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Sulfonyl modified strong cationic hypercrosslinked resin and preparation method thereof

A technology of ultra-high cross-linked resin and strong cations, applied in the field of resins, can solve the problems of low specific surface area, low adsorption capacity, and the preparation method of strong cationic ultra-high cross-linked resin has not yet been reported, and achieves narrow particle size distribution. , the effect of good adsorption performance

Inactive Publication Date: 2015-06-10
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Conventional strong cation exchange resins containing sulfonic acid groups are all macroporous or gel-type resins, so their specific surface area is low, their adsorption capacity is not high, and their selective adsorption capacity is limited.
However, the previous patent (application number 200510095298.X, publication number CN1772774A) discloses a synthetic method of super-high cross-linked adsorption resin containing sulfonic acid group composite function, but the synthetic steps of this method are relatively cumbersome and need to be further improved.
Literature search shows that the strong cationic ultra-high cross-linked resin involved in the present invention and its preparation method have not been reported yet

Method used

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  • Sulfonyl modified strong cationic hypercrosslinked resin and preparation method thereof
  • Sulfonyl modified strong cationic hypercrosslinked resin and preparation method thereof
  • Sulfonyl modified strong cationic hypercrosslinked resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] The preparation of the strong cationic super high cross-linked resin modified by sulfonic acid group comprises the following steps:

[0028] (a) In a 1000ml three-necked flask equipped with a reflux condenser, a thermometer and a nitrogen protection device, add 800ml of acetonitrile, and cool the system to 0° C. in an ice bath. Add 0.46g of azobisisobutyronitrile, 4g of divinylbenzene, and 12g of 4-chloromethylstyrene to the ice-water bath system in sequence, maintain the temperature of the system at 0°C, and blow nitrogen gas for 2 hours to remove the oxygen in the system . Then the reaction was transferred to an oil bath, the magnetic stirrer was adjusted to 200r / min, the system was slowly raised from room temperature to 60°C (according to the heating rate of 4min / °C), and the temperature was maintained to continue the reaction for 46 hours. After the reaction, cool the reaction system to room temperature, filter the reaction solution with a 0.2 μm nylon filter membr...

Embodiment 2

[0033] The strong cationic ultra-high cross-linked resin modified by sulfonic acid groups in this example is used as solid phase extraction filler to selectively adsorb basic organic compounds in aqueous solution. The steps are:

[0034](a) Preparation of stock solution: Accurately weigh 10 mg each of hippuric acid, uric acid, hypoxanthine, and xanthine, dissolve them in a small amount of 0.1 mol / L NaOH solution, and dilute to 10 mL with water. Accurately weigh 10 mg of inosine, and dilute to 10 mL with 0.13% acetic acid solution (pH=3).

[0035] (b) Prepare the solution to be tested: accurately pipette 100 μL each of the five stock solutions prepared in step (a), and dilute to 10 mL with 0.13% acetic acid solution (pH=3).

[0036] (c) Packing of solid-phase extraction column: accurately weigh 60 mg of strong cationic ultra-high cross-linked resin resin modified by sulfonic acid group, disperse it with 30 ml of anhydrous methanol, and use wet packing to pack the resin into a s...

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Abstract

The invention relates to a sulfonyl modified strong cationic hypercrosslinked resin and a preparation method thereof. The performance of the resin serving as a solid-phase extraction filler is evaluated. The preparation method comprises the following steps: by taking chloromethyl styrene and divinyl benzene as reaction raw materials and taking azodiisobutyronitrile as an initiator, synthesizing a resin white ball by virtue of a non-aqueous precipitation polymerization reaction; by taking ferric trichloride as a catalyst, synthesizing a hypercrosslinked resin by virtue of a Fourier crosslinking reaction; and finally, sulfonating by using concentrated sulfuric acid, and synthesizing the sulfonyl-containing strong cationic hypercrosslinked resin. The strong cationic hypercrosslinked resin disclosed by the invention belongs to a new generation of porous polymer resins, has the complex functions of strong cationic exchange interaction and non-polar interaction and serves as a solid-phase extraction filler, the performance of the resin is obviously superior to that of a commercial Oasis MCX solid-phase extraction column, and the resin can be used for separation and enrichment of alkali compounds in complex samples and has good application prospects in the fields of biology and environments.

Description

【Technical field】 [0001] The invention relates to the technical field of resins, in particular to a preparation method of a strong cationic ultra-high cross-linked resin modified with sulfonic acid groups. 【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, less consumption of organic solvents and stable results, and has become the mainstream pretreatment method for the analysis of complex systems. . The separation mode of solid-phase extraction mainly depends on the type of packing material in its stationary phase. Most of the existing commercial extractants use macroporous resin polymers as fillers, which have a small specific surface area and low adsorption capacity. The recently emerging ultra-high cross-linked resin extractant has the characteristics of high specific surface a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F212/14C08F212/36C08F8/36C08F8/26B01J20/285B01J20/30B01D15/08
Inventor 章弘扬徐雅婷胡坪张敏王月荣孙威
Owner EAST CHINA UNIV OF SCI & TECH
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