Diquat synthesis novel process

A diquat and extraction technology, applied in the direction of organic chemistry, can solve the problems of low reaction yield, cumbersome process flow, high production cost, etc., and achieve the effect of simple process, high reaction yield and low production cost

Active Publication Date: 2013-03-20
ANHUI COSTAR BIOCHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method is very complicated from the synthesis of raw material 2,2'-bipyridine to the cyclization of 2,2'-bipyridine and dibromoethane. At...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Embodiment 1: the new technique of diquat synthesis comprises the following steps:

[0021] (1) Coupling: 125kg of 2-chloropyridine, 250kg of solvent DMAC, 70kg of catalyst triphenylphosphine, 60kg of zinc powder, and 5kg of nickel chloride were added to the reaction kettle in sequence, and the temperature was raised to 60°C for 2 hours, and the sample was analyzed;

[0022] (2) Precipitation: Step (1) After sampling and analysis, when the 2-chloropyridine content is less than 0.5%, the reaction is over, the temperature is controlled at 100°C, and the solvent DMAC is removed under reduced pressure;

[0023] (3) Alkaline hydrolysis: Add 900kg of 20% ammonia water and 150kg of ammonium sulfate to the solid obtained in step (2) and raise the temperature to 40°C for alkaline hydrolysis for 4 hours, then add 900kg of toluene, and press filter to obtain the filtrate;

[0024] (4) Extraction: The filtrate after step (3) is subjected to liquid separation, toluene extraction, an...

Embodiment 2

[0031] Embodiment 2: the new technique of diquat synthesis comprises the following steps:

[0032] (1) Coupling: 130kg of 2-chloropyridine, 300kg of solvent DMAC, 75kg of catalyst triphenylphosphine, 70kg of zinc powder, and 10kg of nickel chloride were added to the reaction kettle in sequence, and the temperature was raised to 70°C for 2 hours, and the sample was analyzed;

[0033] (2) Precipitation: Step (1) After sampling and analysis, when the 2-chloropyridine content is less than 0.5%, the reaction is over, the temperature is controlled at 110°C, and the solvent DMAC is removed under reduced pressure;

[0034] (3) Alkaline hydrolysis: Add 1000kg of 20% ammonia water and 250kg of ammonium sulfate to the solid obtained in step (2) and raise the temperature to 40°C for alkaline hydrolysis for 4 hours, then add 950kg of toluene, and press filter to obtain the filtrate;

[0035] (4) Extraction: The filtrate after step (3) is subjected to liquid separation, toluene extraction, ...

Embodiment 3

[0042] Embodiment 3: the new technique of diquat synthesis comprises the following steps:

[0043] (1) Coupling: 125kg of 2-chloropyridine, 300kg of solvent DMAC, 70kg of catalyst triphenylphosphine, 60kg of zinc powder, and 5kg of nickel chloride were added to the reaction kettle in sequence, and the temperature was raised to 90°C for 3 hours, and the sample was analyzed;

[0044] (2) Precipitation: Step (1) After sampling and analysis, when the 2-chloropyridine content is less than 0.5%, the reaction is over, the temperature is controlled at 120°C, and the solvent DMAC is removed under reduced pressure;

[0045] (3) Alkaline hydrolysis: Add 900kg of 20% ammonia water and 250kg of ammonium sulfate to the solid obtained in step (2) and raise the temperature to 60°C for alkaline hydrolysis for 5 hours, then add 950kg of toluene, and press filter to obtain the filtrate;

[0046] (4) Extraction: The filtrate after step (3) is subjected to liquid separation, toluene extraction, an...

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PUM

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Abstract

The present invention discloses a diquat synthesis novel process, which prepares a diquat water agent mainly through the steps of coupling, alkaline hydrolysis, extraction, cyclization, extraction, and decoloration. The whole process of the invention is simple in process, high in reaction yield, low in production cost and environment-friendly.

Description

technical field [0001] The invention relates to a synthesis process of herbicide, in particular to a new synthesis process of diquat. Background technique [0002] Diquat is a non-selective contact herbicide and desiccant developed by British Syngenta Chemical Company. It is one of the most widely used herbicide products in the world. Glyphosate and Paraquat. [0003] Diquat generally exists in the form of dibromide monohydrate, and the commercially available diquat preparations are generally 20% aqueous formulations. [0004] The traditional method of preparing diquat is to co-heat the main raw materials 2,2'-bipyridine and dibromoethane. However, this method is very complicated from the synthesis of raw material 2,2'-bipyridine to the cyclization of 2,2'-bipyridine and dibromoethane. At the same time, the reaction yield is low and the production cost is high. Influencing factors restricting the popularization of diquat synthesis process. [0005] In order to increase t...

Claims

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Application Information

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IPC IPC(8): C07D471/14
Inventor 李健葛九敢刘善和黎广王红明
Owner ANHUI COSTAR BIOCHEM CO LTD
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