A preparation method of pendimethalin and the application of the waste water produced by the preparation method in the treatment of chlorpyrifos waste water

A pendimethalin and amylamine technology, which is applied in the preparation of pendimethalin and the application field of treating chlorpyrifos wastewater, can solve the problems of excessive discharge of three wastes, increase of production cost of enterprises, environmental pollution and the like

Active Publication Date: 2020-07-07
山东华阳农药化工集团有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The national standard of pendimethalin technical GB22177-2008 requires a content of more than 95%. At present, in the domestic market, the content of pendimethalin in circulation is mainly 95%, and the content required for export is greater than 97%. The pendimethalin product has a primary synthesis content of 90-93%, which does not meet the national standard. It needs to be refined and purified on the basis of the pendimethalin prepared by the existing preparation method, and this process will increase production. cost
In addition, in the existing process of preparing pendimethalin, more three wastes are discharged, which will not only cause environmental pollution, but also correspondingly increase the production cost of the enterprise

Method used

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  • A preparation method of pendimethalin and the application of the waste water produced by the preparation method in the treatment of chlorpyrifos waste water
  • A preparation method of pendimethalin and the application of the waste water produced by the preparation method in the treatment of chlorpyrifos waste water
  • A preparation method of pendimethalin and the application of the waste water produced by the preparation method in the treatment of chlorpyrifos waste water

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0059] Unless otherwise specified, the content of each component used below is a mass percentage.

[0060] S1. Synthetic Nitrification

[0061] Such as figure 1 As shown, using pentylamine as a raw material, pentylamine reacts with dilute nitric acid to form a quaternary ammonium salt. In this embodiment, pentylamine is put into a salt-forming kettle and dissolved in methanol, wherein the molar ratio of pentylamine to methanol is 1:1200. After being fully dissolved, it reacts with dilute nitric acid to form a quaternary ammonium salt, in which the molar ratio of pentylamine to dilute nitric acid is 1:1.5.

[0062] The quaternary ammonium salt reacts with concentrated nitric acid to produce pendimethalin nitrated oil phase. In this embodiment, the generated quaternary ammonium salt is added to concentrated nitric acid under the protection of nitrogen for nitration reaction to generate pendimethalin nitrated oil phase, wherein the molar ratio of amylamine to concentrated nitric acid ...

Embodiment 2

[0072] S1. Synthetic Nitrification

[0073] Such as figure 1 As shown, using pentylamine as a raw material, pentylamine reacts with dilute nitric acid to form a quaternary ammonium salt. In this embodiment, pentylamine is put into the salt-forming kettle and dissolved in dichloroethane, wherein the molar ratio of pentylamine to dichloroethane is 1:60. After being fully dissolved, it reacts with dilute nitric acid to form a quaternary ammonium salt, in which the molar ratio of pentylamine to dilute nitric acid is 1:0.8.

[0074] The quaternary ammonium salt reacts with concentrated nitric acid to produce pendimethalin nitrated oil phase. In this embodiment, the generated quaternary ammonium salt is added to concentrated nitric acid under the protection of nitrogen for nitration reaction to generate pendimethalin nitrated oil phase, wherein the molar ratio of amylamine to concentrated nitric acid is 1:1.6. After the nitrification is completed, the nitrified oil phase of pendimethal...

Embodiment 3

[0084] S1. Synthetic Nitrification

[0085] Such as figure 1 As shown, using pentylamine as a raw material, pentylamine reacts with dilute nitric acid to form a quaternary ammonium salt. In this embodiment, pentylamine was put into a salt-forming kettle and dissolved in chloroform, where the molar ratio of pentylamine to chloroform was 1:40. After being fully dissolved, it reacts with dilute nitric acid to form a quaternary ammonium salt, in which the molar ratio of pentylamine to dilute nitric acid is 1:0.6.

[0086] The quaternary ammonium salt reacts with concentrated nitric acid to produce pendimethalin nitrated oil phase. In this embodiment, the generated quaternary ammonium salt is added to concentrated nitric acid under the protection of nitrogen for nitration reaction to generate pendimethalin nitrated oil phase, wherein the molar ratio of amylamine to concentrated nitric acid is 1:1.2. After the nitrification is completed, the nitrified oil phase of pendimethalin and nit...

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Abstract

The invention discloses a preparation method of pendimethalin and application of wastewater generated by the preparation method to treatment of chlorpyrifos wastewater, and belongs to the technical field of drug preparation. According to the preparation method of the pendimethalin, which is disclosed by the invention, amylamine is used as a raw material, and the pendimethalin is synthesized by synthetic nitration and synthetic raw medicine reactions. The preparation method of the pendimethalin, which is disclosed by the invention, is simple in operation process, product quality of the pendimethalin can be greatly improved, the discharge of three waste, such as waste gas, waste water and waste solid can be reduced, production cost is reduced, the profit space is enlarged, the market competitiveness of the product is reinforced, and the preparation method has very wide popularization value.

Description

Technical field [0001] The invention relates to the technical field of medicine preparation, and specifically provides a preparation method of pendimethalin and the application of wastewater produced by the preparation method in the treatment of chlorpyrifos wastewater. Background technique [0002] Pendimethalin is an orange crystalline solid with a melting point of 54-58°C, a boiling point of 300°C, a density of 1.17, and solubility (25°C): 0.275mg / L in water, easily soluble in organic solvents such as acetone and xylene. . Pendimethalin ranks eighth in the world's best-selling pesticide rankings, with sales of 350 million US dollars per year. It is the world's third largest herbicide after the biocidal herbicides glyphosate and paraquat. One of the largest-selling selective herbicides on the market. It can be widely used for weeding in corn, soybeans, peanuts, cotton, direct seeded upland rice, potatoes, tobacco, vegetables and other crop fields. [0003] my country's pendimet...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C209/76C07C209/82C07C209/00C07C211/52C02F9/04C02F103/34
CPCC02F1/66C02F1/72C02F1/725C02F2103/343C07C209/00C07C209/76C07C209/82C07C211/52
Inventor 孙绪兵闫新华李振兴宋文勇陈永平韩萍
Owner 山东华阳农药化工集团有限公司
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