Method for preparing dichloro monoalkyl phosphine

A technology of dichloro-alkylphosphine and dichloro-alkylaluminum, which is applied in the field of metal-organic compound preparation, can solve the problems of low product purity, non-commercialization, and low yield, so as to reduce solid waste residue and increase yield , the effect of increasing the yield
CN106967118AInactive Publication Date: 2017-07-21南京奥格美化学研究所有限公司
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Patent Information

Authority / Receiving Office
CN · China
Current Assignee / Owner
南京奥格美化学研究所有限公司
Publication Date
2017-07-21
Estimated Expiration
Not applicable · inactive patent

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Abstract

The invention discloses a method for preparing dichloro-alkylphosphine, which uses sodium chloride to decomplex the binary complex of dichloro-alkylaluminum or alkyl aluminum sesquichloride and phosphorus trichloride When adding the alkane solvent, the free dichloro-alkylphosphine enters the alkane solvent, and the alkane solution of the dichloro-alkylphosphine is separated from the newly generated sodium tetrachloroaluminate NaAlCl by solid filtration; the target product dichloro-alkyl The mixture of phosphine and alkane solvent can be separated by distillation, or directly enter the next application process without separation. The decomposition of the traditional dichloro-alkylphosphine high-temperature distillation is avoided, the yield is increased and the waste residue is reduced.
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Description

technical field

[0001] The invention relates to a method for preparing dichloro-alkylphosphine, which belongs to the technical field of metal organic compound preparation. Background technique

[0002] Dichloro-alkyl phosphine, especially dichloro-methyl phosphine, is currently an intermediate of reactive flame retardants and is also used in the manufacture of high-efficiency and low-toxicity herbicides.

[0003] The technical route for preparing dichloromonomethylphosphine so far is as follows.

[0004] (1) PCl 3 +MeH→MePCl 2 +HCl

[0005] Methane and phosphorus trichloride react to obtain dichloromonomethylphosphine, which was first proposed by FMC company (US3210418), and Hoechst company (US4101573, US4518538, etc.) has made significant improvements and is commercially used for the preparation of phosphine ring ester flame retardants and The herbicide glufosinate-ammonium.

[0006] Methane and phosphorus trichloride react in gas phase at 500~650℃ and 0.3~0.6MPa in a ...

Claims

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