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Preparation of hybrid integral materials containing polyhedral oligomeric silsesquioxane reagent

A monolithic material, sesquisilane technology, applied in other chemical processes, chemical instruments and methods, etc., can solve the problems affecting separation ability and column efficiency, functional group difficulties, multi-time and labor, etc.

Inactive Publication Date: 2014-10-22
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

The former has good pH stability, but it is easy to swell in organic solvents, resulting in changes in pore structure, affecting separation ability and column efficiency; the latter has the advantages of good mechanical stability and strong tolerance to organic solvents, but also has pH stability. In addition, its preparation process is relatively cumbersome, and it is difficult to introduce functional groups, which requires more time and manpower, which also affects the preparation repeatability.

Method used

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  • Preparation of hybrid integral materials containing polyhedral oligomeric silsesquioxane reagent
  • Preparation of hybrid integral materials containing polyhedral oligomeric silsesquioxane reagent
  • Preparation of hybrid integral materials containing polyhedral oligomeric silsesquioxane reagent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] 1. Wash the quartz capillary (75 or 100 μm i.d.×375 μm o.d.) with 0.1M NaOH solution for 2 hours.

[0033] 2. Rinse the capillary with deionized water for 30 minutes; then rinse with 0.1M HCl solution for 12 hours, and then rinse with deionized water until the effluent is neutral.

[0034] 3. Mix 50% (v / v) γ-methacryloxypropyltrimethoxysilane (γ-MAPS) / methanol solution and ultrasonically fill the capillary, seal both ends and incubate in a constant temperature water bath at 45°C 16h.

[0035] 4. Finally, rinse the capillary with methanol, dry it with nitrogen, and seal it with silicone rubber for later use.

Embodiment 2

[0037] 1. Add 300mg of POSS-MA to the centrifuge tube.

[0038] 2. Add 3 mg of AIBN to the above centrifuge tube.

[0039] 3. Add 800 μL of n-propanol and 400 μL of PEG (molecular weight 400) to the above centrifuge tube.

[0040] 4. Ultrasonicate the centrifuge tube for 30 minutes to mix the components in it evenly.

[0041] 5. Introduce the pre-polymerization solution obtained in step 4 into the quartz capillary prepared in Example 1 with a syringe, and then seal both ends of the capillary with silica gel.

[0042] 6. Place the capillary in step 5 in a water bath at 55°C and react for 10 hours.

[0043] 7. Rinse the capillary with methanol to wash out the porogen and some unreacted substances to obtain a capillary hybrid monolithic column.

[0044] figure 1 It is the scanning electron micrograph of the capillary hybrid monolithic column (before chemical modification) containing POSS. figure 2 It is the capillary liquid chromatography separation diagram of benzene series ...

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Abstract

The invention relates to the polymer field, and particularly relates to a preparation method for organic-inorganic hybrid porous integral materials based on free radical polymerization. The method comprises the steps: firstly, carrying out ultrasonic dissolving of a polyhedral oligomeric silsesquioxane reagent containing a plurality of double-bonds and an initiator in a pore forming agent, carrying out a free radical polymerization reaction at a certain temperature, in-situ forming a porous hybrid integral material, then introducing a solution containing the initiator and organic functional monomers into the integral material, at a certain temperature, carrying out chemical bonding of the organic functional monomers on the surface of the integral material, and finally preparing the hybrid integral materials with different surface properties and functions. The preparation method has the advantages of simple and rapid operation, mild reaction conditions and the like; and in addition, different organic functional monomers can also be selected according to different application requirements, the pore forming system is not required to be adjusted, and various organic inorganic hybrid integral materials can be prepared.

Description

technical field [0001] The invention relates to a method for preparing organic-inorganic hybrid porous monolithic materials based on free radical reaction. Specifically, after dissolving polyhedral oligomeric silsesquisilane reagent (POSS) containing multiple double bonds in a certain porogen, using Organic-inorganic hybrid porous monoliths can be prepared in one step by free radical polymerization, and the surface can be chemically modified to meet different application requirements. Background technique [0002] Monolithic material is a new type of stationary phase developed in recent years. It is known as the fourth-generation chromatographic separation medium. It has the characteristics of simple preparation, strong modifiability and good permeability. It is one of the research hotspots in the field of chromatography. It is receiving more and more attention in the fields of life science, drug analysis and environmental monitoring. According to different chemical propert...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F275/00C08F130/08C08F8/34C08J9/26B01J20/285B01J20/30
Inventor 邹汉法欧俊杰林辉
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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