Diquat synthesizing and refining technology

A diquat and refining technology, applied in herbicides and algaecides, chemicals for biological control, animal repellents, etc., can solve the problem of high consumption of dibromoethane raw materials, affecting the synthesis of diquat efficiency, increase the difficulty of exhaust gas treatment, etc., to achieve the effect of reducing material consumption, shortening reaction time, and reducing toluene consumption

Active Publication Date: 2018-10-16
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

But in prior art method, adopt reflux insulation reaction more, make whole reaction cycle reach more than 18h; The solid obtained by the filtration process not only cannot remove the impurities generated during the reaction, which affects the reaction yield, but also because the dibromoethane raw material has strong corrosion and volatility, it will increase the tail gas during the filter press drying process. The difficulty of processing makes the consumption of dibromoethane raw material higher, which increases the production cost; moreover,

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Diquat synthesis and refining process described in the present embodiment comprises the following steps:

[0024] (1) Precipitation: Take the bipyridyl toluene liquid and remove the solvent toluene through a two-stage thin-film evaporator under reduced pressure to obtain 2.2-bipyridine, and control the temperature during vacuum distillation to be 120-150°C for subsequent use;

[0025] (2) Synthesis: Take 600kg of 2.2-bipyridine obtained in the above step (1) and 6000kg of 1,2-dibromoethane, add them to the reaction kettle in turn, heat up to 140-160°C for heat preservation reaction, and take samples during the reaction Analysis, when the content of 2.2-bipyridine≦2% (compared with the initial amount), the reaction is terminated, and the total reaction time is 11 hours;

[0026] (3) Layering: after the reaction, add 1000 kg of water to the reaction kettle to mix evenly, and let the reaction solution stand still for 2 hours before layering, and separate the lower layer of...

Embodiment 2

[0032] Diquat synthesis and refining process described in the present embodiment comprises the following steps:

[0033] (1) Precipitation: Take the bipyridyl toluene liquid and remove the solvent toluene through a two-stage thin-film evaporator under reduced pressure to obtain 2.2-bipyridine, and control the temperature during vacuum distillation to be 120-150°C for subsequent use;

[0034] (2) Synthesis: Take 600kg of 2.2-bipyridine obtained in the above step (1) and 6300kg of 1,2-dibromoethane, add them to the reaction kettle in turn, heat up to 140-160°C, and carry out insulation reaction. Sampling analysis, when the content of 2.2-bipyridine≦2% (compared with the initial amount), the reaction is terminated, and the total reaction time is 12 hours;

[0035] (3) Layering: after the reaction, add 13300 kg of water to the reaction kettle to mix evenly, and separate the reaction liquid for 3 hours to separate the lower layer of 1,2-dibromoethane to obtain a reaction liquid con...

Embodiment 3

[0041] Diquat synthesis and refining process described in the present embodiment comprises the following steps:

[0042] (1) Precipitation: Take the bipyridyl toluene liquid and remove the solvent toluene through a two-stage thin-film evaporator under reduced pressure to obtain 2.2-bipyridine, and control the temperature during vacuum distillation to be 120-150°C for subsequent use;

[0043] (2) Synthesis: Take 630kg of 2.2-bipyridine obtained in the above step (1) and 6000kg of 1,2-dibromoethane, add them to the reaction kettle in turn, heat up to 140-160°C, and carry out insulation reaction. Sampling analysis, when the content of 2.2-bipyridine≦2% (compared with the initial amount), the reaction is terminated, and the total reaction time is 12 hours;

[0044] (3) Layering: after the reaction, add 1500 kg of water to the reaction kettle to mix evenly, and separate the reaction liquid for 4 hours to separate the lower layer of 1,2-dibromoethane to obtain a reaction liquid cont...

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PUM

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Abstract

The invention belongs to the technical field of pesticide preparation synthesis, and specifically relates to a diquat synthesizing and refining technology. According to the diquat synthesizing and refining technology provided by the invention, a diquat aqueous solution is prepared by the steps such as desolvation, synthesis, layering, filtering, regulation of pH value, extraction and distillation.

Description

technical field [0001] The invention belongs to the technical field of pesticide preparation synthesis, and specifically relates to a diquat synthesis and refining process. Background technique [0002] Diquat, the chemical name is 1,1'-ethylene-2,2'-bipyridine dibromide, is a non-selective contact herbicide and desiccant developed by British Syngenta Chemical Company. It is also one of the most widely used herbicide products in the world, second only to glyphosate and paraquat in global sales and usage. [0003] Diquat is generally used as a conductive contact-killing biogenic herbicide, which can be quickly absorbed by green plant tissues, and will lose its activity soon after contact with the soil. It is mostly used for weeding in fields, orchards, non-arable land, and before harvesting. It can be used as stem and leaf withering of potatoes and sweet potatoes; in places where grass weeds are serious, it is better to use diquat and paraquat together. Diquat generally exi...

Claims

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Application Information

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IPC IPC(8): C07D471/14A01N43/90A01N25/02A01P13/00
CPCA01N25/02A01N43/90C07D471/14
Inventor 徐龙腾王志勇孙立宝
Owner 德州绿霸精细化工有限公司
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