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Preparation method and use of organic-inorganic hydrophilic hybrid integral material

An integral material, hydrophilic technology, applied in other chemical processes, chemical instruments and methods, etc., can solve the problems of insufficient preparation repeatability, easy to be affected by pH, etc., and achieve the function modification method is simple, versatile, chromatographic Good separation ability

Active Publication Date: 2017-12-15
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the preparation of silicon-based inorganic-organic hybrid monolithic materials still needs to go through multiple steps, and is easily affected by pH. The lack of repeatability in the preparation limits its development. Therefore, a faster and more efficient hybrid monolithic material preparation method has been developed. is necessary

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0022] The preparation steps are as follows:

[0023] 1) Add 300mg octavinylsilsesquioxane to the UV transparent centrifuge tube;

[0024] 2) Add 107.9 mg of 1-thioglycerol to the UV transparent centrifuge tube in step 1);

[0025] 3) Add 10mL tetrahydrofuran to the UV transparent centrifuge tube in step 1);

[0026] 4) Add 20 μL of photoinitiator 2,2-dimethoxy-phenylacetophenone (2,2-dimethoxy-2-phenylacetophenone, DMPA) to the UV transparent centrifuge tube in step 1);

[0027] 5) Ultrasonicate the mixed system obtained after step 4) at normal temperature to completely dissolve it to form a uniform transparent solution to remove dissolved oxygen in the mixed system;

[0028] 6) sealing the mixed solution obtained in step 5) in an ultraviolet transparent glass bottle;

[0029] 7) Place the ultraviolet transparent glass bottle sealed with the mixed solution in step 6) under an ultraviolet lamp to react for 20 minutes;

[0030] 8) The product obtained in step 7) the ultravi...

Embodiment 2

[0039] Embodiment 2 preparation steps are as follows:

[0040] 1) Add 300mg octavinylsilsesquioxane to the UV transparent centrifuge tube;

[0041] 2) Add 161.8 mg of 1-thioglycerol to the UV transparent centrifuge tube in step 1);

[0042] 3) Add 10mL tetrahydrofuran to the UV transparent centrifuge tube in step 1);

[0043]4) Add 20 μL of photoinitiator 2,2-dimethoxy-phenylacetophenone (2,2-dimethoxy-2-phenylacetophenone, DMPA) to the UV transparent centrifuge tube in step 1);

[0044] 5) Ultrasonicate the mixed system obtained after step 4) at normal temperature to completely dissolve it to form a uniform transparent solution to remove dissolved oxygen in the mixed system;

[0045] 6) sealing the mixed solution obtained in step 5) in an ultraviolet transparent glass bottle;

[0046] 7) Place the ultraviolet transparent glass bottle sealed with the mixed solution in step 6) under an ultraviolet lamp to react for 20 minutes;

[0047] 8) The product obtained in step 7) the...

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Abstract

The invention relates to a method for preparing a hydrophilic hybrid integral material through a thiol-ene click chemical reaction. The method comprises mixing a modified polyhedral oligomeric silsesquioxane reagent, a sulfhydryl compound, an initiator and a pore-foaming agent, carrying out ultrasonic dissolution and preparing the organic-inorganic hydrophilic hybrid integral material through a thiol-ene click chemical reaction in situ under UV irradiation. The porous hybrid integral material has a uniform and regular microstructure and ordered pores and can be well used in chromatographic separation. The preparation method has the advantages of simple and quick operation, fast reaction speed and the like, and can also select different functional monomers and pore-foaming agent systems according to different application requirements to prepare a series of porous hybrid integral materials with different physical and chemical properties.

Description

technical field [0001] The present invention relates to a rapid preparation of hydrophilic organic-inorganic hybrid porous monolithic material based on photoinitiated mercapto-ene click chemical reaction and its preparation method and application, in particular, octavinyl modified by 1-thioglycerol Silsesquisilane, mercapto compound and photoinitiator are ultrasonically dissolved in a porogenic solvent, and a hydrophilic organic-inorganic hybrid porous monolith is formed in situ by photoinduced thiol-ene click polymerization reaction . By adjusting the concentration of monomers and the ratio of porogens, porous hybrid monolithic materials with different surface properties and functions can be prepared. Background technique [0002] Since the appearance of monolithic columns in the 1990s, monolithic materials as a new type of porous micro-separation media have received extensive attention in the field of analytical separation. Compared with traditional packed columns, capil...

Claims

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Application Information

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IPC IPC(8): C08G77/392C08J9/28B01J20/285B01J20/30
CPCB01J20/285B01J2220/86C08G77/045C08G77/392C08J9/28C08J2383/08
Inventor 欧俊杰白径遥叶明亮
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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