84434-11-7Relevant articles and documents
High performance liquid phase continuous automatic production and co-production technology of organic phosphine compound
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Paragraph 0077-0078, (2021/05/12)
The invention relates to the field of photocuring functional new material chemicals, and discloses a high performance liquid phase streamline type continuous automatic production technology of an acylphosphine oxide organic phosphine compound for the first time, which not only can produce a single specific target product, but also can co-produce a product mixture of two or more than two of the products of the type. The process technology has outstanding low-cost economic competitiveness and environment-friendly characteristics for large-scale manufacturing of target products. The target product comprises sym-trimethylbenzoyl diphenyl phosphine oxide (also known as 2, 4, 6-trimethylbenzoyl diphenyl phosphine oxide, trade name TPO), sym-trimethylbenzoyl phenyl ethyl phosphonate (trade name TPO-L) and structural analogues thereof, and a mixture of the sym-trimethylbenzoyl diphenyl phosphine oxide and the sym-trimethylbenzoyl phenyl ethyl phosphonate. The organic phosphine compound is an olefinic bond-containing (C=C) unsaturated radiation polymerization system photoinitiator and/or flame retardant and the like with wide application.
New preparation method of first-class phenyl phosphine oxide initiator
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Paragraph 0049-0055, (2020/03/05)
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.
Preparation method for high-purity ethyl (2,4,6-trimethylbenzoyl)phenylphosphinate
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Paragraph 0012; 0019; 0020; 0021; 0022; 0023; 0024-0026, (2017/10/13)
The invention discloses a preparation method for high-purity ethyl (2,4,6-trimethylbenzoyl)phenylphosphinate. The preparation method comprises the following concrete steps: reacting phenylphosphinate with aromatic aldehyde so as to prepare an intermediate, subjecting the intermediate to catalytic oxidation so as to obtain benzoylphenylphosphinic acid and subjecting benzoylphenylphosphinic acid and diethyl sulfate to an ethylation reaction so as to obtain ethyl (2,4,6-trimethylbenzoyl)phenylphosphinate. According to the invention, raw materials have high quality and stable properties; by-produced impurities produced during synthesis of ethyl (2,4,6-trimethylbenzoyl)phenylphosphinate can be removed through neutralization, and ethyl (2,4,6-trimethylbenzoyl)phenylphosphinate with a purity of higher than 99.0%, which meets market demands for the high-purity photoinitiator ethyl (2,4,6-trimethylbenzoyl)phenylphosphinate.