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Synthesizing method of O,O-dimethyl phosphorodithioate

A technology of dimethyl dithiophosphate and methyl sulfide, which is applied in the field of synthesis of O,O-dimethyl dithiophosphate, can solve the problems of low product yield and the like, and achieves improved content and yield. rate, improve the low content of synthetic products, and promote the effect of positive progress

Active Publication Date: 2018-11-23
德州绿霸精细化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] For this reason, the technical problem to be solved by the present invention is to provide a method for synthesizing O, O-dimethyl phosphorodithioate to solve the problem of O, O-dimethyl phosphorodithioate synthesis method in the prior art. The problem of low product yield

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0020] The method for synthesizing O, O-dimethyl phosphorodithioate described in this embodiment comprises the following steps:

[0021] (1) Add 1500kg of methyl sulfide mother liquor to the reaction kettle, then add 1000kg of phosphorus pentasulfide to the reaction kettle, fully stir for 0.5h, and perform beating treatment for 1h, so that phosphorus pentasulfide and methyl sulfide mother liquor become slurry, and the reaction material is obtained Liquid A;

[0022] (2) Mix 0.5kg DMAP and 0.5kg pyridine as a catalyst, add to 580kg methanol and mix to obtain reaction feed liquid B;

[0023] (3) control the pressure condition of the reactor to be 30mmHg vacuum degree, and raise the temperature of the reaction feed liquid A in the reactor to 25° C., and start to drop the reaction feed liquid B in the reactor; and After the dropwise addition is completed, the reaction kettle is heated to 50° C. for heat preservation reaction for 1 hour. During the reaction, the hydrogen sulfide g...

Embodiment 2

[0026] The method for synthesizing O, O-dimethyl phosphorodithioate described in this embodiment comprises the following steps:

[0027] (1) Add 1500kg of methyl sulfide mother liquor to the reaction kettle, then add 1000kg of phosphorus pentasulfide to the reaction kettle, fully stir for 0.5h, and perform beating treatment for 1h, so that phosphorus pentasulfide and methyl sulfide mother liquor become slurry, and the reaction material is obtained Liquid A;

[0028] (2) Get 1.5kg DMAP and 1kg of pyridine to mix as catalyst, add to 584kg methanol and mix well to obtain reaction feed liquid B;

[0029] (3) Control the pressure condition of the reactor to be 30mmHg vacuum degree, and raise the temperature of the reaction feed liquid A in the reactor to 30° C., and start to drop the reaction feed liquid B in the reactor; and After the dropwise addition is completed, the reaction kettle is heated to 55° C. for a heat preservation reaction for 1 hour. During the reaction, the hydro...

Embodiment 3

[0032] The method for synthesizing O, O-dimethyl phosphorodithioate described in this embodiment comprises the following steps:

[0033] (1) Add 1500kg of methyl sulfide mother liquor to the reaction kettle, then add 1000kg of phosphorus pentasulfide to the reaction kettle, fully stir for 0.5h, and perform beating treatment for 1h, so that phosphorus pentasulfide and methyl sulfide mother liquor become slurry, and the reaction material is obtained Liquid A;

[0034] (2) Take 0.8kg DMAP and 1kg of pyridine and mix it as a catalyst, add to 581kg methanol and mix well to obtain reaction feed liquid B;

[0035] (3) Control the pressure condition of the reactor to be 40mmHg vacuum, and raise the temperature of the reaction feed liquid A in the reactor to 35° C., and start to add the reaction feed liquid B dropwise to the reactor; and After the dropwise addition is completed, the reaction kettle is heated to 55° C. for a heat preservation reaction for 1 hour. During the reaction, t...

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Abstract

The invention belongs to the technical field of chemical synthesis, and particularly relates to a synthesizing method of O,O-dimethyl phosphorodithioate. The synthesizing method of the O,O-dimethyl phosphorodithioate has the advantages that on the basis of existing technical method, a proper catalyst is further screened, added into a methanol solution and dripped into a sulfide mother liquid, so that the content and yield of the target product are further increased; the whole methanol dripping process is performed under the micro-negative pressure condition, so that the step of dripping the methanol to react can be performed at lower temperature of 25 to 35 DEG C, and the reaction product of hydrogen sulfide can escape out at micro-negative pressure of 30 to 50mmHg, so as to effectively accelerate the reaction to perform along the positive direction.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a synthesis method of O, O-dimethyl phosphorodithioate. Background technique [0002] O, O-dimethyl dithiophosphate, referred to as methyl sulfide, is an important intermediate of organophosphorus pesticides, which can be directly synthesized into insecticides such as dimethoate, malathion, imidophos, and Daofengsan , Herbicide Shabai phosphorus, fungicide Kejun Zhuang and other organophosphorus pesticides. O, O-dimethyl phosphorodithioate can also be chlorinated to obtain another important organophosphorus intermediate - that is, O, O-dimethyl phosphorothioate chloride. [0003] In the prior art, the method for producing O,O-dimethylphosphorothioate is mainly prepared by esterification of phosphorus pentasulfide and methanol, that is, a certain amount of sulfide mother liquor, phosphorus pentasulfide and catalyst are added to the reaction tank, and stirre...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/17
CPCC07F9/17
Inventor 田俊杰孙在臣张学忠张金旺
Owner 德州绿霸精细化工有限公司
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