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Preparation method of di (2,4,6-trimethylbenzoyl) phenyl phosphine oxide and (2,4,6-trimethylbenzoyl) diphenyl phosphine oxide

A technology of trimethylbenzoyl and diphenylphosphine oxide, which is applied in the fields of chemical instruments and methods, organic chemistry, and compounds of Group 5/15 elements of the periodic table, and can solve the problem that the by-product phenylphosphonic acid cannot be consumed, The theoretical yield can only reach 33% and other issues

Active Publication Date: 2015-09-16
TIANJIN MOSEN TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Chinese patents CN102942593A and CN103044485A also propose to use phenylphosphinic acid disproportionation to obtain phenylphosphine to prepare initiator 819, but the theoretical yield can only reach 33%, and the by-product phenylphosphonic acid cannot be consumed
[0008] There is not yet a method to produce the above two target products simultaneously with the same raw material and equipment

Method used

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  • Preparation method of di (2,4,6-trimethylbenzoyl) phenyl phosphine oxide and (2,4,6-trimethylbenzoyl) diphenyl phosphine oxide
  • Preparation method of di (2,4,6-trimethylbenzoyl) phenyl phosphine oxide and (2,4,6-trimethylbenzoyl) diphenyl phosphine oxide
  • Preparation method of di (2,4,6-trimethylbenzoyl) phenyl phosphine oxide and (2,4,6-trimethylbenzoyl) diphenyl phosphine oxide

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Embodiment 1

[0045] The preparation of two (2,4,6-trimethylbenzoyl) phenyl phosphine oxides, the steps are as follows:

[0046] (1) Add 150ml of re-distilled ether into a 250mL four-neck flask, purge and replace with nitrogen for 10 minutes, insert the gas inlet below the liquid level, and slowly introduce 6.8g of phosphine gas to make it fully absorbed in the solvent, Exhaust gas recycling.

[0047] (2) Add 23.7g of pyridine to the flask, control the temperature at 95-110°C, and add 24.8g of chlorobenzene dropwise into the flask while stirring. After the addition was complete, the mixture was incubated for 2 hours. 38.4g of 2,4,6-trimethylbenzoyl chloride was added dropwise at a controlled temperature of 45-50°C for reaction, and after the addition was complete, the mixture was kept warm for 2 hours.

[0048] (3) Control the temperature at 30-45°C, add 45g of 30% hydrogen peroxide dropwise, keep the reaction at 30-45°C for 2 hours after the addition, separate the liquid, wash the organi...

Embodiment 2

[0051] The preparation of (2,4,6-trimethylbenzoyl) diphenylphosphine oxide, the steps are as follows:

[0052] (1) Add 150ml of re-distilled ether into a 250mL four-neck flask, and blow nitrogen for replacement for 10 minutes. The air inlet is inserted below the liquid level, and 6.8g of phosphine gas is slowly introduced to make it fully absorbed in the solvent. Exhaust gas recycling.

[0053] (2) Add 23.7g of pyridine to the flask, control the temperature at 95-110°C, and add 49.6g of chlorobenzene dropwise into the flask while stirring. After the addition was complete, the mixture was incubated for 2 hours. 19.2 g of 2,4,6-trimethylbenzoyl chloride was added dropwise at a controlled temperature of 45-50° C. for reaction. After the addition was complete, the reaction was kept at a temperature for 2 hours.

[0054] (3) Control the temperature at 30-45°C, add 45g of 30% hydrogen peroxide dropwise, keep the reaction at 30-45°C for 2 hours after the addition, separate the liq...

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Abstract

The invention relates to a preparation method of di (2,4,6-trimethylbenzoyl) phenyl phosphine oxide and (2,4,6-trimethylbenzoyl) diphenyl phosphine oxide used in the technical field of radiation polymerization curing new materials, hydrogen phosphide as a raw material is reacted with chlorobenzene or bromobenzene and 2,4,6-trimethylbenzoyl chloride, and an acyl oxygen phosphonic compound is obtained by oxidizing with an oxidant. By adjusting the feed ratio, the di (2,4,6-trimethylbenzoyl) phenyl phosphine oxide and the (2,4,6-trimethylbenzoyl) diphenyl phosphine oxide are respectively obtained, and the purpose for simultaneously producing the two target products of di (2,4,6-trimethylbenzoyl) phenyl phosphine oxide and the (2,4,6-trimethylbenzoyl) diphenyl phosphine oxide can be achieved by use of same material and device, and compared with known technology paths reported in literatures, the preparation method has the significant advantages of novelty of the chemical reaction technology, cost economic competitiveness and environmental friendliness.

Description

technical field [0001] The invention belongs to the technical field of photoinitiators, in particular to bis(2,4,6-trimethylbenzoyl)phenylphosphine oxide and (2,4,6-trimethylbenzoyl)diphenylphosphine oxide method of preparation. Background technique [0002] Acylphosphine oxide compounds are used as high-efficiency photoinitiators, suitable for initiating radiation polymerization of some unsaturated resins under ultraviolet light, especially for white formulations and glass fiber reinforced polyester / styrene systems and with light stabilizers Compatible with varnish systems and paint systems for exterior use, such as for wood, paper, metal, plastics, optical fibers, printing inks and pre-impregnated systems, etc. [0003] Among them, bis(2,4,6-trimethylbenzoyl)phenylphosphine oxide (initiator 819) and (2,4,6-trimethylbenzoyl)diphenylphosphine oxide (initiator TPO) These are two of them that are commonly and widely used. The structural formula is as follows: [0004] ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/53
Inventor 孙建郑康健
Owner TIANJIN MOSEN TECH CO LTD
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