Preparation method of diphenyl phosphoryl chloride

Abstract

The invention relates to a preparation method of diphenyl chlorophosphate, which is characterized in that phenol and phosphorus oxychloride are put into a reaction kettle, a catalyst is added, the temperature is raised to 130-150°C after 2.5-5.5 hours, heat preservation reaction, GC The phenol content in the middle control is less than 0.5% and the reaction is completed. After the reaction, the reaction liquid is rectified to obtain the finished diphenyl chlorophosphate; the catalyst is triphenylphosphine and triphenylphosphine oxide; the molar ratio of phenol to phosphorus oxychloride The ratio is 1:1 to 3:1, the dosage of triphenylphosphine is 0.5 to 5% of the weight of phenol, and the dosage of triphenylphosphine oxide is 0.5 to 8% of the weight of phenol; the reaction temperature is 50 to 150°C. The present invention has the advantage that no solvent is used.

Description

technical field [0001] The invention relates to a preparation method of diphenyl chlorophosphate, which belongs to the field of chemical industry. Background technique [0002] Diphenyl chlorophosphate (DPCP), English name: Diphenyl chlorophosphate, Chinese alias: diphenoxyphosphoryl chloride, phosphoryl chloride diphenyl or chlorophosphate, etc. DPCP is an important organophosphorus intermediate, which can be used as an intermediate of flame retardant, and can also be used to synthesize diphenylphosphoryl azide which is widely used. Its general synthesis method is to prepare by reacting phenol and phosphorus oxychloride under the action of a catalyst. Using different catalysts, the selectivity and yield of the reaction will have different effects. The reaction formula is as follows: [0003] [0004] There are three products: diphenyl chlorophosphate (DPCP), triphenyl phosphate (TPP) and monophenyl dichlorophosphate (MPCP). In the Chinese journal "Chemical Research", ...

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Problems solved by technology

There are two problems in this process: 1) The dichloroethane solvent is a type of solvent stipulated in the "Technical Guidelines for the Research of Residual Solvents in Chemical Drugs", which is easy to cause great harm to the human body and the environment. 2) Adding water destroys the three Aluminum chloride will inevitably lead to the hydrolysis of phosphorus oxychloride of DPCP and then continue to react with DPCP to generate tetraphenyl diphosphate. The reaction formula is as follows:

[0007] Tetrahedron Letters, 2013 , vol. 54, # 15 p. 2026 – 2028, using triethylamine as the catalyst, toluene as the solvent, the yield is unknown; Collection of Czechoslovak Chemical Communications, 1989 , vol. 54, # 3 p. 608 – 615 , using magnesium chloride as a catalyst, xylene as a solvent, and the yield is unknown; none of the catalysts described in these documents can be recycled, and solvents are used in the process. Compared with no solvent, the capacity of the reactor with the same volume is relatively small

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