Preparation process of photo-initiator bis(2,4,6-trimethylbenzoyl)phenylphosphine oxide

A technology of trimethylbenzoyl and trimethylbenzoyl, applied in the field of preparation technology of photoinitiator phenylphosphine oxide, can solve the problems of easy spontaneous combustion, inconvenient feeding of solid materials, high price of lithium aluminum hydride, etc. Ease of operation, lower production costs, and the effect of simplifying separation steps

Inactive Publication Date: 2015-12-09
ZHANGJIAGANG JIMUTE CHEM TECH
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AI Technical Summary

Problems solved by technology

Lithium aluminum hydride used in this method is expensive, prone to spontaneous combustion in use, and solid feeding is inconvenient

Method used

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  • Preparation process of photo-initiator bis(2,4,6-trimethylbenzoyl)phenylphosphine oxide

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Embodiment 1

[0027] A kind of preparation technology of two (2,4,6-trimethylbenzoyl) phenyl phosphine oxides of photoinitiator, concrete steps are as follows:

[0028] 1) Under nitrogen protection, add 1L toluene and 300mL red aluminum solution into a 2L reaction kettle, cool down to -10±5°C, add 179g of phenylphosphine dichloride dropwise, and keep the system temperature at -10±5°C, After the dropwise addition, warm up to room temperature, heat and reflux for 8 hours, GC detects that the reaction of phenylphosphine dichloride is complete, and obtains a toluene solution containing sodium chloride, excess red aluminum, and phenylphosphine, and then pours the toluene solution into a continuous flash Flash evaporation is carried out in the evaporator, the flash pressure is controlled at 0.1kPa, the gas phase temperature is controlled at 60±5°C, sodium chloride and excess red aluminum are removed to obtain a toluene solution containing phenylphosphine (mass fraction is 8%) 1.1L;

[0029] 2) P...

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Abstract

The invention discloses a preparation process of a photo-initiator bis(2,4,6-trimethylbenzoyl)phenylphosphine oxide, wherein the process comprises the following steps: 1) performing a reaction to phenyl phosphine dichloride and excessive sodium dihydro-bis-(2-methoxyethoxy)aluminate solution at -50 - 50 DEG C in inert gas, and after the reaction finished, removing a by-product sodium chloride and excessive sodium dihydro-bis-(2-methoxyethoxy)aluminate to obtain a methylbenzene solution of phenyl phosphine; 2) performing a reaction to the methylbenzene solution of phenyl phosphine with 2,4,6-trimethylbenzoyl chloride at -10 - 50 DEG C to obtain a methylbenzene solution of bis(2,4,6-trimethylbenzoyl)phenylphosphine after the reaction finished; and 3) oxidizing the methylbenzene solution of the bis(2,4,6-trimethylbenzoyl)phenylphosphine, and performing liquid separation, concentration and crystallization to the organic phase, and drying to obtain the target product, bis(2,4,6-trimethylbenzoyl)phenylphosphine oxide. The whole process is stable in raw material cost, is low in cost, is safe and easy-to-control in reactions and is easy to achieve large-scale production.

Description

technical field [0001] The invention relates to a preparation process of a photoinitiator (2,4,6-trimethylbenzoyl)phenylphosphine oxide, belonging to the technical field of organic synthesis. Background technique [0002] Bis(2,4,6-trimethylbenzoyl)phenylphosphine oxide (product code photoinitiator 819), has good photochemical reactivity, and can efficiently generate aroyl-oxygen Phosphine-based free radicals have fast photodecomposition speed, fast photocuring speed, and bleaching effect, which is beneficial to the curing of thick coatings. It is widely used in coatings, inks, adhesives, resists, soldering agents and many other fields. In recent years, with the development of UV curing technology, the initiator has also been widely used and developed in this field, which can initiate the polymerization of some unsaturated resins, especially suitable for white formulations and glass fiber reinforced plastics. Polyester / styrene systems and clearcoat systems for exterior use...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/53
Inventor 赵经纬信勇
Owner ZHANGJIAGANG JIMUTE CHEM TECH
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