Preparation method of 3,6-dichloropicolinic acid osmotic membrane for concentrating

A technology of dichloropicolinic acid and permeable membrane is applied in the field of preparation of concentrated 3,6-dichloropicolinic acid permeable membrane, which can solve the problem that impurities cannot be removed and can achieve the effect of improving permeability

Active Publication Date: 2016-08-03
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

[0005] The 3,6-dichloropicolinic acid concentration technology in the prior art can only be concentrated to about 97% (wt%), and there are still about 2% of impurities that cannot be removed.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] In a 2000L reactor, wash the surface of 100Kg homogeneous anion exchange membrane with 8Kg methanol, dry, and immerse the dry film in 1500Kg4-styrylpyridine, 0.3Kg1-allyl-3-methylimidazole hexafluorophosphate , 3Kg vinyl terephthalic acid mixed solution, N 2 protection, with 60Co gamma ray irradiation dose of about 30kGy, irradiation time of 40 minutes, take out the grafted membrane, wash the surface of the membrane with 1500Kg tetrahydrofuran, and dry to obtain a permeable membrane that can be used for concentration of 3,6-dichloropicolinic acid . Product number B-1.

Embodiment 2

[0016] In a 2000L reactor, wash the surface of 100Kg homogeneous anion exchange membrane with 5Kg methanol, dry, and immerse the dry film in 1000Kg4-styrylpyridine, 0.1Kg1-allyl-3-methylimidazole hexafluorophosphate , in 1Kg vinyl terephthalic acid mixed solution, N 2 protection, with 60Co γ-ray irradiation dose of about 10kGy, irradiation time of 10 minutes, take out the grafted membrane, wash the surface of the membrane with 1000Kg tetrahydrofuran, and dry to obtain a permeable membrane that can be used for concentration of 3,6-dichloropicolinic acid . Product number B-2.

Embodiment 3

[0018] In a 3000L reactor, wash the surface of 100Kg homogeneous anion exchange membrane with 10Kg methanol, dry, and immerse the dry film in 2000Kg4-styrylpyridine, 0.5Kg1-allyl-3-methylimidazole hexafluorophosphate ,5Kg vinyl terephthalic acid mixed solution, N 2 Protection, with 60Co γ-ray irradiation dose of about 50kGy, irradiation time of 60 minutes, take out the grafted membrane, wash the surface of the membrane with 2000Kg tetrahydrofuran, and dry it to obtain a permeable membrane that can be used for the concentration of 3,6-dichloropicolinic acid . Product number B-3.

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Abstract

The invention relates to a preparation method of a 3,6-dichloropicolinic acid osmotic membrane for concentrating .A homogeneous anion exchange membrane is immersed into a mixed solution of 4-styrylpyridine, 1-allyl-3-methylimidazolium hexafluorophosphate and vinyl terephthalic acid, irradiation grafting modification is conducted, and the 3,6-dichloropicolinic acid osmotic membrane is obtained.

Description

technical field [0001] The invention relates to a method for preparing a membrane, in particular to a method for preparing a permeable membrane for concentrating 3,6-dichloropicolinic acid. Background technique [0002] The current post-treatment method for the clopyralid solution obtained by the electrochemical reduction method is to add acid to the solution to precipitate clopyralid crystallization, and then separate and extract clopyralid and sodium chloride salts by filtration and vacuum evaporation. 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 refining clopyralid, which uses membrane concentration and separation technol...

Claims

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Application Information

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IPC IPC(8): B01D71/78B01D67/00C07D213/803C07D213/79
CPCB01D67/0006B01D71/78C07D213/79C07D213/803
Inventor 王琪宇
Owner 中新科农(山东)生态农业有限公司
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