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Method for recovering sodium trichloropyrindinol from sodium trichloropyrindinol production waste

A technology of sodium trichloropyridine and the sodium trichloropyridine, applied in directions such as organic chemistry, can solve problems such as time-consuming alkaline hydrolysis, a lot of catalyst consumption, long time, etc., and achieve the effect of cost saving

Active Publication Date: 2017-01-04
CHONGQING HUAGE BIOCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the process cost of separating and purifying tetrachloropyridine from the waste with many impurities is high, and the time is long, and it is also time-consuming to carry out alkaline hydrolysis of the purified solid tetrachloropyridine, and the yield is not ideal
In the prior art, catalysts are also used to realize waste treatment. Although such a method has a good yield, the amount of catalyst used is not small, which may lead to catalyst residues while causing a large amount of waste of catalysts. Once the pesticides with catalyst residues put into use, it may be enriched by plants and eventually cause harm to the human body

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] The present embodiment provides a kind of method that reclaims clopyridox sodium from the clopyridox sodium production waste:

[0026] 15.0kg of water and 7.5kg of sodium hydroxide solution with a concentration of 30wt% were dropped into the alkaline hydrolysis kettle, and stirred and mixed evenly to obtain the first lye. Turn on the circulating condensed water, and control the temperature in the alkaline hydrolysis tank to not be higher than 50°C. Take 4.5 kg of sodium clopyridinate production waste and drop it slowly and uniformly into the alkaline hydrolysis kettle within 6 to 7 hours. After the dropwise addition, continue to react for 1 to 2 hours, take out and press filter to obtain the crude product of alkali hydrolysis. During the reaction, check the pH every 20 minutes, replenish the sodium hydroxide solution in time and control the pH of the reaction between 10 and 12.

[0027] Put 20kg of water and 4.0kg of solid sodium hydroxide into the high-pressure alkal...

Embodiment 2

[0029] The present embodiment provides a kind of method that reclaims clopyridox sodium from the clopyridox sodium production waste:

[0030] Put 16.0kg of water and 4.0kg of sodium hydroxide solid into the alkaline hydrolysis kettle, stir and mix evenly to obtain the first lye. Turn on the circulating condensed water, and control the temperature in the alkaline hydrolysis tank to not be higher than 55°C. Take 4.5 kg of sodium clopyridinate production waste and drop it slowly and uniformly into the alkaline hydrolysis kettle within 7 to 8 hours. After the dropwise addition, continue to react for 2 to 3 hours, take out and press filter to obtain the crude product of alkali hydrolysis. During the reaction, check the pH every 20 minutes, replenish the sodium hydroxide solution in time and control the pH of the reaction between 12 and 14.

[0031] Put 20kg of water and 2.0kg of solid sodium hydroxide into the high-pressure alkali analysis kettle, stir and mix evenly to obtain th...

Embodiment 3

[0033] The present embodiment provides a kind of method that reclaims clopyridox sodium from the clopyridox sodium production waste:

[0034] Put 6.0kg of water and 18.0kg of 40wt% sodium hydroxide solution into the alkaline hydrolysis kettle, stir and mix evenly to obtain the first lye. Turn on the circulating condensed water, and control the temperature in the alkaline hydrolysis tank to not be higher than 60°C. Take 4.5 kg of sodium clopyridinate production waste and drop it slowly and uniformly into the alkaline hydrolysis kettle within 8 to 9 hours. After the dropwise addition, continue to react for 3 to 4 hours, take out and press filter to obtain the crude product of alkali hydrolysis. During the reaction, check the pH every 20 minutes, replenish the sodium hydroxide solution in time and control the pH of the reaction between 11 and 13.

[0035]Put 20kg of water and 6.0kg of solid sodium hydroxide into the high-pressure alkali analysis kettle, stir and mix evenly to o...

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Abstract

The invention provides a method for recovering sodium trichloropyrindinol from sodium trichloropyrindinol production waste and belongs to the field of chemical engineering. The method comprises the steps that the sodium trichloropyrindinol production waste and a first alkali liquor are mixed to perform first-time alkaline hydrolysis reaction, and an alkaline-hydrolysis coarse material is obtained; the alkaline-hydrolysis coarse material is mixed with a second alkali liquor to perform second-time alkaline hydrolysis reaction, wherein the second-time alkaline hydrolysis reaction is performed under the pressure of 0.1-0.6 MPa and the temperature of 100-160 DEG C. By the adoption of the method, the sodium trichloropyrindinol can be recovered in a high-yield and high-purity mode. The method is simple in operation, the device requirements are not high, the production cost is low, and the method can be adopted in a large-scale mode. The wastewater obtained after treatment conducted by adopting the method can be directly discharaged into a biochemical pool, the trouble of further treatment is omitted, and the wastewater treatment cost is saved.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a method for recovering sodium clopyridinate from production waste of clopyridinate sodium. Background technique [0002] 3,5,6-Triclopyridin-2-sodium, referred to as triclopyridine sodium, is an important chemical raw material, and it is also used to synthesize organic phosphorus insecticides such as chlorpyrifos, chlorpyrifos-methyl, and herbicide triclopyr, etc. An important intermediate of many pesticides. The production process of clopyridinate sodium is mainly the addition of trichloroacetyl chloride and acrylonitrile to generate butyryl chloride, which is cyclized to obtain pyridin-4(1H)-one (hereinafter referred to as pyridone), and pyridone in alkaline conditions Under the formation of sodium alkoxide. During the cyclization of butyryl chloride to generate pyridone, a large amount of waste will be produced, which contains more by-product tetrachloropyridine, some pyrid...

Claims

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Application Information

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IPC IPC(8): C07D213/64
CPCC07D213/64
Inventor 何小强蒲桃刘涛李传武林军万雪琴
Owner CHONGQING HUAGE BIOCHEM
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