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Method for continuous production of 0,0-dimethyl thiophosphoryl chloride

A technology of dimethyl thiophosphoryl and methyl thiophosphoryl dichloride, applied in the field of continuous preparation of O, can solve the problems of low equipment utilization, long reaction time, low yield and the like, and it is extremely easy to achieve production capacity Amplify, improve labor productivity, reduce the effect of labor intensity

Active Publication Date: 2008-06-11
XIANGTAN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The traditional process adopts batch production mode, which has the characteristics of long reaction time, low equipment utilization rate, low yield, unstable product quality, and small production capacity of a single reactor.

Method used

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  • Method for continuous production of 0,0-dimethyl thiophosphoryl chloride

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Experimental program
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Effect test

Embodiment 1

[0019] 1 mol of O-dimethyl thiophosphoryl dichloride and 4.8 mol of methanol are added to the first-stage reactor, while 0.46 mol of alkali is added to the first-stage reactor, and the temperature of each stage of the reactor is controlled as follows: -5~ At 0°C, 0.31 mol of alkali is added to the second stage reactor, 0.16 mol of alkali is added to the third stage reactor, and 0.12 mol of alkali is added to the fourth stage reactor. The reaction mixture was washed with water and separated into layers to obtain O, O-dimethyl thiophosphoryl chloride with a mass content of 91.3%.

Embodiment 2

[0021] 100kmol of O-dimethylthiophosphoryl dichloride and 600kmol of methanol are added to the first stage reactor, while 35kmol of alkali is added to the first stage reactor, and the temperature of each stage of the reactor is controlled as follows: -8~-2 ℃, add 20kmol alkali into the second stage reactor, 15kmol alkali into the third stage reactor, 10kmol alkali into the fourth stage reactor, and 10kmol alkali into the fifth stage reactor. Add 5 kmol alkali to the reactor, add 5 kmol alkali in the seventh-stage reactor, and the reaction mixture enters the oil-water separator after being washed with water to obtain O, O-dimethyl thiophosphoryl chloride with a mass content of 92.6%.

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Abstract

The invention relates to a continuous preparation method of O, O-dimethyl thiophosphoryl chloride, which comprises adding O-methyl thiophosphoryl chloride, methanol and alkali continuously into a combination reactor composed of serial multistage reactors, adding alkali into the reactor at each stage, using a hydraulic cyclone to separate the material continuously flown outside the reactor, using the oil phase as product, and feeding water phase into a settler to further separate residual O, O-dimethyl thiophosphoryl chloride, recovers methanol in the water phase, and removes waste water. The invention has high reaction yield and equipment utilization, high product quality, short reaction time and reduced production cost, which can continuously prepare O, O-dimethyl thiophosphoryl chloride.

Description

Technical field [0001] The invention relates to a method for continuously preparing O, O-dimethyl thiophosphoryl chloride. Background technique [0002] O, O-dimethyl thiophosphoryl chloride is an important intermediate for the production of chlorpyrifos methyl, acephate, and chlormethamido. At present, the traditional reaction process for industrial production of O, O- dimethyl thiophosphoryl chloride , Using a stirred reactor for intermittent production, the reaction is to add O-dimethyl thiophosphoryl dichloride first, then quickly add methanol, control the reaction temperature-5 ~ 0 ℃, drip alkali, after each batch of reaction is completed, discharge Static layering to obtain O, O-dimethyl thiophosphoryl chloride. The reaction equation is as follows: [0003] [0004] The traditional process adopts the intermittent production method, which has the characteristics of long reaction time, low equipment utilization, low yield, unstable product quality, and small production capa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/42
Inventor 罗和安艾秋红王良芥刘平乐刘志明张彬彬张方灯刘孝平从兴红
Owner XIANGTAN UNIV
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