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Method for recovering imidacloprid from imidacloprid production concentrated mother liquor residues

A technology of imidacloprid and mother liquor, applied in the direction of organic chemistry, etc., can solve the problems of increased processing costs, high consumption, high production costs, etc.

Pending Publication Date: 2022-07-01
JIANGSU CHANGLONG AGROCHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It turned out that it was treated as solid waste, which not only increased the treatment cost, but also had low yield, high consumption and high production cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] The concentrated mother liquor of imidacloprid production (100g) was put into a four-necked flask, 100g of dichloroethane was added, 27.6g (0.2344mol) of 31% hydrochloric acid was added dropwise with stirring, the reaction was exothermic, and the reaction temperature was kept below 35°C. After the dropwise addition was completed, the mixture was stirred for 30 minutes and then allowed to stand for 1 hour. The lower solvent layer was separated, and the solvent layer was concentrated to remove residue. Add 20 g of dichloroethane to the water layer, add 30% sodium hydroxide solution dropwise with stirring, neutralize to pH 7-8, stand for stratification, cool the solvent layer for crystallization, filter at -5 to 0 °C, and dry to obtain imidacloprid. 18.9 g with a purity of 97.12%. The product recovery rate is 61.18%. The filtrate was combined into the first solvent layer to remove the leaching residue.

Embodiment 2

[0017] The concentrated mother liquor of imidacloprid production (100g) was put into a four-necked flask, 100g of dichloroethane was added, 20.7g (0.1758mol) of 31% hydrochloric acid was added dropwise with stirring, the reaction was exothermic, and the reaction temperature was kept below 35°C. After the dropwise addition was completed, the mixture was stirred for 30 minutes and then allowed to stand for 1 hour. The lower solvent layer was separated, and the solvent layer was concentrated to remove residue. Add 20 g of dichloroethane to the water layer, add 30% sodium hydroxide solution dropwise with stirring, neutralize to pH 7-8, stand for stratification, cool the solvent layer for crystallization, filter at -5 to 0 °C, and dry to obtain imidacloprid. 17.04g with a purity of 97.03%. The product recovery rate was 55.12%. The filtrate was combined into the first solvent layer to remove the leaching residue.

Embodiment 3

[0019] The concentrated mother liquor of imidacloprid production (100g) was put into a four-necked flask, 100g of dichloromethane was added, 27.6g (0.2344mol) of 31% hydrochloric acid was added dropwise with stirring, the reaction was exothermic, and the reaction temperature was kept below 35°C. After the dropwise addition was completed, the mixture was stirred for 30 minutes and then allowed to stand for 1 hour. The lower solvent layer was separated, and the solvent layer was concentrated to remove residue. 20g of dichloromethane was added to the water layer, 30% sodium hydroxide solution was added dropwise with stirring, neutralized to pH 7-8, left to stand for stratification, the solvent layer was cooled and crystallized, filtered at -5~0°C, and dried to obtain imidacloprid product 18.1 g, the purity is 97.22%. The product recovery rate is 58.66%. The filtrate was combined into the first solvent layer to remove the leaching residue.

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Abstract

The invention provides a method for recovering imidacloprid from imidacloprid production concentrated mother liquor residues. The method comprises the following steps: adding a non-polar solvent into imidacloprid concentrated mother liquor residues at 0-35 DEG C under a stirring condition, dropwise adding an inorganic strong acid, and reacting the inorganic strong acid with imidacloprid in the mother liquor residues according to a molar ratio of (1.0-5.0): 1; and after stirring for a certain time, standing to separate out an acid water layer, adding a non-polar solvent into the acid water layer, dropwise adding alkali liquor while stirring to neutralize until the pH value is 7-8, standing to separate out a solvent layer, cooling, crystallizing and filtering to obtain the product imidacloprid. After the product imidacloprid is recovered from mother liquor concentrated residues, the synthesis yield of the product is improved while three wastes are reduced.

Description

[0001] Technology leader [0002] The invention relates to a method for recovering imidacloprid products from the concentrated mother liquor residue of imidacloprid production. Background technique [0003] Imidacloprid, 1-(6-chloro-3-pyridylmethyl)-N-nitroimidazolidine-2-imine, is a chloronicotinyl pesticide that can be absorbed internally and is used for Soil, seeds and leaves to prevent and control pests with sucking mouthparts, including ricehoppers, aphids, thrips, whiteflies, termites, lawn pests, and underground pests and beetles. This insecticide is most commonly used on rice, cereals, corn, potatoes, vegetables, sugar beets, fruits, cotton, hops or turf. The insecticide is particularly systemically absorbed when used in seed or soil treatments. [0004] In the production of imidacloprid, after the centrifuged mother liquor of the product is distilled to recover the solvent, a large amount of concentrated mother liquor residue is produced. About 250kg of concentrate...

Claims

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Application Information

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IPC IPC(8): C07D401/06
CPCC07D401/06
Inventor 王卫华张昭荣金小波田庆海何小捷徐勤业芮燕春
Owner JIANGSU CHANGLONG AGROCHEM CO LTD
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