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Pyridine/bipyridine conjugated micro-porous polymer, preparation method and application thereof

A technology of conjugated micropores and bipyridyl, which is applied in separation methods, chemical instruments and methods, educts, etc., can solve the problems of uncertainty in pyridine nitrogen content, harsh synthesis conditions, and the need for heavy metal catalysis, etc., and achieve the goal of increasing CO2 The effect of adsorption capacity and CO2/N2 selectivity, increasing nitrogen content, and good application value

Active Publication Date: 2019-09-10
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The technical problem to be solved by the present invention is to provide a class of pyridine / bipyridine conjugated microporous polymers and its preparation method and application, which overcomes the harsh synthesis conditions of existing conjugated microporous polymers, the need for heavy metal catalysis, and the introduction of pyridine Nitrogen content is uncertain, CO 2 / N 2 Defects such as poor selectivity

Method used

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  • Pyridine/bipyridine conjugated micro-porous polymer, preparation method and application thereof
  • Pyridine/bipyridine conjugated micro-porous polymer, preparation method and application thereof
  • Pyridine/bipyridine conjugated micro-porous polymer, preparation method and application thereof

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Embodiment 1

[0040] Mix 2,2'-bipyridine-5,5'-dicarbaldehyde (212.2mg, 1mmol) and 1,4-diacetylbenzene (324.4mg, 2mmol) in a 100ml round bottom flask, add ammonium acetate ( 2.31g, 30mmol), then 50ml of pyridine was added, and the mixture was placed in an oil bath at 115°C and stirred for 12h. After the reaction, filter with suction, wash with deionized water and chloroform at 60°C for 24 hours, and then dry in a vacuum oven at 100°C for 24 hours to obtain the pyridine / bipyridine conjugated microporous polymer, which is denoted as polymer Matter-1, its BET specific surface area is 347m 2 / g.

[0041] The polymer-1 that present embodiment obtains 13 C-NMR test results such as figure 1 As shown, it can be seen that the peaks at 153.8 and 146.1ppm chemical shifts are respectively the peaks of ortho and para C in the pyridyl chemical environment, proving the existence of pyridine nitrogen; the peaks at 134.6, 126.1 and 120.3ppm chemical shifts It is the peak of C in the chemical environment...

Embodiment 2

[0048] Mix 2,2'-bipyridine-5,5'-dicarbaldehyde (212.2mg, 1mmol) and 1,3-diacetylbenzene (324.4mg, 2mmol) in a 100ml round bottom flask, add ammonium acetate ( 2.31g, 30mmol), then add 25ml of acetic acid to dissolve the above mixed powder, and finally place the mixed solution in an oil bath at 115°C and stir for 12h. After the reaction, filter with suction, wash with deionized water and chloroform at 60°C for 24 hours, and then dry in a vacuum oven at 100°C for 24 hours to obtain the pyridine / bipyridine conjugated microporous polymer, which is denoted as polymer Matter-2, its BET specific surface area is 418m 2 / g.

[0049] The polymer-2 that present embodiment obtains 13 C-NMR test results such as Figure 7 As shown, it can be seen that the peaks at 155.6 and 148.5ppm chemical shifts are respectively the peaks of ortho and para C in the pyridyl chemical environment, proving the existence of pyridine nitrogen; the peaks at 135.6, 126.5 and 119.3ppm chemical shifts It is th...

Embodiment 3

[0056] Mix 2,2'-bipyridine-5,5'-dicarbaldehyde (212.2mg, 1mmol) and 2,6-diacetylpyridine (326.3mg, 2mmol) in a 100ml round bottom flask, add ammonium acetate ( 2.31g, 30mmol), then 50ml of pyridine was added, and finally the mixture was placed in an oil bath at 120°C and stirred for 12h. After the reaction, filter with suction, wash with deionized water and chloroform respectively at 60°C for 24 hours, and dry in a vacuum oven at 60°C for 24 hours after suction filtration to obtain the pyridine / bipyridine conjugated microporous polymer, which is denoted as polymer Matter-3, its BET specific surface area is 400m 2 / g.

[0057] The polymer-3 that present embodiment obtains 13 C-NMR test results such as Figure 13 As shown, it can be seen that the peaks at 154.5 and 148.2ppm chemical shifts are respectively the peaks of ortho and para C in the pyridyl chemical environment, proving the existence of pyridine nitrogen; the peaks at 135.3 and 120.0ppm chemical shifts are at The p...

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Abstract

The invention relates to a pyridine / bipyridine conjugated micro-porous polymer, a preparation method and application thereof. The polymer is prepared by using 2,2'-bipyridyl-5,5'-diformaldehyde, an aromatic ketone compound and ammonium acetate as raw materials and using a solvothermal synthesis method. The conjugated micro-porous polymer has certain specific surface area and pores, exhibits good adsorption performance and CO2 / N2 selectivity as a CO2 adsorbing agent, has good reversible adsorption-desorption properties, and has good application prospect.

Description

technical field [0001] The invention belongs to the technical field of microporous polymers, in particular to a class of pyridine / bipyridine conjugated microporous polymers and a preparation method and application thereof. Background technique [0002] The greenhouse effect and global warming are a major environmental problem faced by human beings all over the world. Therefore, scientists are committed to developing carbon dioxide adsorption and separation systems to achieve the purpose of capturing carbon dioxide in the atmosphere. Conjugated microporous polymers are a type of amorphous porous organic polymers that connect structural units with π-conjugated structures. They have the characteristics of high specific surface area, hierarchical pores, various synthesis methods, and structural design. Separation has a good application prospect. [0003] However, existing CO 2 The collector shows a certain adsorption effect only under high pressure, but the selectivity is poo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G61/12B01D53/02B01J20/26B01J20/30
CPCC08G61/122B01D53/02B01J20/262B01D2257/504C08G2261/124C08G2261/18C08G2261/3221Y02C20/40Y02P20/151
Inventor 廖耀祖何颜程中桦
Owner DONGHUA UNIV
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