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Method for processing 0,0-ethyl thioether substituted phosphorus oxychloride residual liquid

A technology of ethyl thiophosphoryl and a treatment method, applied in the field of O, can solve the problems of serious environmental pollution and high production cost, and achieve the effects of increasing income, reducing environmental protection treatment, and simple and convenient process

Active Publication Date: 2008-02-27
ZHEJIANG XINNONG CHEM CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The first method has high production cost and serious environmental pollution, while the latter method is the current general production method

Method used

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  • Method for processing 0,0-ethyl thioether substituted phosphorus oxychloride residual liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Put 173 kg of ethyl chloride distillation raffinate (through gas phase detection, ethyl chloride content is 20%, dimer sulfide content is 40%) into a 500L reactor, under vigorous stirring, within 1 hour at 50 20.5 kg of chlorine gas was passed in at 70 °C, and then kept at 70 °C for 30 minutes, 60 kg of ethanol was added, and the temperature was kept at 1 hour. The content of ethyl chloride in the liquid is 58%). First recover low boilers below 100°C under normal pressure, and then switch to vacuum distillation to collect 110 kg of fractions at 80-90°C / 10mmHg. This fraction was then subjected to high vacuum rectification to obtain 83 kg of 97.0% ethyl chloride.

Embodiment 2

[0022] 173 kg of ethyl chloride distillation raffinate (through gas phase detection, the content of ethyl chloride is 20%, the content of dimer sulfide is 40%) is put into a 500L reactor, under vigorous stirring, within 1.5 hours at 60 20.5 kg of chlorine gas was introduced at 80 °C, and then kept at 80 °C for 30 minutes, 60 kg of ethanol was added, and the temperature was kept at 1 hour. The content of ethyl chloride in the liquid is 58%). First recover low boilers below 100°C under normal pressure, and then switch to vacuum distillation to collect 112 kg of fractions at 80-90°C / 10mmHg. This fraction was then subjected to high vacuum rectification to obtain 85 kg of 97.8% ethyl chloride.

Embodiment 3

[0024] Put 173 kg of ethyl chloride distillation raffinate (through gas phase detection, ethyl chloride content is 20%, dimer sulfide content is 40%) into a 500L reactor, under vigorous stirring, within 1 hour at 50 20.5 kg of chlorine gas was introduced at ℃, and then kept at 70 ℃ for 30 minutes, then 100 kg of water was added, and the temperature was kept at 1 hour. The material was hydraulically transferred to the settling tank. The content of ethyl chloride in the liquid is 50%). First, the low boilers below 100°C are distilled at normal pressure, and then replaced by vacuum distillation, and 95 kg of fractions at 80-90°C / 10mmHg are collected. This fraction was further subjected to high vacuum rectification to obtain 71 kg of 98.3% ethyl chloride.

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Abstract

The invention discloses a manufacturing method of O,O-diethyl thiophosphorus oxychloride; aerating certain quantity of chlorine gas into residual liquid; inverting the dipolysulfide into the O,O-diethyl thiophosphorus oxychloride; adding fitful quantity of aliphatic alcohol into the chloride liquid; evaporating under normal pressure before boiling; decompressing to distill the crude product after collecting; rectifying through high-vacuum rectifying tower; obtaining the high-purity product with simple technique; recycling O,O-diethyl thiophosphorus oxychloride from residual liquid of ethyl chloride with high receiving rate and high purity; increasing the income due to changing the waste into value; reducing the environmental protective disposal of water liquid; reaching the request of green manufacturing.

Description

technical field [0001] The invention relates to a production and treatment method of O, O-diethylthiophosphoryl chloride raffinate. The method is applicable to the production process of chlorination with chlorine gas, treatment with fatty alcohol and distillation with high yield and high yield from the raffinate. O,O-diethylphosphorylthiochloride was prepared purely. Background technique [0002] O, O-diethylthiophosphoryl chloride (referred to as ethyl chloride) is an important preparation of organophosphorus pesticides such as: parathion, triazophos, chlorpyrifos, phoxim, musphos, quinthion and other products intermediate. At present, the annual demand at home and abroad is tens of thousands of tons. Due to the different raw materials used, its production methods can be classified into two types, namely the phosphorus trichloride method and the phosphorus pentasulfide method. The first method has high production cost and serious environmental pollution, while the latter...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/20
Inventor 赵金浩戴金贵徐振元
Owner ZHEJIANG XINNONG CHEM CO LTD