Green synthesis technology of O,O-diethyl thiophosphoryl chloride

A technology of ethyl thiophosphoryl and diethyl dithiophosphoric acid ester, which is applied in the field of green synthesis technology of O,O-diethyl thiophosphoryl chloride, can solve the problem of affecting the surrounding environment, serious environmental pollution, production It can prevent air pollution, easily obtain raw materials, and reduce processing costs.

Inactive Publication Date: 2019-02-22
CHONGQING HUAGE BIOCHEM
View PDF6 Cites 4 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The phosphorus trichloride method has high production costs, many side reactions, and serious environmental pollution. It is basically not used in production. The phosphorus pentasulfide method is currently a common production method.
The impurity in the crude product of O, O-diethylthiophosphoryl chloride produced by phosphorus pentasulfide method is mainly disulfur dichloride (content is about 25%). Alkali metal reducing salt method, ammonium bisulfite method and sodium sulfite method, but a large amount of sulfur-containing and foul-smelling wastewater will be generated during the process of production, which seriously affects the surrounding environment

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] This embodiment provides a green synthesis process for O, O-diethylphosphorylthiochloride, which comprises the following steps:

[0031] S1. Put 800kg of ethanol into the reaction kettle, then put 2000kg of phosphorus pentasulfide into the reaction kettle, and stir; after adding phosphorus pentasulfide, add the remaining 1000kg of absolute ethanol and 3kg of the mixed solution of vulcanization catalyst to the reaction kettle dropwise, and keep it warm after the addition 30min, then cooled to 50°C, and filtered to obtain 3318kg of O,O-diethyl phosphorodithioate.

[0032] S2. Transfer the obtained O, O-diethyl phosphorodithioate to a chlorination kettle, stir at 35°C, feed chlorine gas into the reaction kettle, and control the chlorine flow rate at 1.6kg / min. When the molar ratio of chlorine gas to O, O-diethyl phosphorodithioate reaches 1:1.2, stop the chlorine flow.

[0033] S3. Put the material in the chlorination kettle into the high-temperature kettle, start stirrin...

Embodiment 2

[0037] This embodiment provides a green synthesis process for O, O-diethylphosphorylthiochloride, which comprises the following steps:

[0038] S1. Put 750kg of ethanol into the reaction kettle, then put 2000kg of phosphorus pentasulfide into the reaction kettle, and stir; after the phosphorus pentasulfide is put in, add the remaining 1000kg of absolute ethanol and 3kg of vulcanization catalyst to the reaction kettle dropwise, and keep it warm after the addition 30min, then cooled to 50°C, and filtered to obtain 3312kg of O,O-diethyl phosphorodithioate.

[0039] S2. Transfer the obtained O, O-diethyl phosphorodithioate to a chlorination kettle, stir at 40°C, feed chlorine gas into the reaction kettle, and control the chlorine flow rate at 1.6kg / min. When the molar ratio of chlorine gas to O,O-diethyl phosphorodithioate reaches 1:1.3, stop the chlorine flow.

[0040] S3. Put the material in the chlorination kettle into the high-temperature kettle, start stirring, add 2kg of co...

Embodiment 3

[0044] This embodiment provides a green synthesis process for O, O-diethylphosphorylthiochloride, which comprises the following steps:

[0045] S1. Put 700kg of ethanol into the reaction kettle, then put 2000kg of phosphorus pentasulfide into the reaction kettle, and stir; after the addition of phosphorus pentasulfide, add the remaining 1000kg of absolute ethanol and 3kg of vulcanization catalyst to the reaction kettle dropwise, and keep it warm after the addition 30min, then cooled to 50°C, and filtered to obtain 3306kg of O,O-diethyl phosphorodithioate.

[0046] S2. Transfer the obtained O, O-diethyl phosphorodithioate to a chlorination kettle, stir at 45°C, feed chlorine gas into the reaction kettle, and control the chlorine flow rate at 1.8kg / min. When the molar ratio of chlorine gas to O, O-diethyl phosphorodithioate reaches 1:1.2, stop the chlorine flow.

[0047] S3. Put the material in the chlorination kettle into the high-temperature kettle, start stirring, add 2kg of...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention provides a green synthesis technology of O,O-diethyl thiophosphoryl chloride and relates to the field of chemical synthesis. The green synthesis technology comprises the following steps:taking O,O-diethyl dithiophosphate to react with chlorine gas at low temperature, so as to obtain a crude product of the O,O-diethyl thiophosphoryl chloride; then transferring the crude product to react at high temperature; enabling the residual O,O-diethyl dithiophosphate to further completely react with the chlorine gas. Meanwhile, in a high-temperature reaction process, a polymeric compound isprevented from being generated when a compound catalyst is used and sulfur monochloride impurities are completely removed through reaction, so that a byproduct sulfur has a crystalline state and a product more easily separated and purified. Moreover, HCl and sulfur-containing odorous gas are pumped away through applying negative pressure and the tail gas is absorbed to prevent air pollution. In awhole reaction process, technological water does not need to be added, so that wastewater is not generated and the treatment cost of sulfur-containing and phosphorus-containing wastewater is reduced.The technology has the advantages of simplicity in operation, easiness for obtaining raw materials, moderate reaction conditions, small pollution and environment friendliness.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a green synthesis process of O, O-diethylphosphorylthiochloride. Background technique [0002] O, O-diethylthiophosphoryl chloride is an important pesticide and pharmaceutical intermediate, which can be used to synthesize organophosphorus insecticides parathion, phoxim, diazinon, quinoxafos, pyridazine sulfur Phosphorus, triazophos, pyrimidinoxon, phosphinophos, chlorpyrifos, demeton and synergist synergistic phosphorus, etc., can also be used as synthetic raw materials for lubricating oil additives and other sulfur-containing organophosphorus compounds. At present, there are many domestic manufacturers with large annual output. [0003] The production method of O,O-diethylphosphorothioate is based on different raw materials, and there are two methods: phosphorus trichloride method and phosphorus pentasulfide method. The production cost of phosphorus trichloride is high, the s...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/20
CPCC07F9/2003
Inventor 陈志忠何小强郎兴洪刘凯李传武郝磊林军
Owner CHONGQING HUAGE BIOCHEM
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap