dropwise at this temperature, and react after dropping, keep warm for reaction, after the reaction is complete , add water to the reaction system, stir and reac...

Embodiment 2

[0036] The preparation method of embodiment 2 phenyl bis (2,4,6-trimethylbenzoyl) phosphine oxide

[0037] 1) Under the protection of nitrogen, suspend metal sodium block (13.8g, 0.6mol) in 120ml toluene, heat until reflux, and stir vigorously to form a suspension of powdery sodium, then add triphenylphosphine dropwise under vigorous stirring (13.1g, 0.05mol), after dropping, add 6ml of tert-butanol and chlorobenzene (3.2g, 0.03mol), heat to reflux for reaction, when the reaction of triphenylphosphine is complete, cool down to room temperature, add dropwise phosphorus trichloride ( 13.7g, 0.1mol), vigorously stir the reaction during the dropwise addition, heat to 100°C for the reaction after the dropwise addition, and monitor the reaction by TLC;

[0038] 2) Cool the mixture obtained in step 1) to 80°C, add 2,4,6-trimethylbenzoyl chloride (54.8g, 0.3mol) dropwise at this temperature, and react after dropping, keep warm for the reaction, after the reaction is complete , add wa...

Embodiment 3

[0040] The preparation method of embodiment 3 phenyl bis (2,4,6-trimethylbenzoyl) phosphine oxide

[0041] 1) Under the protection of nitrogen, suspend metal sodium block (13.8g, 0.6mol) in 120ml ethylbenzene, heat until reflux, and stir vigorously to form a suspension of powdery sodium, then add triphenyl triphenyl under vigorous stirring Phosphine (13.1g, 0.05mol), after dropping, add 6ml of tert-butanol and chlorobenzene (3.2g, 0.03mol), heat and reflux for reaction, when the reaction of triphenylphosphine is complete, cool down to room temperature, add phosphorus trichloride dropwise (13.7g, 0.1mol), stirred vigorously during the dropwise addition, heated to 100°C for reaction after dropping, and monitored the reaction by TLC;

[0042] 2) Cool the mixture obtained in step 1) to 80°C, add 2,4,6-trimethylbenzoyl chloride (54.8g, 0.3mol) dropwise at this temperature, and react after dropping, keep warm for the reaction, after the reaction is complete , add water to the react...

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Abstract

The invention discloses a preparation method for phenyl bis(2,4,6-trimethylbenzoyl)phosphine oxide. The preparation method comprises the following steps: selecting triphenylphosphine as a raw material for reactions with sodium metal and phosphorus halide in the presence of one or more catalysts; carrying out an acyl chloride reaction; carrying out oxidation to prepare phenyl bis(2,4,6-trimethylbenzoyl)phosphine oxide. The preparation method has the advantages of being easy in raw material obtaining, low in cost, easy to operate, environmentally friendly, and easy for industrialization.

Description

technical field [0001] The invention relates to a preparation process of phenylbis(2,4,6-trimethylbenzoyl)phosphine oxide (819), in particular to a process using triphenylphosphine as a raw material, which has the advantages of simple process, low cost and environmental protection. Friendly way to prepare 819. Background technique [0002] Phenylbis(2,4,6-trimethylbenzoyl)phosphine oxide is a very efficient bisacylphosphine oxide photoinitiator, suitable for the radiation polymerization of some unsaturated resins under ultraviolet light irradiation , its deep curing effect is ideal. Suitable for UV-curable varnish and paint systems, such as for wood, paper, metal, plastic, optical fiber and printing inks and prepreg systems, etc., especially suitable for white formulations and glass fiber reinforced polyester / styrene systems and with The light stabilizer is used in the outdoor varnish system and is an ideal photoinitiator for weather-resistant UV-curable coatings. Pheny...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/53
CPCC07F9/5337
Inventor 张齐武瑞敖文亮吴吉蒋雷韩时操
Owner 内蒙古久日新材料有限公司
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