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A kind of anion exchange type macroporous crystal colloid medium and preparation method thereof

A crystal gel medium and exchange-type technology, applied in chemical instruments and methods, other chemical processes, etc., can solve the problems of insoluble water and preparation methods that cannot be used directly, and achieve the effects of low cost, easy large-scale production, and simple process

Active Publication Date: 2011-12-21
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Compared with DEAEMA, dimethylaminoethyl methacrylate is structurally only aminomethyl converted to aminoethyl, but it is almost insoluble in water, and the preparation method reported in existing literature cannot be used directly.

Method used

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  • A kind of anion exchange type macroporous crystal colloid medium and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Dissolve 1.5g of DMAAm monomer, 0.3g of crosslinking agent N,N'-diacryloylethylenediamine and 0.5g of AGE and 0.15g of ethylene glycol diglycidyl ether mixture ligand material in 30ml of deionized water, and stir well Then, quickly add 20mg TEMED and 53mg APS, put the resulting mixture into a chromatographic column with an inner diameter of 26mm and a length of 200mm. Then keep the temperature for 20 hours to cool and crystallize to cause pores. The temperature was raised to room temperature to obtain a super-large-pore continuous bed crystal gel medium matrix with a volume of about 33 mL.

[0027] 70ml 0.1M diethylaminoethyl methacrylate monomer solution (solvent is DMSO: H 2 O=2:1, volume ratio) in 70ml 0.02M Zn 2+ 、Cu 2+ Aqueous solution (each 0.01M) (complex ion SO 4 2- ) under the catalysis of 60° C. to carry out graft polymerization on the aforementioned crystal gel medium matrix for 6 hours to obtain anion-exchange crystal gel medium immobilized with amino f...

Embodiment 2

[0029] Dissolve 1.0g of AAm monomer, 0.05g of cross-linking agent MBAAm and 0.08g of AGE in 10mL of deionized water, stir well, then quickly add 7mg of TEMED and 15mg of APS, and put the resulting mixture into a glass layer with an inner diameter of 16mm and a length of 200mm In the analysis column, after sealing, the cooling crystallization-induced porosis polymerization is carried out in a programmable temperature-controlled constant temperature cooling system. The temperature change process is: (A) cooling: from 0 °C to -30 °C; (B) heating: heating to -5 °C; (C) constant temperature: constant temperature for 5 hours; (D) cooling: cooling from -5 °C again to -20°C; (E) constant temperature: constant temperature for 16 hours; (F) temperature rise: heat up to room temperature to obtain a super-large-pore continuous bed crystal gel medium matrix with a volume of about 12 mL.

[0030] 30ml 0.1M diethylaminoethyl methacrylate monomer solution (solvent is DMSO: H 2 O=5:1, volume ...

Embodiment 3

[0032]Dissolve 0.5g of DMAEMA monomer, 0.1g of crosslinking agent MBAAm and 0.15g of ligand material ethylene glycol diglycidyl ether in 20ml of deionized water. After stirring evenly, quickly add 18mg of TEMED and 25mg of APS, and put the resulting mixture into In a glass chromatography column with an inner diameter of 16mm and a length of 200mm, after sealing, the temperature is lowered to -25°C in a programmable temperature-controlled constant temperature cooling system to perform cooling and crystallization to form pores. Then, it was melted to obtain a super-large-pore continuous bed gel matrix with a volume of about 22 mL.

[0033] 25ml 0.1M diethylaminoethyl methacrylate aqueous solution, 25ml 0.1M HCl reacted and stirred for 30min, and then mixed with the aforementioned crystal gel medium matrix in 50ml 4M Ni 2+ 、Cu 2+ (molar ratio 1:5) aqueous solution (complex ion NO 3 - ) under the catalysis of 40 DEG C for 3 hours of graft polymerization reaction, to obtain an a...

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Abstract

The invention provides an anion-exchange macroporous crystal gel medium, which is obtained by immobilizing groups represented by formula (1) or (2) on the inner surface of the pores of the crystal gel medium matrix; the anion-exchange macroporous crystal gel The pore diameter of the medium is 5-300 μm, and the porosity is 50-98%. The pores of the crystal gel medium contain amide groups, and its physical form is a monolithic column. The anion-exchange macroporous crystal gel medium has a small theoretical plate height, and when the flow rate is 0.1-10 cm / min, the plate height of the crystal gel bed column is less than 0.2 cm. The beneficial effects of the present invention are mainly reflected in: 1) the monomer material is easy to obtain, the process is simple, the cost is low, and the large-scale production is easy; 2) the ultra-large pore size is uniform, the connectivity is good, the mass transfer resistance is small, and it can be used in the range of high flow rate Operation; 3) It can directly separate the target substance from complex feed-liquid systems such as fermentation broth, culture fluid, and lysate containing microbial cells and cell debris at high flow rates, with easy elution and convenient regeneration.

Description

(1) Technical field [0001] The invention relates to an anion exchange macroporous crystal gel medium and a preparation method thereof. (2) Background technology [0002] The ultra-large pore crystal gel medium (cryogel) is a chromatographic medium obtained through the method of crystallization and pore formation, and the solvent freeze crystallization and the polymerization reaction of the column material are carried out simultaneously. During the preparation process, the phase change of the solvent (such as water) crystallizes, and at the same time, the exclusivity of crystal growth makes the monomer and crosslinking agent enriched around the crystal and polymerized to form a bed skeleton. After the crystals are melted, super-large pores with tens to hundreds of microns are formed, through which microbial cells, cell fragments and other solid phases in the raw material solution can pass directly, and several steps such as centrifugation, filtration, concentration and chroma...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/26B01J20/30
Inventor 高云玲沈绍传贠军贤姚克俭
Owner ZHEJIANG UNIV OF TECH
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