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Preparation method of hybrid porous monolith based on mercapto-epoxy click polymerization

A technology of click polymerization and monolithic materials, which is applied in the field of preparation of hybrid porous monolithic materials based on mercapto-epoxy click polymerization, which can solve the problems of cumbersome preparation process, poor mechanical properties, and uneven internal microstructure, etc. The effect of structural uniformity

Active Publication Date: 2019-05-07
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

The three kinds of monolithic materials have their own advantages and disadvantages. Among them, the organic monolithic materials have the advantages of good pH stability and convenient adjustment of pore properties, but their mechanical properties are poor and they are easy to swell in organic solvents; while the inorganic monolithic materials have good mechanical properties. Organic solvent tolerance is also strong, but it also has disadvantages such as poor pH stability, cumbersome preparation process, and poor preparation repeatability.
However, in the synthesis of porous monolithic materials, the application of mercapto-epoxy click chemistry is still relatively small, especially in the preparation of hybrid porous monolithic materials, there are no related patents or literature reports.
[0006] In order to further simplify the preparation process of hybrid monolithic materials and effectively improve the inhomogeneity of its internal microstructure, the present invention has developed a method based on thiol-epoxy click polymerization reaction to prepare organic-inorganic A New Approach to Hybrid Porous Monoliths

Method used

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  • Preparation method of hybrid porous monolith based on mercapto-epoxy click polymerization
  • Preparation method of hybrid porous monolith based on mercapto-epoxy click polymerization
  • Preparation method of hybrid porous monolith based on mercapto-epoxy click polymerization

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] 1. Add 50 mg of POSS-epoxy reagent to the centrifuge tube.

[0033] 2. Add 26 mg of PTM to the above centrifuge tube.

[0034] 3. Add 280 μL of ethanol to the reaction vessel.

[0035] 4. Add 15 mg of porogen PEG 10,000 to the reaction vessel.

[0036] 5. Add 5 μL of 0.25mol / L KOH aqueous solution into the reaction vessel;

[0037] 6. Ultrasound the above mixed system for 10 minutes in an ice-water bath to completely dissolve it to form a uniform transparent solution, and remove the dissolved oxygen;

[0038] 7. Introduce the prepolymerized solution obtained in step 6 into a capillary tube of 75 μm (inner diameter) that has been pre-sulfhydrylized with a syringe, then seal both ends of the capillary with silica gel, and then seal the centrifuge tube containing the remaining prepolymerized solution Membrane seal.

[0039] 8. Put the capillary and centrifuge tube in step 7 in a water bath at 75°C and react for 1 hour. At this time, the prepolymerization solution in th...

Embodiment 2

[0043] 1. Add 50 mg of POSS-epoxy reagent to the centrifuge tube.

[0044] 2. Add 27 mg of TPTM to the above centrifuge tube.

[0045] 3. Add 260 μL of ethanol to the reaction vessel.

[0046] 4. Add 15 mg of porogen PEG 10,000 to the reaction vessel.

[0047] 5. Add 5 μL of 0.25mol / L KOH aqueous solution into the reaction vessel;

[0048] 6. Ultrasonicate the above mixed system for 5 minutes in an ice-water bath to completely dissolve it to form a uniform transparent solution, and remove the dissolved oxygen in it;

[0049] 7. Introduce the prepolymerized solution obtained in step 6 into a capillary tube of 75 μm (inner diameter) that has been pre-sulfhydrylized with a syringe, then seal both ends of the capillary with silica gel, and then seal the centrifuge tube containing the remaining prepolymerized solution Membrane seal.

[0050] 8. Put the capillary and centrifuge tube in step 7 in a water bath at 55°C and react for 1 hour. At this time, the prepolymerization solut...

Embodiment 3

[0054] 1. Add 50 mg of POSS-epoxy reagent to the centrifuge tube.

[0055] 2. Add 15 mg of HDT to the above centrifuge tube.

[0056] 3. Add 160 μL of ethanol and 40 μL of 1,4-butanediol to the reaction vessel.

[0057] 4. Add 20 mg of porogen PEG 10,000 to the reaction vessel.

[0058] 5. Add 5 μL of 0.25mol / L KOH aqueous solution into the reaction vessel;

[0059] 6. Ultrasound the above mixed system for 10 minutes in an ice-water bath to completely dissolve it to form a uniform transparent solution, and remove the dissolved oxygen;

[0060] 7. Introduce the prepolymerized solution obtained in step 6 into a capillary tube of 75 μm (inner diameter) that has been pre-sulfhydrylized with a syringe, then seal both ends of the capillary with silica gel, and then seal the centrifuge tube containing the remaining prepolymerized solution Membrane seal.

[0061] 8. Put the capillary and centrifuge tube in step 7 in a water bath at 50°C, and react for 1 hour. At this time, the pre...

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Abstract

The invention relates to the preparation of a hybrid porous monolithic material based on mercapto-epoxy click polymerization. Specifically, polyhedral oligomeric silsesquioxanes (POSS), polymercapto crosslinking agent, porogenic solvent, porogen and catalyst containing polyepoxy functional groups are mixed and ultrasonically dissolved, and then dissolved at a certain temperature After the thiol-epoxy click polymerization reaction (thiol-epoxy click polymerization reaction) occurs, the organic-inorganic hybrid porous monolithic material can be prepared in one step. The preparation method has the advantages of simple and fast operation, mild conditions, and strong versatility. In addition, different polymercapto organic crosslinking agents can be selected according to different application requirements and the combination of polyepoxy monomer and polymercapto crosslinking agent can be changed. By adjusting the ratio of those or adjusting the porogenic system, a series of different organic-inorganic hybrid monolithic materials can be prepared.

Description

technical field [0001] The invention relates to the preparation of an organic-inorganic hybrid porous monolithic material based on mercapto-epoxy click polymerization reaction, specifically, polyhedral oligomeric silsesquisilane reagent (POSS) containing polyepoxide functional groups, organic dimercapto or poly After the thiol cross-linking agent, porogenic solvent, porogen and catalyst are mixed uniformly by ultrasound, the organic-inorganic hybrid porous monolith with specific organic functional groups is prepared in one step by thiol-epoxy click polymerization reaction. Material. 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 three categories, namely organ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08J9/26C08G75/04
Inventor 邹汉法林辉欧俊杰
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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