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A method for refining 3,6-dichloropicolinic acid

A technology of clopicolinic acid and dimethyl, which is applied in the field of refining, and can solve the problems of low product purity, many impurities, and increased production costs

Active Publication Date: 2018-01-16
中新科农(山东)生态农业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The 3,6-dichloropicolinic acid purification technology in the prior art is often not high in purity due to the large amount of impurities in the reaction solution, and secondary crystallization is required, which will undoubtedly reduce the product yield and increase production costs

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] step 1.

[0021] Preparation of adsorbent: Add 100Kg Ambermite XAD16HP chelated high-flow rate agarose microspheres, 5Kg 3,7-dimethyl-2,6-octadienal, 0.05Kg 1-vinyl-3-ethylimidazole into a 1000L reactor Tetrafluoroborate, 800Kg water, 2Kg hydroxypropyl methylcellulose, 1Kg benzoyl peroxide, react at 80°C for 6h, then heat up to 85°C for 2h, then heat up to 95°C for 6h, filter and dry After obtaining the adsorbent;

[0022] Step 2. Adsorption and purification of 3,6-dichloropicolinic acid:

[0023] Mix 100Kg of 3,6-dichloropicolinic acid crude product, 10Kg of sodium hydroxide, and 600Kg of water for 3 hours, and at 75°C, pass through a chromatographic column equipped with an adsorbent for adsorption at a flow rate of 3BV / h to obtain purified 3 , 6-dichloropicolinic acid sodium salt, then add hydrochloric acid to neutralize to PH = 7, and then obtain the purified product of 3,6-dichloropicolinic acid through known desalting and dehydration techniques. The mass percent...

Embodiment 2

[0025] Step 1. Preparation of adsorbent:

[0026] Add 100Kg Ambermite XAD16HP chelated high-flow agarose microspheres, 1Kg 3,7-dimethyl-2,6-octadienal, 0.01Kg 1-vinyl-3-ethylimidazole tetrafluoroborate into a 1000L reactor , 500Kg water, 1Kg hydroxypropyl methylcellulose, 0.5Kg benzoyl peroxide, react at 80°C for 6h, then heat up to 85°C for 2h, then heat up to 95°C for 6h, filter, and dry to obtain the adsorbent ;

[0027] Step 2. Adsorption and purification of 3,6-dichloropicolinic acid:

[0028] Mix 100Kg of crude 3,6-dichloropicolinic acid, 5Kg of sodium hydroxide, and 300Kg of water for 1 hour, and conduct adsorption through a chromatographic column equipped with an adsorbent at 50°C at a flow rate of 1BV / h to obtain purified 3 , 6-dichloropicolinic acid sodium salt, then add hydrochloric acid to neutralize to PH = 7, and then go through known desalination and dehydration techniques to obtain the purified product of 3,6-dichloropicolinic acid. The mass percentage conte...

Embodiment 3

[0030] Step 1. Preparation of adsorbent:

[0031] Add 100Kg Ambermite XAD1180 chelating high-flow agarose microspheres, 10Kg 3,7-dimethyl-2,6-octadienal, 0.1Kg 1-vinyl-3-ethylimidazole tetrafluoroborate into a 1000L reaction kettle , 1000Kg water, 4Kg hydroxypropyl methylcellulose, 2Kg benzoyl peroxide, react at 80°C for 6h, then heat up to 85°C for 2h, then heat up to 95°C for 6h, filter, and dry to obtain the adsorbent;

[0032] Step 2. Adsorption and purification of 3,6-dichloropicolinic acid:

[0033] Mix 100Kg of crude 3,6-dichloropicolinic acid, 20Kg of sodium hydroxide, and 1000Kg of water for 5 hours, and at 100°C, pass through a chromatographic column equipped with an adsorbent for adsorption at a flow rate of 5BV / h to obtain purified 3 , 6-dichloropicolinic acid sodium salt, then add hydrochloric acid to neutralize to PH = 7, and then go through known desalination and dehydration techniques to obtain the purified product of 3,6-dichloropicolinic acid. The mass perc...

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PUM

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Abstract

The invention relates to a method for refining 3, 6-clopyralid. The method includes preparing adsorbents; mixing 3, 6-clopyralid crude products with water to obtain mixtures and adsorbing the mixtures by the aid of the adsorbents to obtain purified 3, 6-clopyralid products.

Description

Technical field [0001] The present invention relates to a refining method, in particular to a refining method of 3,6-dichloropicolinic acid. Background technique [0002] The current post-processing method for the clopyralic acid solution obtained by the electrochemical reduction method is to add acid to the solution to crystallize the clopyralic acid, and then separate and extract the clopyralic acid and sodium chloride salt through filtration and vacuum evaporation. The disadvantages of vacuum evaporation are high energy consumption and high operating costs. Therefore, people need to explore a new separation technology that is both efficient, economical and environmentally friendly. After a long period of exploration, diffusion dialysis membrane separation technology has become the focus of researchers. [0003] CN102351788A relates to a method for extracting and purifying clopyralic acid, which uses membrane concentration and separation technology to concentrate the clop...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D213/79C07D213/803B01J20/30B01J20/26
CPCB01J20/22B01J20/24B01J20/265C07D213/79C07D213/803
Inventor 王琪宇
Owner 中新科农(山东)生态农业有限公司