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Preparation method of organic-inorganic hybrid porous integral material

A monolithic material and hybridization technology, which is applied in the field of preparation of organic-inorganic hybrid porous monolithic materials, can solve problems such as not showing the potential of high-efficiency separation and analysis

Inactive Publication Date: 2016-05-11
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

Although the research group also used the thermal initiation process to prepare capillary monolithic column materials, this material did not show the potential for high-efficiency separation and analysis

Method used

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  • Preparation method of organic-inorganic hybrid porous integral material
  • Preparation method of organic-inorganic hybrid porous integral material
  • Preparation method of organic-inorganic hybrid porous integral material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 1. Add 25.0mg of TMTVS reagent to the UV transparent glass bottle.

[0028] 2. Add 21.3 mg of 2SH to the above-mentioned UV transparent glass bottle.

[0029] 3. Add 80 μL of diethylene glycol diethyl ether and 100 μL of n-propanol into the above-mentioned ultraviolet transparent glass bottle.

[0030] 4. Add 0.1 mg of photoinitiator DMPA to the above-mentioned ultraviolet transparent glass bottle, and ultrasonicate the above-mentioned ultraviolet transparent glass bottle for 1 min to mix the components therein evenly, and remove the dissolved oxygen dissolved therein.

[0031]5. Use a syringe to introduce the mixed solution obtained in step 4 into a 75 μm (inner diameter) UV transparent capillary tube that has been pre-activated with vinyltrimethoxysilane, then seal both ends of the capillary tube with silica gel, and then put the remaining mixing liquid in a UV transparent glass bottle with airtight seal.

[0032] 6. Place the UV transparent capillary and UV transpa...

Embodiment 2

[0035] 1. Add 15.5 mg of TVS reagent to the UV transparent glass bottle.

[0036] 2. Add 26.8 mg of 2SH to the above-mentioned UV transparent glass bottle.

[0037] 3. Add 170 μL of diethylene glycol diethyl ether and 10 μL of n-propanol into the above-mentioned ultraviolet transparent glass bottle.

[0038] 4. Add 0.1 mg of photoinitiator DMPA to the above-mentioned ultraviolet transparent glass bottle, and ultrasonicate the above-mentioned ultraviolet transparent glass bottle for 1 min to mix the components therein evenly, and remove the dissolved oxygen dissolved therein.

[0039] 5. Use a syringe to introduce the mixed solution obtained in step 4 into a 75 μm (inner diameter) UV transparent capillary tube that has been pre-activated with vinyltrimethoxysilane, then seal both ends of the capillary tube with silica gel, and then put the remaining mixing liquid in a UV transparent glass bottle with airtight seal.

[0040] 6. Place the UV transparent capillary and UV transpa...

Embodiment 3

[0043] 1. Add 32.4mg of TMTVS reagent to the UV transparent glass bottle.

[0044] 2. Add 35.0 mg of 4SH to the above-mentioned UV transparent glass bottle.

[0045] 3. Add 100 μL of diethylene glycol diethyl ether and 140 μL of n-propanol into the above-mentioned ultraviolet transparent glass bottle.

[0046] 4. Add 0.1 mg of photoinitiator DMPA to the above-mentioned ultraviolet transparent glass bottle, and ultrasonicate the above-mentioned ultraviolet transparent glass bottle for 1 min to mix the components therein evenly, and remove the dissolved oxygen dissolved therein.

[0047] 5. Use a syringe to introduce the mixed solution obtained in step 4 into a 75 μm (inner diameter) UV transparent capillary tube that has been pre-activated with vinyltrimethoxysilane, then seal both ends of the capillary tube with silica gel, and then put the remaining mixing liquid in a UV transparent glass bottle with airtight seal.

[0048] 6. Place the UV transparent capillary and UV trans...

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Abstract

The invention relates to a method for rapid preparation of an organic-inorganic hybrid porous integral material based on photoinduced thiol-ene polymerization reaction. Specifically, the method includes: mixing a tetravinyl compound (functional monomer), a multi-mercapto compound (functional monomer), a pore-forming agent and a photoinitiator and conducting ultrasonic dissolution, then carrying out photoinduced thiol-ene polymerization reaction under the irradiation of an ultraviolet lamp with certain wavelength, thus obtaining the porous organic-inorganic hybrid integral material by one step. The preparation method has the advantages of mild conditions, high efficiency and controllability, etc., also can select different functional monomers according to different application requirements, or adjust the pore-foaming agent system to prepare a series of organic-inorganic hybrid integral materials with different physical and chemical properties.

Description

technical field [0001] The invention relates to a rapid preparation of organic-inorganic hybrid porous monolithic materials based on photoinitiated mercapto-alkenyl polymerization, specifically mixing tetravinyl compounds, polymercapto compounds, porogenic solvents and photoinitiators uniformly and ultrasonically, and then using Photoinduced thiol-enepolymerization reaction (photoinducedthiol-enepolymerization reaction) prepares organic-inorganic hybrid porous monolithic materials with specific organic functional groups in one step. Background technique [0002] Monolithic materials with continuous porous structures have received increasing attention and have been widely used in fields such as catalysis, adsorption, separation media, and storage supports. In the field of separation and analysis, the capillary monolithic column is a monolithic material (mainly including organic monolithic materials, inorganic silica gel monolithic materials and organic-inorganic hybrid monoli...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J9/26C08G75/04
Inventor 邹汉法刘忠山欧俊杰
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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