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Organic-inorganic hybrid porous monolithic material, preparation and applications thereof

An integral material and hybrid technology, applied in chemical instruments and methods, other chemical processes, etc., can solve the problems of difficult reaction control and complex preparation process, and achieve high column efficiency, good biocompatibility, and strong versatility.

Active Publication Date: 2020-04-17
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the sol-gel method has good versatility, its preparation process is relatively complicated
Radical polymerization is relatively simple and easy to operate, but the reaction is difficult to control due to the very fast chain growth rate

Method used

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  • Organic-inorganic hybrid porous monolithic material, preparation and applications thereof
  • Organic-inorganic hybrid porous monolithic material, preparation and applications thereof
  • Organic-inorganic hybrid porous monolithic material, preparation and applications thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 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 (37%) dropwise to the solution, and reflux in an oil bath at 90°C for 24h ; After the reaction is completed, cool the reaction solution in an ice bath (-4 ~ 4 ° C) to obtain a crude product, wash the crude product with methanol five times to remove residual mercaptopropyltrimethoxysilane; then, dissolve it in dichloromethane The resulting crude product was extracted by adding water to the solution, collecting the dichloromethane layer, and then adding water to extract, repeating three times, finally collecting dichloromethane, adding anhydrous sodium sulfate to it and drying overnight (12h); finally, the obtained The solution was distilled under reduced pressure to obtain the product POSS-SH.

[0024] 1) Add POSS-SH 63.6mg into an empty centrifuge tube as a functional monomer;

[0025] 2) A...

Embodiment 2

[0043] 1) Add POSS-SH 51.0mg into an empty centrifuge tube as a functional monomer;

[0044] 2) Add 90 μL of diethylene glycol diethyl ether to the centrifuge tube in step 1) as a porogen;

[0045] 3) Add 149 μL of n-propanol to the centrifuge tube in step 2) as a porogen;

[0046] 4) Add 19.4 μL of 1,2,4-triethylcyclohexane as a functional monomer to the centrifuge tube in step 3);

[0047] 5) Add 35.3 μL of isophytol to the centrifuge tube in step 4) as a functional monomer;

[0048] 6) Add 0.2 mg of 2,2-dimethoxy-phenylacetophenone to the centrifuge tube of step 5) as a photoinitiator;

[0049] 7) Ultrasonicate the centrifuge tube in step 6) at room temperature for 3 minutes to completely dissolve it to form a uniform transparent solution;

[0050] 8) Introduce 1 μL of the prepolymer solution obtained in step 7) into a 75 μm (inner diameter) capillary tube that has been previously activated by 3-(methacryloxy)propyltrimethoxysilane with a syringe, and then Seal with sil...

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Abstract

The invention relates to rapid preparation of an organic-inorganic hybrid porous monolithic material on the basis of a thiol-ene click polymerization reaction. The preparation method specifically comprises the following steps: uniformly mixing a polyhedral oligomeric silsesquioxane reagent (POSS) (functional monomer) containing a multi-sulfydryl functional group, an organic compound (functional monomer) containing three double-bonds, an organic compound (functional monomer) containing one double-bond, a photoinitiator, a pore-foaming agent and the like; and carrying out a thiol-ene click polymerization reaction at a certain temperature to prepare the organic-inorganic hybrid porous monolithic material with special function. The preparation method has the advantages of mild conditions, rapidness, controllability and the like. The prepared hybrid monolithic material can be applied to chromatographic separation so as to realize efficient separation and analysis of small molecular compounds and complex biological samples.

Description

technical field [0001] The invention relates to a rapid preparation of organic-inorganic hybrid porous monolithic material based on Thiol-ene click polymerization. Specifically, the multimercapto-containing functional group compound (functional monomer), the organic compound (functional monomer) containing three double bonds, the organic compound (functional monomer) containing one double bond, photoinitiator and porogen etc. are mixed and stir evenly, and then mercapto-methacrylate click polymerization occurs at a certain temperature to prepare an organic-inorganic hybrid porous monolithic material with special functions. Background technique [0002] Capillary liquid chromatography (cLC) is one of the most important techniques in microanalysis and plays an important role in the field of separation science. Compared with traditional liquid chromatography, capillary liquid chromatography not only improves the effectiveness of the chromatographic column and the selectivity o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F283/12C08F230/08C08J9/14B01J20/285
CPCB01J20/285C08F283/122C08J9/142
Inventor 欧俊杰王妍马淑娟叶明亮
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI