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

3 Cites 1 Cited by

AI-Extracted 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 real...

Method used

Can find out that a kind of method that the present invention adopts reclaims clopyridinate sodium from the production waste of clopyridinate sodium by above comparison adopts the mode of step-by-step alkaline hydrolysis, can high yield, the recovery of high purity Triclopyridin Sodium. The method is simp...

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.

Application Domain

Organic chemistry

Technology Topic

ScrapChemistry +5

Examples

Experimental program(6)
Comparison scheme(2)
Effect test(1)

Example Embodiment

[0024] Example 1

[0025] This embodiment provides a method for recovering sodium triclopyridine from the production waste of triclopyridine sodium:

[0026] Put 15.0 kg of water and 7.5 kg of 30 wt% sodium hydroxide solution into the alkaline hydrolysis kettle, stir and mix uniformly to obtain the first lye. Turn on the circulating condensate and control the temperature in the alkaline hydrolysis kettle to not be higher than 50°C. Take 4.5 kg of sodium triclopyridate production waste and add it slowly and uniformly into the alkaline hydrolysis kettle within 6-7 hours. After the addition is complete, the reaction is continued for 1 to 2 hours, and then taken out for pressure filtration to obtain the crude alkaline hydrolysis product. During the reaction, the pH is checked every 20 minutes, the sodium hydroxide solution is added in time, and the pH of the reaction is controlled between 10-12.

[0027] Put 20kg of water and 4.0kg of solid sodium hydroxide into the high-pressure alkaline precipitation kettle, stir and mix uniformly to obtain the second lye. The crude alkaline hydrolysis product is added to a high-pressure alkaline precipitation kettle, the pressure is increased to 0.1MPa, and the temperature is increased to 110°C to react for 3 hours to obtain a primary alkaline hydrolysis material. The primary alkaline hydrolysis material is pressurized again to 0.2MPa, and the temperature is raised to 120° C. to react for 2 hours to obtain the secondary alkaline hydrolysis material. The secondary alkaline hydrolysis material is taken out and filtered to obtain sodium triclopyridate.

Example Embodiment

[0028] Example 2

[0029] This embodiment provides a method for recovering sodium triclopyridine from the production waste of triclopyridine sodium:

[0030] Put 16.0 kg of water and 4.0 kg of sodium hydroxide solid into the alkaline hydrolysis kettle, stir and mix uniformly to obtain the first lye. Turn on the circulating condensate, and control the temperature in the alkaline hydrolysis kettle to not be higher than 55°C. Take 4.5 kg of sodium triclopyridine production waste and add it slowly and uniformly into the alkaline hydrolysis kettle within 7-8 hours. After the dripping is completed, the reaction is continued for 2 to 3 hours, and then taken out for pressure filtration to obtain the crude alkaline hydrolysis product. During the reaction, the pH was checked every 20 minutes, the sodium hydroxide solution was added in time, and the pH of the reaction was controlled between 12 and 14.

[0031] Put 20kg of water and 2.0kg of solid sodium hydroxide into the high-pressure alkaline precipitation kettle, stir and mix uniformly to obtain the second lye. The crude alkaline hydrolysis product is added to a high-pressure alkaline precipitation kettle, the pressure is increased to 0.2MPa, and the temperature is raised to 120°C to react for 5 hours to obtain a primary alkaline hydrolysis material. The primary alkaline hydrolysis material is re-pressurized to 0.3 MPa, and the temperature is raised to 130° C. to react for 3 hours to obtain the secondary alkaline hydrolysis material. The secondary alkaline hydrolysis material is taken out and filtered to obtain sodium triclopyridate.

Example Embodiment

[0032] Example 3

[0033] This embodiment provides a method for recovering sodium triclopyridine from the production waste of triclopyridine sodium:

[0034] Put 6.0 kg of water and 18.0 kg of 40 wt% sodium hydroxide solution into the alkaline hydrolysis kettle, stir and mix uniformly to obtain the first lye. Turn on the circulating condensate, and control the temperature in the alkaline hydrolysis kettle to not be higher than 60°C. Take 4.5 kg of sodium triclopyridine production waste and add it slowly and uniformly into the alkaline hydrolysis kettle within 8-9 hours. After the dripping is completed, the reaction is continued for 3 to 4 hours, and then taken out for pressure filtration to obtain the crude alkali hydrolysis. During the reaction, the pH was checked every 20 minutes, the sodium hydroxide solution was added in time, and the pH of the reaction was controlled between 11-13.

[0035] Put 20kg of water and 6.0kg of solid sodium hydroxide into the high-pressure alkaline precipitation kettle, stir and mix uniformly to obtain the second lye. The crude alkaline hydrolysis product is added to a high-pressure alkaline precipitation kettle, pressurized to 0.4 MPa, and heated to 140° C. to react for 6 hours to obtain a primary alkaline hydrolysis material. The primary alkaline hydrolysis material is re-pressurized to 0.5 MPa, and the temperature is raised to 150° C. to react for 4 hours to obtain the secondary alkaline hydrolysis material. The secondary alkaline hydrolysis material is taken out and filtered to obtain sodium triclopyridine.

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Description & Claims & Application Information

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Classification and recommendation of technical efficacy words

low cost

Method, apparatus and article for microfluidic control via electrowetting, for chemical, biochemical and biological assays and the like

InactiveUS7163612B2low cost

Owner:KECK GRADUATE INST OF APPLIED LIFE SCI

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

AI-Extracted Technical Summary

Problems solved by technology

Method used

Abstract

Examples

Example Embodiment

Example Embodiment

Example Embodiment

PUM

Description & Claims & Application Information

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