New preparation method of first-class phenyl phosphine oxide initiator

Abstract

The invention provides a new preparation method of a first-class phenyl phosphine oxide initiator. The method comprises the steps that (1) benzene and aluminum trichloride are added into a reaction vessel and stirred uniformly, then phosphorus trichloride is added, the temperature is slowly increased, and after a complete reaction, the temperature is reduced to room temperature; (2) a reaction mixture obtained in the step (1) is slowly added dropwise into a solvent containing a decomplexing agent, and the temperature is controlled for decomplexing; (3) a decomplexing product obtained in the step (2) is filtered to separate solids, and filtrate is subjected to pressure reduction distillation to obtain phenyl dialkoxy phosphine or diphenyl alkoxy phosphine; (4) a product obtained in the step(3) is dissolved in a benzene or methylbenzene solvent, and a trichloromethyl acetyl compound is added dropwise for a reaction; and (5) a solution obtained after the complete reaction in the step (4)is subjected to low-pressure desolvation, and light-yellow liquid or solid, namely the phenyl phosphine oxide initiator, is obtained through crystallization, suction filtering and drying. The methodhas the advantages that raw materials are easy to obtain, cost is low, operation is easy to perform, and mass production can be realized.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, in particular to a new preparation method of a class of phenylphosphine oxide initiators. Background technique [0002] Phenylphosphine oxide initiator is a high-efficiency free radical (I) type photoinitiator, which absorbs in the long wavelength range. Due to its wide absorption range, its effective absorption peak is 350nm -400nm, absorbing to about 420nm, its absorption peak is longer than that of conventional initiators, it can generate two free radicals of benzoyl and phosphoryl after being illuminated, both of which can initiate polymerization, so the photocuring speed is fast, suitable for thick The film is deeply cured, it also has photobleaching effect, and the coating does not yellow. It can be completely cured on white or high-titanium dioxide pigmented surfaces. The post-polymerization effect is low and there is no residue. It can also be used for transparent coatings. For ...

AI Technical Summary

Problems solved by technology

[0004] The industrial synthesis method of diphenylphosphine chloride and phenylphosphorus dichloride is to use benzene and phosphorus trichloride as raw materials, react under the catalysis of anhydrous aluminum trichloride, and the phenylphosphine chloride and chlorine trichloride of generation Complexation, by adding phosphorus oxychloride, solid sodium chloride or solid potassium chloride for decomplexation reaction, the disadvantage of this method is that the decomplexation reaction process is complicated, and a large amount of solid waste sensitive to water is generated. liquid separation, can not be completely separated, so the resulting product yield is low, generally around 40%, resulting in higher cost of the product, and with serious environmental problems, just because of these shortcomings are diphenyl phosphorus chloride and The reason why phenylphosphorous dichloride cannot be mass-produced is that they are the key raw materials for the production of TPO and TPO-L, with high cost and small production volume, which seriously restricts the production volume of TPO and TPO-L, and greatly increases the production cost

[0005] Simultaneously the main way of synthesizing TPO or TPO-L in the prior art is that diphenyl phosphorus chloride and phenyl phosphorus dichloride first react with alcohols such as ethanol to generate ethoxyphenyl phosphine chloride, and then replace with alkyl The reaction of benzoyl chloride not only reflects that the steps are long, but also produces chlorinated alkanes such as ethyl chloride and causes VOC (volatile organic compound) waste gas emissions, which cannot be recycled and used, which increases the cost of environmental protection treatment. Other methods for synthesizing TPO or TPO-L The reaction process requires the use of dangerous reaction processes such as oxidation, which brings great potential risks to safe production

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