A polymer brush grafted boric acid affinity separation material and its preparation method and application

A separation material, the technology of acrylamide phenylboronic acid, which is 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 long service life

Inactive Publication Date: 2017-06-16
NORTHWEST UNIV
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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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  • A polymer brush grafted boric acid affinity separation material and its preparation method and application
  • A polymer brush grafted boric acid affinity separation material and its preparation method and application
  • A polymer brush grafted boric acid affinity separation material and its preparation method and application

Examples

Experimental program
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Effect test

Embodiment 1

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

[0030] Dissolve 5 g (30 mmol) of 3-aminophenylboronic acid in 75 mL of 2 mol / L sodium hydroxide at 0 °C, then slowly add 6 mL of cold acryloyl chloride dropwise (over 30 min) to the in the mixed solution. Then slowly add 1mol / L HCl dropwise to make the solution pH=1. A white solid precipitated, filtered, and washed with cold water several times. Saturated sodium chloride was added to the filtrate, 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, wash the product with cold water, and dry it in vacuum 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) of n-dodecyl mercaptan, 38 g (0.65 mol) of acetone, and 1.3 g of methyl trioctyl ammonium chloride into a 500 mL three...

Embodiment 2

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

[0034] Disperse 2 g of surface-aminated polymer microspheres in 20 mL 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, and washed with ethanol and acetone for multiple times, respectively, to obtain polymer microspheres modified by RAFT reagent and ammonified on the surface.

[0035] Add 2 g of RAFT reagent-modified polymer microspheres, 30 mL of redistilled N,N-dimethylformamide, 4 g (20 mmol) of m-acrylamidophenylboronic acid, 0.032 g (0.2 mmol) of azo Diisobutyronitrile, using freezing-thawing-vacuum degassing for more than three times, reacted in a 70 °C oil bath for 24 h under the protection of nitrogen, and quenched the schlenk tube in an ice bath to termina...

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-aminated silica gel in 20 mL 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 under stirring at room temperature for 48 hours, filtered, and washed with ethanol and acetone several times respectively to obtain RAFT reagent-modified surface-aminated silica gel.

[0038] Add 2 g RAFT reagent-bonded silica gel, 20 mL redistilled isopropanol, 2 g (10 mmol) m-acrylamidophenylboronic acid, 0.008 g (0.005 mmol) azobisisobutyronitrile to a schlenk tube, and freeze- Thawing-vacuumize and degas more than three times, react in an oil bath at 60 °C for 12 h under nitrogen protection, quench the schlenk tube in an ice bath to terminate the reaction, precipitate with ice methanol, filter, and use N,N-dimethy...

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Abstract

The invention discloses a polymer brush grafted boric acid affinity separation material and a preparation method thereof. The present invention adopts the reversible addition-fragmentation chain transfer (RAFT) polymerization method, uses amide compounds containing phenylboronic acid groups as monomers, and polymerizes them on the surfaces of polyacrylic acid, silica gel, agarose and magnetic nanoparticles to obtain a polymer brush. Grafted boronic acid affinity separation materials. The separation material of the present invention has the characteristics of high adsorption capacity, good selectivity and fast mass transfer rate. It can be used for the separation, preparation and content analysis of cis-diol-containing biomolecules, and can greatly improve the separation and 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 field of separation technology and functional material preparation. Background technique [0002] Molecules containing cis-o-diols have important physiological functions in living organisms. Some cis-o-diol molecules, such as sugars, glycoproteins, RNA, nucleosides, catecholamines, etc., are markers in the diagnosis process of many diseases, because these cis-o-diol substances are very low in biological samples and have a large amount In the presence of interfering substances, efficient separation and enrichment is the key to accurate analysis of cis-diols. In addition, some cis-o-diol molecules, such as certain flavonoids, anthraquinones and polyphenols, are the main medicinal ingredients in traditional Chinese medicine, vegetables, and fruits. Efficient separation of such substances i...

Claims

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Application Information

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