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Phenylboronic acid-modified covalent affinity hypercrosslinked resin, and preparation method and application thereof

A technology of ultra-high cross-linked resin and phenylboronic acid, which is applied in the field of resin to achieve the effects of good adsorption performance, simple preparation steps, and avoidance of the activation process

Inactive Publication Date: 2015-07-22
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Literature search shows that this novel covalent affinity super-crosslinked resin modified by phenylboronic acid and its preparation method have not been reported.

Method used

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  • Phenylboronic acid-modified covalent affinity hypercrosslinked resin, and preparation method and application thereof
  • Phenylboronic acid-modified covalent affinity hypercrosslinked resin, and preparation method and application thereof
  • Phenylboronic acid-modified covalent affinity hypercrosslinked resin, and preparation method and application thereof

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Experimental program
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Effect test

Embodiment 1

[0034] The preparation of the covalent affinity ultra-high cross-linked resin modified by phenylboronic acid comprises the following steps:

[0035] (a) In a 500ml three-neck flask equipped with a reflux condenser, a thermometer and a nitrogen protection device, add 400ml of acetonitrile, and cool the system to 0°C in an ice bath;

[0036] (b) Add 0.25g of azobisisobutyronitrile, 2.98ml of divinylbenzene, 3.81ml of 4-chloromethylstyrene and 1.2g of 4-vinylbenzeneboronic acid to the ice-water bath system, in which 4-ethylene Phenylboronic acid needs to be dissolved in 40ml of absolute ethanol and then added to the reaction system. The temperature of the system is maintained at 0°C, and the nitrogen gas is blown for 2 hours to remove the oxygen in the system;

[0037] (c) Then transfer the reaction to an oil bath, adjust the magnetic stirrer to an appropriate rotation speed, and slowly raise the system from room temperature to 70°C (according to a heating rate of 4min / °C), and m...

Embodiment 2

[0047] The covalent affinity ultra-high cross-linked resin of this example is used as a solid phase extraction filler to separate catechol (cis-diol type) and hydroquinone (non-cis-diol type) isomers, the steps for:

[0048] (a) Preparation of solvent: Accurately weigh 0.1750 g of disodium hydrogen phosphate, and set the volume to 500 ml to obtain pH=8.5 phosphate buffer A. Accurately pipette 0.5ml of trifluoroacetic acid and 15ml of acetonitrile, and dilute to 50ml with ultrapure water to obtain solution B containing 1% trifluoroacetic acid in acetonitrile:water=30:70. Accurately pipette 10 ml of acetonitrile, and dilute to 100 ml with ultrapure water to obtain acetonitrile solution C of acetonitrile:water=10:90.

[0049] (b) Prepare the solution to be tested: Accurately weigh 0.2000 g of catechol and hydroquinone, and use the solutions prepared in step (a) to make up to 50 ml respectively.

[0050] (c) Packing of solid-phase extraction column: Accurately weigh 60 mg of cov...

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Abstract

The invention relates to a phenylboronic acid-modified covalent affinity hypercrosslinked resin and a preparation method thereof. The performance of the phenylboronic acid-modified covalent affinity hypercrosslinked resin used as a solid phase extraction filler is evaluated. The preparation method comprises the following steps: carrying out a non-aqueous precipitation polymerization reaction on vinylbenzyl chloride, divinyl benzene and 4-vinylphenylboronic acid as reaction raw materials with azodiisobutyronitrile as an initiator and iron trichloride as a catalyst to synthesize phenylboronic acid-containing resin white balls, and carrying out a Friedel-Crafts crosslinking reaction to synthesize the covalent affinity hypercrosslinked resin. The covalent affinity hypercrosslinked resin is a new generation porous polymer resin, has an ultrahigh specific surface area (800m<2> / g) and particle size of 3-5[mu]m, has covalent affinity action force and non-polar action force compounding functions, and can be used in the separation enrichment of cis-diol compounds in complex samples as a solid phase extraction filler.

Description

【Technical field】 [0001] The invention relates to the technical field of resins, in particular to a covalent affinity super-crosslinked resin modified with phenylboronic acid and its preparation method and application. 【Background technique】 [0002] In the sample pretreatment technology, solid phase extraction technology has gradually replaced the traditional liquid-liquid extraction method due to its advantages of simplicity, high efficiency, easy automation and low consumption of organic solvents, and has become the mainstream pretreatment method for complex system analysis. . The separation mode of SPE depends mainly on the type of packing in the stationary phase. In conventional types of polymer fillers, due to the use of macroporous resin materials, their specific surface area is small (<500m2 / g), and their adsorption capacity is not high; The selectivity of special group compounds is not enough, and the selectivity must be improved by chemical modification. Ther...

Claims

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Application Information

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IPC IPC(8): C08F212/14C08F212/36C08F230/06C08J3/24B01J20/26B01J20/30
Inventor 胡坪章弘扬吴世坤仰贤莉王月荣张敏
Owner EAST CHINA UNIV OF SCI & TECH
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