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A kind of separation and purification method of 2-chloro-5-chloromethylthiazole

A technology of chloromethylthiazole and a purification method, applied in the direction of organic chemistry and the like, can solve the problems of high difficulty and high cost of dilute acid recovery and treatment, and achieve the effects of small amount of three wastes, stable quality and low energy consumption

Active Publication Date: 2016-09-21
SHANDONG ACADEMY OF PESTICIDE SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The concentration of a large amount of dilute acid formed is about 18%, which contains a large amount of organic matter. The recovery and treatment of this part of dilute acid is very costly and difficult

Method used

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  • A kind of separation and purification method of 2-chloro-5-chloromethylthiazole
  • A kind of separation and purification method of 2-chloro-5-chloromethylthiazole
  • A kind of separation and purification method of 2-chloro-5-chloromethylthiazole

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] (1) Washing: In a washing kettle, dissolve 400kg of crude 2-chloro-5-chloromethylthiazole in 300kg of dichloroethane, add 900kg of water in batches for washing, and the pH value of the organic phase of washing is 6~ 7. After washing with water, separate the lower organic phase;

[0044] (2) Adsorption and color removal: Add 50kg of activated carbon to the material obtained in step (1), and stir at 40°C for 3 hours until the color of the mother liquor changes from dark yellow to light yellow;

[0045] (3) Pressure filtration: transfer the material obtained in step (2) to a pressure filter kettle for pressure filtration, and the light yellow material obtained by pressure filtration enters the collection tank;

[0046](4) Precipitation: Transfer the material in the collection tank of step (3) to the precipitator, and distill dichloroethane at 50-60°C under a pressure of -0.06 to -0.07 bar to obtain dichloroethane It can be directly applied to step (1) as a dissolving solv...

Embodiment 2

[0050] (1) Washing: In a washing kettle, dissolve 400kg of crude 2-chloro-5-chloromethylthiazole in 150kg of toluene, add 900kg of water in batches for washing, the pH value of the organic phase of washing is 6-7, wash with water After completion, separate the lower organic phase;

[0051] (2) Adsorption and color removal: Add 25kg of macroporous adsorption resin to the material obtained in step (1), and stir at 35°C for 3 hours until the color of the mother liquor changes from dark yellow to light yellow;

[0052] (3) Pressure filtration: transfer the material obtained in step (2) to a pressure filter kettle for pressure filtration, and the light yellow material obtained by pressure filtration enters the collection tank;

[0053] (4) Desolventization: Transfer the material in the collection tank of step (3) to the desolventization kettle, and distill the toluene at 65-75°C under the pressure of -0.08 to -0.095 bar, and the obtained toluene can be directly applied to the step ...

Embodiment 3

[0057] (1) Washing: In a washing kettle, dissolve 400kg of crude 2-chloro-5-chloromethylthiazole in 150kg of toluene, add 900kg of water in batches for washing, the pH value of the organic phase of washing is 6-7, wash with water After completion, separate the lower organic phase;

[0058] (2) Adsorption and color removal: add 30kg of activated carbon to the material obtained in step (1), and stir at 45°C for 3 hours until the color of the mother liquor changes from dark yellow to light yellow;

[0059] (3) Pressure filtration: transfer the material obtained in step (2) to a pressure filter kettle for pressure filtration, and the light yellow material obtained by pressure filtration enters the collection tank;

[0060] (4) Desolventization: Transfer the material in the collection tank of step (3) to the desolventization kettle, and distill the toluene at 65-75°C under the pressure of -0.08 to -0.095 bar, and the obtained toluene can be directly applied to the step ( 1) As a d...

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Abstract

The invention relates to a separating and refining method of 2-chloro-5-chloromethylthiazole. High-purity 2-chloro-5-chloromethylthiazole is prepared through a crystallization method by taking crude 2-chloro-5-chloromethylthiazole as a raw material. The method comprises the following steps: (1) washing with water; (2) performing adsorbing and color-removing; (3) performing pressure filtration; (4) desolventizing; (5) adding an organic solvent; (6) crystallizing with a crystallization device, heating and melting; collecting to obtain high-purity 2-chloro-5-chloromethylthiazole. High-purity 2-chloro-5-chloromethylthiazole is prepared through the crystallization method of the self-made crystallization device according to the characteristics of low melting point of 2-chloro-5-chloromethylthiazole and high melting point of impurities. The separating method is simple, the production purity is high, the quality is stable, the energy consumption is low, the three-waste output is low, and the green chemical industry development requirements are met.

Description

technical field [0001] The invention relates to a method for separating and refining 2-chloro-5-chloromethylthiazole, which belongs to the technical field of fine chemicals. Background technique [0002] 1.1 Properties and uses of 2-chloro-5-chloromethylthiazole [0003] English name: 2-Chloro-5-chloromethylthiazole CAS: 105827-91-6 [0004] Molecular weight: 168; Melting point: 29.5°~30.0°C [0005] Structural formula: [0006] Industrial product content: 98%, light yellow liquid. [0007] 2-Chloro-5-chloromethylthiazole is an important intermediate for the synthesis of the second-generation neonicotinoid insecticides thiamethoxam and clothianidin. [0008] 1.2 Existing technology for preparing 2-chloro-5-chloromethylthiazole and main problems [0009] Currently, there are two main techniques for refining 2-chloro-5-chloromethylthiazole. [0010] Direct distillation method: After the main reaction of synthesizing 2-chloro-5-chloromethylthiazole is completed, the vac...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D277/32
CPCC07D277/32
Inventor 李旭坤左伯军李磊李德军刘伟华石隆平刘钦胜
Owner SHANDONG ACADEMY OF PESTICIDE SCI
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