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Hybrid porous monolithic material, and preparation method and application thereof

A monolithic material and hybridization technology, applied in chemical instruments and methods, and other chemical processes, can solve problems such as poor stability, easy swelling, and poor mechanical strength of organic monolithic columns

Active Publication Date: 2019-12-17
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, organic monolithic columns have poor mechanical strength, poor stability, and are prone to swelling in some organic solvents.

Method used

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  • Hybrid porous monolithic material, and preparation method and application thereof
  • Hybrid porous monolithic material, and preparation method and application thereof
  • Hybrid porous monolithic material, and preparation method and application thereof

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Embodiment 1

[0024] Preparation of POSS-SH functional monomer: First, take 15mL of mercaptopropyltrimethoxysilane (MPTS) and dissolve it in 360mL of methanol, add 30mL of concentrated hydrochloric acid (36% to 38%) dropwise to the solution, and in an oil bath at 90°C Reflux reaction for 24 hours; after the reaction is completed, cool the reaction solution in an ice bath (-4°C-4°C) to obtain a crude product, wash the crude product with methanol three times to remove residual mercaptopropyltrimethoxysilane; then, use di Dissolve the obtained crude product in methyl chloride, add water to the solution for extraction, collect the dichloromethane layer, then add water for extraction, repeat three times, finally collect dichloromethane, add anhydrous sodium sulfate to it and dry overnight; finally, the obtained The solution was distilled under reduced pressure to obtain the product POSS-SH. The obtained POSS-SH was dissolved in tetrahydrofuran solution (50.0%, w / v, mg / ml) for use.

[0025] The ...

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Abstract

The invention relates to a preparation method of a polyacrylate hybrid monolithic material containing a polyhedral oligomeric silsesquioxane (POSS) reagent. The preparation method comprises the following steps: mixing the polyhedral oligomeric silsesquioxane reagent containing a thiol group with other two acrylate monomers, adding a pore-foaming solvent, and performing ultrasonic dissolution; andinitiating an in-situ acrylate self-polymerization reaction and a thiol-acrylate click chemical reaction with ultraviolet light to obtain the hybrid monolithic material. The preparation method of themonolithic material has the advantages of simple and rapid preparation process and mild reaction conditions, and the monolithic material has a uniform pore structure and a good thermal stability, andcan be applied to high performance chromatographic separation analysis of small molecular compounds and complex biological samples.

Description

technical field [0001] The present invention relates to a rapid preparation of organic-inorganic hybrid porous monolithic material based on photoinitiated mercapto free radical-mediated polymerization and its preparation method and application. Polyhedral oligomeric silsesquioxane of mercapto groups, acrylate compounds and photoinitiators were ultrasonically dissolved in a porogenic solvent, and photoinduced acrylate self-polymerization and mercapto-acrylate click chemical reaction (photoinduced thiol-eneclick polymerization reaction) were used. ) in situ formation of organic-inorganic hybrid porous monoliths. By adjusting the concentration of monomers, the amount of mercapto groups added and the ratio of porogens, a porous hybrid monolithic material with excellent chromatographic performance can be prepared finally, specifically a hybrid porous monolithic material and its preparation and application. Background technique [0002] In recent years, miniaturization has become...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/282C08F220/18C08F222/20C08F2/48C08F8/42
CPCB01J20/282B01J2220/58C08F2/48C08F8/42C08F220/18C08F222/1006
Inventor 欧俊杰王妍马淑娟叶明亮
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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