Preparation method and application of porous polymer containing iron and boron

A porous polymer, iron source technology, applied in electrodes, electrolysis processes, electrolysis components, etc., can solve problems such as instability and achieve the effect of enriching the pore structure

Active Publication Date: 2022-01-28
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

On the other hand, boronic acid-containing porous polymers are usually unstable due to their easy hydrolysis, thus, the synthesis of stable boronic acid-containing porous polymers is a challenge.

Method used

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  • Preparation method and application of porous polymer containing iron and boron
  • Preparation method and application of porous polymer containing iron and boron
  • Preparation method and application of porous polymer containing iron and boron

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] The preparation method of the porous polymer containing iron and boron in this embodiment is as follows:

[0036] (1) 0.3 mmol of boron-containing tetrahedral building block tetrakis (4-boronic acid phenyl), 1.2 mmol of ferrous chloride and 1.8 mmol of 2,6-diformyl-4-methylphenol di Oxime (synthetic schematic diagram see Figure 6 ) into 50mL of methanol solvent, stirring and dispersing evenly.

[0037] (2) Stir and disperse evenly and put it into a round bottom flask.

[0038] (3) The round-bottomed flask was refluxed and stirred at 65° C. for 48 hours, cooled to room temperature after the reaction, and the solid was collected by suction filtration.

[0039] (4) The collected solid was centrifuged and washed 10 mL×5 times with DMF and THF successively, and the solid was collected again.

[0040] (5) After Soxhlet extraction of the solid with THF for 24 hours, vacuum drying at 90° C. for 8 hours to obtain a black solid, which is the porous polymer containing iron and...

Embodiment 2

[0047] The preparation method of the porous polymer containing iron and boron in this embodiment is as follows:

[0048] (1) 0.3mmol of benzene-1,3,5-triyltriboric acid, 0.45mmol of ferrous chloride and 1.35mmol of glyoxime (see figure 1 ) into 55mL of methanol solvent, stirring and dispersing evenly.

[0049] (2) Stir and disperse evenly and put it into a round bottom flask.

[0050] (3) The round-bottomed flask was refluxed and stirred at 60° C. for 42 hours, cooled to room temperature after the reaction, and the solid was collected by suction filtration.

[0051] (4) The collected solid was centrifuged and washed 10 mL×5 times with DMF and THF successively, and the solid was collected again.

[0052] (5) After Soxhlet extraction of the solid THF for 24 hours, vacuum drying at 90° C. for 8 hours to obtain a black solid, which is the porous polymer containing iron and boron, marked as FeB-POP-1.

[0053] The same method as in Example 1 was used to carry out the electrocataly...

Embodiment 3

[0055] The preparation method of the porous polymer containing iron and boron in this embodiment is as follows:

[0056] (1) 0.3mmol of benzene-1,3,5-triyltriboric acid, 0.45mmol of ferrous chloride and 1.35mmol of dimethylglyoxaloxime (synthetic schematic diagram see figure 1 ) into 50mL of methanol solvent, stirring and dispersing evenly.

[0057] (2) Stir and disperse evenly and put it into a round bottom flask.

[0058] (3) The round-bottomed flask was refluxed and stirred at 60° C. for 40 hours at a constant temperature. After the reaction was completed, it was cooled to room temperature and the solid was collected by suction filtration.

[0059] (4) The collected solid was centrifuged and washed 20 mL×6 times with DMF and THF successively, and the solid was collected again.

[0060] (5) After Soxhlet extraction of solid THF for 24 hours, vacuum drying at 85° C. for 24 hours to obtain a black powder, which is the porous polymer containing iron and boron, marked as FeB-P...

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Abstract

The invention discloses a preparation method of a porous polymer containing iron and boron, which is characterized in that ferrous ions provided by different iron sources, a series of different organic boric acid derivatives and a series of different oximido derivatives are used as raw materials, methanol is used as a solvent, reflux reaction is carried out for several hours, the porous polymer is obtained through one-step coordination and boric acid esterification dehydration polymerization, a crude product is sequentially washed through DMF and THF, THF Soxhlet extraction is conducted for 24 hours, vacuum drying is conducted, and then the dark porous polymer is obtained and has good thermal stability and chemical stability. The metal center in a mononuclear or binuclear iron oxime unit facing different pore structures is used as an active catalytic site, so that the material shows good catalytic activity in electro-catalytic oxygen evolution.

Description

technical field [0001] The invention belongs to the field of porous polymer materials, and in particular relates to a preparation method of a porous polymer containing iron and boron. Background technique [0002] Since the discovery of zeolites and their successful industrial applications, porous materials have become one of the most fascinating frontiers in modern chemistry; in the past ten years, the field of porous materials has undergone revolutionary development; some new Porous materials, such as metal-organic frameworks (MOFs), covalent organic frameworks (COFs) and amorphous porous organic polymers (POPs), have emerged. Compared with traditional porous materials such as zeolites and activated carbons, porous materials not only have higher The porosity of the porous framework can also incorporate targeted chemical functions or multiple chemical functions into porous frameworks through bottom-up or post-synthetic modifications, and thus has received extensive attentio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G79/14C25B11/085
CPCC08G79/14C25B11/085Y02E60/36
Inventor 顾志国石亚翔晏晓东张文达方欣
Owner JIANGNAN UNIV
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