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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

Inactive Publication Date: 2017-07-21
南京奥格美化学研究所有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Not commercialized due to low product purity and yield

Method used

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  • Method for preparing dichloro monoalkyl phosphine
  • Method for preparing dichloro monoalkyl phosphine

Examples

Experimental program
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Effect test

Embodiment 1 2

[0047] Embodiment 1 Dichloromonomethylphosphine aluminum trichloride complex MePCl 2 ·AlCl 3 Preparation of:

[0048] A five-necked glass flask is used as a reaction bottle equipped with an electric stirrer, a thermometer, two dropping funnels, and a vent port connected to a Schlenk Line. After the flask is replaced with pure nitrogen, it is filled with nitrogen to normal pressure.

[0049] Dichloromonomethylaluminum 100g (0.886mol) was dissolved in 660g n-octane at room temperature, and placed in a dropping funnel. Phosphorus trichloride 121.6g was diluted with 243g n-octane, and placed in another dropping funnel. 50ml of n-octane was preset at the bottom of the reaction bottle.

[0050] Stir at room temperature and start to add dichloromonomethylaluminum and phosphorus trichloride n-octane solution synchronously. At this time, the temperature in the reaction bottle rises automatically. Complete dichloromonomethylaluminum n-octane solution and phosphorus trichloride n-oct...

Embodiment 2

[0054] Phosphorus trichloride binary phosphorus aluminum exchange product (3MePCl of embodiment 2 methyl sesquichloride aluminum 2 )·(2·AlCl 3 ) preparation:

[0055] The reaction apparatus is the same as in Example 1, 100 g (0.487 mol) of methyl aluminum sesquichloride is diluted with 1000 g of n-octane, and placed in a dropping funnel. Phosphorus trichloride 301g (2.25mol, excessive phosphorus trichloride) is diluted with 600g n-octane, and placed in another dropping funnel. 50ml of n-octane was preset at the bottom of the reaction bottle.

[0056] Stir at room temperature and start to add methyl sesquichloride and phosphorus trichloride n-octane solution synchronously. At this time, the temperature in the reaction bottle rises automatically. After the addition of methyl aluminum sesquichloride n-octane solution and phosphorus trichloride n-octane solution, stir at room temperature for 24 hours or raise the temperature to 60° C. and stir for 5 hours to stop. Change to va...

Embodiment 3

[0057] Example 3 From MePCl 2 ·AlCl 3 Preparation of dichloromonomethylphosphine:

[0058] MePCl 2 ·AlCl 3 +NaCl→MePCl 2 +NaAlCl 4

[0059] Get embodiment 1 gained and contain 70.8% MePCl 2 ·AlCl 3 Add 28.1 g of 200-mesh sodium chloride to 141.2 g of n-octane mixture, stir and heat up to 125° C., stir at this temperature for 6 hours, cool and filter, and wash the filter residue in 3 batches with 100 ml of n-octane. Obtain 81g of filter residue, which is sodium tetrachloroaluminate containing sodium chloride; combine the filtrates, collect fractions at 79-81°C by fractional distillation, and obtain dichloromonomethylphosphine MePCl 2 42.8g, purity 99.4%, density 1.3005 (20°C), yield 91%. The n-octane recovery sleeve is used for the next batch of operations.

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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.

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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Application Information

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IPC IPC(8): C07F9/52
CPCC07F9/52C07F9/5068C07F9/5095
Inventor 庄建元
Owner 南京奥格美化学研究所有限公司
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