Method for producing alkyl phosphorus dichloride

Abstract

The invention relates to the field of chemical industry and further relates to a production method of an organic phosphorus intermediate, and in particular relates to a method for producing alkyl phosphorus dichloride. The method comprises the following specific step: in the presence of a catalyst, enabling phosphorus trichloride and alkane to react in a tubular reactor under high temperature andhigh pressure, so as to generate the alkyl phosphorus dichloride, wherein the alkane is selected from one or two of methane and ethane and the catalyst is selected from one or two of chloroform and dichloromethane. The method provided by the invention has the advantages of low production cost, great industrial feasibility, measurable and controllable technological conditions, high reaction conversion rate and selectivity, good product quality and the like.

Description

technical field [0001] The invention relates to the field of chemical industry, and further relates to a production method of an organic phosphorus intermediate, in particular to a method for producing alkyl phosphorus dichloride. Background technique [0002] As an important basic chemical raw material, alkyl phosphorus dichloride is widely used, mainly used in the production of flame retardants and agricultural herbicide glufosinate-ammonium, and can also be used in the synthesis of chemical weapons [Angew.Chem.Int.Ed.Engl. 20, 1981, 223; Phosphorus, Sulfur and Silicon, 1999, 144, 21; Handbook of Organophosphorus Chemistry, Robert Engel, CRC, 1992]. [0003] At present, there are a lot of bibliographical reports about the synthetic method of alkyl phosphorus dichloride [Angew.Chem.Int.Ed.Engl.12,1973,877; Angew.Chem.Int.Ed.Engl.15,1976,468; Angew. Chem.Int.Ed.Engl.20, I981,223; Pesticides, 41, 2002, 46], but mainly synthesized by methyl phosphorus dichloride. Their synth...

AI Technical Summary

Problems solved by technology

The composition of the reaction product is complex and the yield is not high

[0023] The above four methods are compared from the cost of raw materials and the amount of three wastes produced. The first direct reaction process of alkane and phosphorus trichloride is the best, but this process has high technical difficulty, high reaction temperature, high energy consumption, and high equipment requirements. , low conversion rate of phosphorus trichloride in one pass, etc., so how to realize the effective recovery and utilization of heat, the control of reaction parameters and the recycling of phosphorus trichloride are the key points of this production process

Owing to there is very big potential safety hazard in using oxygen as catalyst / initiator, so the carbon tetrachloride developed by German Hearst Company is catalyst / initiator, and methane and phosphorus trichloride gas-phase reaction synthesis methyl dichloride at high temperature The method of phosphorus removal [US4518538; US4104299; USP4104304] should be a better industrial production method

However, carbon tetrachloride is one of the ODS substances (Ozone Depleting Substances) that destroy the atmospheric ozone layer. China has joined the "Montreal Protocol on Substances that Deplete the Ozone Layer", which limits the use of carbon tetrachloride.

Secondly, with carbon tetrachloride as the catalyst / initiator, in the actual production process, the pipeline easily generates solid matter and causes pipeline blockage

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