A method for continuously synthesizing O, S-dimethylphosphorothioate based on a tubular reaction device

A technology of dimethylphosphorothioate and tubular reaction device, applied in chemical/physical/physicochemical stationary reactors, chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, etc., capable of solving The production capacity of a single reactor is small, the product quality and yield are unstable, and the production process is prone to problems such as material flushing, which meets the requirements of large-scale industrial production, is easy to automatically control, and has the effect of small equipment investment.

Inactive Publication Date: 2016-08-17
XIANGTAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The synthesis process of methamidophos in the prior art cannot be continuously produced, resulting in long reaction time, low equipment utilization rate, small production capacity of a single reactor, difficult operation control, unstable product quality and yield, and poor production process. Defects such as flushing are prone to occur. The purpose of the present invention is to provide a continuous synthesis of O, S-dimethylsulfide using a tubular reaction device using O, O-dimethylphosphoramide and dimethyl sulfate as raw materials. The method of phosphoramide substitution has high reaction efficiency, high equipment utilization rate, large production capacity of a single reaction device, easy control of the reaction process, good safety performance, and meets the requirements of industrial continuous production

Method used

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  • A method for continuously synthesizing O, S-dimethylphosphorothioate based on a tubular reaction device
  • A method for continuously synthesizing O, S-dimethylphosphorothioate based on a tubular reaction device
  • A method for continuously synthesizing O, S-dimethylphosphorothioate based on a tubular reaction device

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Embodiment 1

[0032] O, O-dimethylphosphorothioate and dimethyl sulfate are respectively metered by piston metering pumps, and then enter the first section of the tubular reactor, which is equipped with a static mixer inside and outside the tube. Jacketed cooling jacket. The mass ratio of dimethyl sulfate to O, O-dimethylphosphorothioate is 5.3:100. The flow rate of the material in the first section of the tubular reactor is 1m / s, the residence time is 6 minutes, and the temperature of the first section of the tubular reactor is 40°C to 45°C. Then enter the second section of the tubular reactor. The second-stage tubular reactor is provided with an annular central baffle, and the second-stage tubular reactor is submerged in a container with a coolant, and the flow rate of the material in the second-stage tubular reactor is 0.01m / s. The time is 8 hours, and the temperature of the second-stage tubular reactor is 40°C to 45°C. At the reaction outlet, the content of O,S-dimethylphosphorothioa...

Embodiment 2

[0034] O,O-dimethylphosphorothioate is metered with dimethyl sulfate by a piston metering pump respectively, and then enters the first section of the tubular reactor. A static mixer is installed inside the tubular reactor, and a static mixer is installed outside the tube. There is a jacketed cooling jacket. The mass ratio of dimethyl sulfate to O, O-dimethylphosphorothioate is 6:100. The flow rate of the material in the first section of the tubular reactor is 0.1m / s, the residence time is 60 minutes, and the temperature of the first section of the tubular reactor is 35°C to 40°C. Then by entering the second-stage tubular reactor, the second-stage tubular reactor is provided with a central circular baffle, and the second-stage tubular reactor is submerged in a container with a coolant, and the second-stage tubular reactor The flow rate of the material in the reactor is 0.01m / s, the residence time is 7 hours, and the temperature of the second-stage tubular reactor is 40°C-45°C....

Embodiment 3

[0036] O,O-dimethylphosphorothioate is metered with dimethyl sulfate by a piston metering pump respectively, and then enters the first section of the tubular reactor. A static mixer is installed inside the tubular reactor, and a static mixer is installed outside the tube. There is a jacketed cooling jacket. The mass ratio of dimethyl sulfate to O, O-dimethylphosphorothioate is 5:100. The flow rate of the material in the first section of the tubular reactor is 0.05m / s, the residence time is 30 minutes, and the temperature of the first section of the tubular reactor is 35°C to 40°C. Then it enters the second-stage tubular reactor, and the second-stage tubular reactor is provided with a porous baffle, and a cooling jacket with a jacket is arranged outside the pipe. The flow rate of the material in the second section of the tubular reactor is 0.001m / s, the residence time is 7 hours, and the temperature of the second section of the tubular reactor is 40°C-45°C. At the reaction ou...

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Abstract

The invention discloses a method for continuously synthesizing O,S-dimethyl phosphoroamidothioate based on a pipe type reaction device. According to the method, O,O-dimethyl phosphoroamidothioate and dimethyl sulfate are used as raw materials, and O,S-dimethyl phosphoroamidothioate is continuously synthesized by virtue of the pipe type reaction device; the pipe type reaction device comprises two sections of pipe type reactors which are connected in series, and the temperature in each pipe type reactor is set to be appropriate during reaction; and O,O-dimethyl phosphoroamidothioate and dimethyl sulfate are continuously pumped into the first section of the pipe type reactors after being metered to perform mixing and reaction, and then flow through the second section of the pipe type reactors for further reaction, so that an O,S-dimethyl phosphoroamidothioate product is continuously obtained from a material outlet of the second section of the pipe type reactors. The method is high in reaction efficiency and high in equipment utilization ratio, a single set of reaction device is high in productivity, the reaction process is easy to control, the safety performance is good, and the requirements for industrial production can be met.

Description

technical field [0001] The invention relates to a method for continuously synthesizing O, S-dimethylphosphorothioate, which belongs to the field of organic synthesis. Background technique [0002] At present, with the continuous increase of the world population, the emergence of a series of problems such as global warming and land desertification, the arable land area is decreasing year by year, and the demand for food is becoming more and more tense. To ensure food security and supply, we must increase food production. As an effective means of preventing and resisting pests and weeds, chemical pesticides are an important guarantee for controlling hazards, reducing losses, and ensuring high and stable yields of crops. Therefore, the research and development of high-efficiency and low-toxic chemical pesticides has immeasurable practical significance for reducing environmental pollution, protecting human health and improving corporate benefits. [0003] O,S-Dimethylthiophosp...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/24B01J19/24
Inventor 艾秋红文敬滨罗和安倪小斌游奎一刘平乐黄荣辉
Owner XIANGTAN UNIV
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