Polymer brush graft boracic acid affinity separation material and preparation method and application

A separation material and acid affinity technology, applied in the field of separation technology and functional material preparation, can solve the problems of slow mass transfer rate and low adsorption capacity, and achieve the effect of fast mass transfer rate, high adsorption capacity and good selectivity

Inactive Publication Date: 2015-08-26
NORTHWEST UNIV(CN)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a novel boric acid affinity separation material grafted with a polymer brush with high adsorption capacity and fast mass transfer rate, so as to overcome the shortcomings of existing boric acid affinity separation materials such as low adsorption capacity and slow mass transfer rate.

Method used

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  • Polymer brush graft boracic acid affinity separation material and preparation method and application
  • Polymer brush graft boracic acid affinity separation material and preparation method and application
  • Polymer brush graft boracic acid affinity separation material and preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] (1) Synthesis of m-acrylamidobenzeneboronic acid monomer

[0030] Dissolve 5 g (30 mmol) of 3-aminophenylboronic acid into 75 mL of 2 mol / L sodium hydroxide at 0 °C, and then slowly add 6 mL of cold acryloyl chloride dropwise (over 30 min) to the mixture with stirring in an ice bath. in the mixed solution. Then 1 mol / L HCl was slowly added dropwise to make the solution pH=1. A white solid was precipitated, which was filtered and washed with cold water several times. To the filtrate was added saturated sodium chloride and extracted three times with 60 mL of ethyl acetate. The combined organic phases were rotary evaporated and combined with the above white precipitate. Recrystallize in hot water at 60 °C, rinse the product with cold water, and vacuum dry at 30 °C to obtain needle-like crystals, which are m-acrylamide phenylboronic acid.

[0031] (2) Synthesis of RAFT reagent DDACT

[0032] Add 16 g (79 mmol) n-dodecyl mercaptan, 38 g (0.65 mol) acetone, and 1.3 g met...

Embodiment 2

[0033] Example 2: Preparation of polymer brush-grafted boric acid affinity separation material with surface ammoniated polymer microspheres as matrix

[0034] Disperse 2 g of surface ammoniated polymer microspheres in 20 mL of redistilled tetrahydrofuran, add 4 g (10 mmol) DDATC, then add 1.2 g (6 mmol) DCC (dicyclohexylcarbodiimide), 1.2 g NHS ( 10 mmol) (N-hydroxysuccinimide), reacted under stirring at room temperature for 48 hours, filtered, washed with ethanol and acetone for several times, to obtain polymer microspheres with RAFT reagent modified surface amination.

[0035] To a schlenk tube, add 2 g of RAFT reagent-modified polymer microspheres, 30 mL of redistilled N,N-dimethylformamide, 4 g (20 mmol) of m-acrylamide phenylboronic acid, 0.032 g (0.2 mmol) of azo Diisobutyronitrile was degassed by freeze-thaw-evacuation for more than three times, and the reaction was carried out in an oil bath at 70 °C for 24 h under nitrogen protection. After the reaction, the schlenk t...

Embodiment 3

[0036] Example 3: Preparation of polymer brush-grafted boric acid affinity separation material based on surface ammoniated silica gel

[0037] Disperse 2 g of surface ammoniated silica gel in 20 mL of redistilled tetrahydrofuran, add 4 g (10 mmol) of DDATC, then add 1.2 g of DCC (6 mmol) (dicyclohexylcarbodiimide), 1.2 g of NHS (10 mmol) ( N-hydroxysuccinimide), reacted for 48 hours under stirring at room temperature, filtered and washed with ethanol and acetone for several times to obtain silica gel with RAFT reagent modified surface amination.

[0038] To a schlenk tube add 2 g of RAFT reagent-bonded silica gel, 20 mL of redistilled isopropanol, 2 g (10 mmol) of m-acrylamide phenylboronic acid, 0.008 g (0.005 mmol) of azobisisobutyronitrile, using cryo- Thawing-vacuum degassing for more than three times, react in an oil bath at 60 °C for 12 h under nitrogen protection, after the reaction, quench the schlenk tube in an ice bath to terminate the reaction, precipitate with ice me...

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Abstract

The invention discloses a polymer brush graft boracic acid affinity separation material and a preparation method and application, which use a reversible-addition fragmentation chain transfer (RAFT) polymerization method, use amide compounds with phenylboronic acid groups as monomers, wherein the amide compounds are polymerized on the surfaces of polyacrylic acids, silica gels, agarose and magnetic nanoparticles to obtain the polymer brush graft boracic acid affinity separation material. The polymer brush graft boracic acid affinity separation material has the advantages of high adsorption capacity, excellent selectivity and rapid mass transfer rate, can be used for preparation, separation and content analysis of biomolecules containing cis vicinal diols, and can greatly improve separation enrichment efficiency.

Description

technical field [0001] The invention relates to a novel separation material and a preparation method thereof, in particular to a boric acid affinity separation material, which belongs to the fields of separation technology and functional material preparation. Background technique [0002] Molecules containing cis-vicinal diols have important physiological roles in living organisms. Some cis-diol molecules, such as sugars, glycoproteins, RNA, nucleosides, catecholamines, etc., are markers in the diagnosis of many diseases, because the content of these cis-diol substances in biological samples is very low, and there are a large number of them. The existence of interfering substances, efficient separation and enrichment is the key to accurate analysis of cis-diols. In addition, some cis-adjacent diol molecules, such as certain flavonoids, anthraquinones and polyphenols are the main medicinal components in traditional Chinese medicines, vegetables and fruits, and the efficient ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F293/00B01J20/281B01J20/30B01D15/38
Inventor 许欢欢王超展卫引茂
Owner NORTHWEST UNIV(CN)
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