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Preparation method for organic-inorganic hybrid porous monolith material based on epoxide ring-opening reaction

An epoxy ring-opening and monolithic material technology is applied in the field of preparation of organic-inorganic hybrid porous monolithic materials based on epoxy ring-opening reaction, which can solve problems such as uneven internal microstructure

Inactive Publication Date: 2014-06-25
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

[0006] In order to further simplify the preparation steps of hybrid monolithic materials and effectively improve the inhomogeneity of its internal microstructure, the present invention has developed a new "one-step method" method for preparing organic-inorganic hybrid porous monolithic materials

Method used

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  • Preparation method for organic-inorganic hybrid porous monolith material based on epoxide ring-opening reaction
  • Preparation method for organic-inorganic hybrid porous monolith material based on epoxide ring-opening reaction
  • Preparation method for organic-inorganic hybrid porous monolith material based on epoxide ring-opening reaction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] 1. Add 50 mg of POSS-epoxy reagent to the centrifuge tube.

[0031] 2. Add 15 mg of HDA to the above centrifuge tube.

[0032] 3. Add 30 mg of porogen PEG10,000 into the centrifuge tube.

[0033] 4. Add 280 μL of n-propanol and 40 μL of 1,4-butanediol into the above centrifuge tube, and ultrasonicate the above centrifuge tube for 15 minutes to mix the components evenly and remove the dissolved oxygen dissolved therein.

[0034] 5. Introduce the pre-polymerization solution obtained in step 4 into a 75 μm (inner diameter) capillary tube that has been aminated in advance with a syringe, and then seal both ends of the capillary with silica gel, and then seal the centrifuge tube containing the remaining pre-polymerization solution Membrane seal.

[0035] 6. Place the capillary and centrifuge tube in step 5 in a water bath at 50°C for 10 hours of reaction. At this time, the prepolymerized liquid in the centrifuge tube has formed a white solid.

[0036] 7. Rinse the capilla...

Embodiment 2

[0040] 1. Add 50 mg of POSS-epoxy reagent to the centrifuge tube.

[0041] 2. Add 40 μL of PEI to the above centrifuge tube.

[0042] 3. Add 25mg of porogen PEG10,000 into the centrifuge tube.

[0043] 4. Add 280 μL of n-propanol and 40 μL of 1,4-butanediol to the above centrifuge tube, and ultrasonicate the above centrifuge tube for 10 minutes to mix the components evenly and remove the dissolved oxygen dissolved therein.

[0044] 5. Introduce the pre-polymerization solution obtained in step 4 into a capillary tube of 75 μm (inner diameter) that has been aminated in advance with a syringe, and then seal both ends of the capillary with silica gel, and then put the centrifuge tube containing the remaining pre-polymerization solution with Parafilm seals.

[0045] 6. Place the capillary and centrifuge tube in step 5 in a water bath at 50° C., and react for 12 hours. At this time, the prepolymerization solution in the centrifuge tube has formed a white solid.

[0046] 7. Rinse ...

preparation Embodiment 3

[0048] 1. Add 50 mg of POSS-epoxy reagent to the centrifuge tube.

[0049] 2. Add 15 mg of DAO to the above centrifuge tube.

[0050] 3. Add 35 mg of porogen PEG10,000 into the centrifuge tube.

[0051] 4. Add 280 μL of n-propanol and 40 μL of 1,4-butanediol to the above centrifuge tube, and ultrasonicate the above centrifuge tube for 20 minutes to mix the components evenly and remove the dissolved oxygen dissolved therein.

[0052] 5. Introduce the pre-polymerization solution obtained in step 4 into a capillary tube of 75 μm (inner diameter) that has been aminated in advance with a syringe, and then seal both ends of the capillary with silica gel, and then put the centrifuge tube containing the remaining pre-polymerization solution with Parafilm seals.

[0053] 6. Place the capillary and centrifuge tube in step 5 in a water bath at 50°C for 8 hours of reaction, at which time the prepolymerization solution in the centrifuge tube has formed a white solid.

[0054] 7. Rinse t...

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Abstract

The invention relates to a preparation method for an organic-inorganic hybrid porous monolith material based on epoxide ring-opening reaction. Specifically, the porous organic-inorganic hybrid monolith material is prepared in one step by mixing polyhedral oligomeric silsesquioxanes (POSS), an organic cross-linking agent (an epoxide ring-opening agent), an organic solvent and a pore-forming agent and dissolving under assistance of ultrasound, and then carrying out ring-opening polymerization at a certain temperature. The preparation method has the advantages of simple and rapid operation, and mild conditions. Besides, different organic cross-linking agents (epoxide ring-opening agents) can be selectively used and a pore-forming system can be adjusted according to different application requirements, so that a series of different organic-inorganic hybrid monolith materials can be prepared.

Description

technical field [0001] The invention relates to the preparation of an organic-inorganic hybrid porous monolithic material based on epoxy ring-opening reaction, specifically, polyhedral oligomeric silsesquisilane reagent (POSS), organic diamine or polyamine crosslinking agent and porogenic solvent And after the porogen is mixed uniformly by ultrasound, the organic-inorganic hybrid porous monolithic material with specific organic functional groups is prepared in one step by using epoxy ring-opening polymerization reaction. Background technique [0002] Porous monolithic materials have the characteristics of easy preparation, strong modifiability, and good permeability, and are attracting more and more attention, and have been widely used in the field of chromatographic separation and analysis. According to different chemical properties, porous monolithic materials can be divided into two categories, namely organic monolithic materials and inorganic monolithic materials. The f...

Claims

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Application Information

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IPC IPC(8): C08G59/50C08G59/32C08J9/28
Inventor 邹汉法林辉其他发明人请求不公开姓名
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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