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Method for recycling imidacloprid from imidacloprid production mother liquor

A technology for imidacloprid mother and imidacloprid, which is applied in the field of imidacloprid recovery, can solve the problems of increased cost, consumption, large spermatozoa and the like, and achieves the effects of stable operation, easy process flow and convenient operation.

Inactive Publication Date: 2009-05-20
荆州沙隆达控股有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this treatment is: the preparation of 10% powder consumes a large amount of refined raw powder, so that the yield of 95% refined raw powder is only 57%, which increases the cost of production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] Take 300g of imidacloprid mother liquor after the condensation reaction, containing 25.3% of imidacloprid, heat up to 45-50°C, add 600g of dichloromethane, stir evenly, and the material is transparent. Remove the water bath, stir at room temperature for 30 min, and a large amount of solid precipitates out. Then the temperature was lowered to 0° C. to crystallize for 2 hours, and after filtration and centrifugal drying, 158 g of imidacloprid dry powder was obtained, with a content of 40% and a recovery rate of 83.3%. The dry powder can be directly formulated into 10% imidacloprid powder without adding essence powder.

Embodiment 2

[0013] Take 300g of imidacloprid mother liquor after the condensation reaction, containing 24.6% of imidacloprid, heat up to 45-50°C, add 450g of methanol, stir evenly, and the material is transparent. Remove the water bath, stir at room temperature for 30 minutes, a large amount of solid precipitates, and add 40 g of light calcium carbonate. Then the temperature was lowered to 0° C. to crystallize for 2 hours, and after filtration and centrifugal drying, 192 g of imidacloprid dry powder was obtained, with a content of 32.5% and a recovery rate of 84.6%. The dry powder can be directly formulated into 10% imidacloprid powder without adding essence powder.

Embodiment 3

[0015] Get the imidacloprid mother liquor 300g after the condensation reaction, contain imidacloprid 24.6%, be warming up to 45~50

[0016] ℃, add butanone 450g, stir evenly, remove the water bath, stir at room temperature for 30min, a large amount of solids precipitate out. Then cool down to 5° C. to crystallize for 2 hours, filter and dry to obtain 120.5 g of imidacloprid dry powder with a content of 49.0% and a recovery rate of 80.0%. The dry powder can be directly formulated into 10% imidacloprid powder without adding essence powder.

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PUM

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Abstract

The invention relates to a reclamation method of a pesticide, in particular to a method for reclaiming imidacloprid from an imidacloprid production mother solution. The imidacloprid production mother solution is heated to 45 DEG C to 50 DEG C, added with an organic solvent and stirred, then naturally cooled until solids are separated out, and then the soulution is cooled to minus 10 DEG C for crystallizing, filtered and dried to obtain imidacloprid powder; the mother solution is distilled and solvents in the mother solution are reclaimed. The method can greatly promote the yield of imidacloprid original fine powder; the yield of the 95-percent original fine powder is promoted from 57 percent to 87 percent.

Description

technical field [0001] The invention relates to a method for recovering pesticides, in particular to a method for recovering imidacloprid from imidacloprid production mother liquor. Background technique [0002] Imidacloprid is a super-efficient neonicotinoid insecticide with broad-spectrum, high efficiency, low toxicity, and low residue. It is not easy for pests to develop resistance, and it is safe for humans, animals, plants, and natural enemies. It also has contact, stomach, and systemic toxicity. and other multiple functions. At present, in the synthesis of imidacloprid in my country, 2-chloro-5-chloromethylpyridine (CCMP) is used as a raw material, which is condensed with nitroimidazolidine in the presence of solvent and anhydrous potassium carbonate to obtain pure imidacloprid. In addition to obtaining essence powder with a content of 95%, this method also produces a large amount of mother liquor. Due to the high viscosity of the mother liquor, it is not easy to be ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D401/06A01P7/00
Inventor 何福春殷宏薛光才刘孝平周骋戴锋鄢圣光廖艳何红霞张诗忠
Owner 荆州沙隆达控股有限公司