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Modification method and application of microporous polymer with high nitrogen content

A microporous polymer, high nitrogen content technology, applied in the field of microporous polymer modification, can solve the problem that the specific surface area of ​​the microporous polymer cannot meet the expected requirements, achieve good application value and improve the effect of specific surface area

Active Publication Date: 2018-09-07
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the specific surface area of ​​such microporous polymers cannot meet the expected requirements.

Method used

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  • Modification method and application of microporous polymer with high nitrogen content
  • Modification method and application of microporous polymer with high nitrogen content
  • Modification method and application of microporous polymer with high nitrogen content

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Place tetrakis(4-bromophenyl)methane and p-phenylenediamine in the Schlenk tube in proportion to two monomers, add reaction auxiliary bis(dibenzylideneacetone)palladium, 2-dicyclohexylphosphine-2′ , 4′,6′-triisopropylbiphenyl, sodium tert-butoxide, injected toluene in a nitrogen atmosphere, and reacted in an oil bath at 110°C for 24h. After the reaction, purify with deionized water, chloroform and methanol for 12 hours, and finally place it in a vacuum oven at 60°C for 24 hours to obtain Polymer-1 with a BET specific surface area of ​​94m 2 / g. Mix and grind Polymer-1 and potassium carbonate into a three-necked flask, inject 30mL N, N-dimethylformamide, microwave for 60 minutes, inject diiodomethane in a nitrogen atmosphere, and react in an oil bath at 152°C 3 days. After the reaction, wash with deionized water for 12 h, and then wash with chloroform for 24 h in a Soxhlet extractor to remove unreacted raw materials. Finally, dry in a vacuum oven at 60°C for 24 hours,...

Embodiment 2

[0043]Place tetrakis(4-bromophenyl)methane and m-phenylenediamine in the Schlenk tube in proportion, and add bis(dibenzylideneacetone)palladium, 2-dicyclohexylphosphine-2' , 4',6'-triisopropylbiphenyl, sodium tert-butoxide, injected toluene in a nitrogen atmosphere, and reacted in an oil bath at 110°C for 24h. After the reaction, purify with deionized water, chloroform and methanol for 12 hours, and finally place it in a vacuum oven at 60°C for 24 hours to obtain Polymer-2 with a BET specific surface area of ​​47m 2 / g. Mix and grind Polymer-2 and potassium carbonate into a three-necked flask, inject 30mL N,N-dimethylformamide, microwave for 60 minutes, inject diiodomethane in a nitrogen atmosphere, and react in an oil bath at 152°C 3 days. After the reaction, wash with deionized water for 12 h, and then wash with chloroform for 24 h in a Soxhlet extractor to remove unreacted raw materials. Finally, dry in a vacuum oven at 60°C for 24 hours, then wash and dry to obtain a mo...

Embodiment 3

[0049] Place tetrakis(4-bromophenyl)methane and o-phenylenediamine in a Schlenk tube in proportion to two monomers, and add reaction assistant bis(dibenzylideneacetone)palladium, 2-dicyclohexylphosphine-2' , 4',6'-triisopropylbiphenyl, sodium tert-butoxide, injected toluene in a nitrogen atmosphere, and reacted in an oil bath at 110°C for 24h. After the reaction, purify with deionized water, chloroform and methanol for 12 hours, and finally place it in a vacuum oven at 60°C for 24 hours to obtain Polymer-3 with a BET specific surface area of ​​81m 2 / g. Put polymer-3 and potassium carbonate into a three-necked flask after mixing and grinding, inject 30mL N,N-dimethylformamide, microwave for 60 minutes, inject diiodomethane in a nitrogen atmosphere, and react in an oil bath at 152°C 3 days. After the reaction, wash with deionized water for 12 h, and then wash with chloroform for 24 h in a Soxhlet extractor to remove unreacted raw materials. Finally, dry in a vacuum oven at 6...

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Abstract

The invention discloses a modification method of a microporous polymer with a high nitrogen content, and application of the microporous polymer with the high nitrogen content in gas absorption and catalyst carrier or energy storage. The modification method comprises the following steps: mixing the microporous polymer with the high nitrogen content and potassium carbonate, grinding the mixture, andthen placing the ground mixture in a container; injecting N, N-dimethylformamide, and carrying out microwave oscillation; injecting diiodomethane in a nitrogen atmosphere for carrying out a reaction;washing the reactant, and drying. The modification method provided by the invention adopts a super-crosslinking reaction, the microporous polymer with the high nitrogen content and diiodomethane react in presence of a alkali, so that -NH- imine bonds and C-I bonds are enabled to react with each other, hydrogen iodide is removed, and C-N bonds are generated; the C-N bonds also endow the polymer with excellent redox property; the two C-I bonds in the diiodomethane are similar to a crosslinked scaffold, and can both expand the accumulated chain segments in the polymer and enable the interior ofthe polymer to be subjected to a cross-linking reaction, so that the specific surface area of the polymer is enlarged. The microporous polymer with the high nitrogen content has a better application value in the fields such as gas adsorption, catalyst carrier storage and energy storage.

Description

technical field [0001] The invention relates to a modification method and application of a microporous polymer with high nitrogen content, and belongs to the technical field of microporous polymer modification. Background technique [0002] Conjugated microporous polymers are composed of light elements such as carbon, hydrogen, oxygen, nitrogen, and boron, and contain a large number of micropores with a pore size less than 2nm. They have high surface area, three-dimensional conjugated skeleton, good stability, and adjustable channel structure. Modification and other characteristics have shown great application value in many fields, such as gas adsorption / separation, sensors, heterogeneous catalysis, light energy capture and transfer, electrochemistry, etc. Conjugated microporous polymers are a research hotspot in recent years. [0003] Microporous polymers with high nitrogen content are a typical representative of microporous polymers. In addition to the characteristics of...

Claims

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Application Information

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IPC IPC(8): C08G73/02C08J9/28C08L79/02
CPCC08G73/02C08J9/28C08J2379/02
Inventor 廖耀祖胡孝文王海鸽程中桦
Owner DONGHUA UNIV
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