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Synthesis method of porous organic covalent framework material having triazine structure

A framework material and synthesis method technology, applied in the synthesis field of organic porous framework materials, can solve the problems of complex experimental process, high cost and high technical requirements, and achieve the effects of simple synthesis process, low synthesis cost and good application prospect.

Inactive Publication Date: 2017-09-05
NORTHWEST NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, most of these synthesized COFs are expensive, the experimental process is complicated, and the technical requirements are high.

Method used

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  • Synthesis method of porous organic covalent framework material having triazine structure
  • Synthesis method of porous organic covalent framework material having triazine structure
  • Synthesis method of porous organic covalent framework material having triazine structure

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Dissolve 0.6036g melamine and 0.9225g cyanuric chloride (mass ratio: 1:1) in 20ml of freshly steamed dimethyl sulfoxide (DMSO), then mix the two solutions and place in an oil bath at 150°C Stir the reaction in medium temperature, stop the reaction after four days, and carry out suction filtration after standing and aging overnight (10~12h). Wash with methanol. After washing, vacuum-dry at 60°C for 24 hours, and fully grind to obtain a white powder, which is the product COF product. The yield is about 70%, and the specific surface area of ​​the product is about 301.149 m 2 / g, the pore diameter is about 1.41 nm.

Embodiment 2

[0028] Keeping other conditions constant in Example 1, and increasing the ratio of melamine (the ratio of the amount of substance is 1:1.1), the specific surface area of ​​the product will be reduced, and this is because unreacted melamine is more difficult to obtain from the reaction product Separation in the medium, attached to the surface of the product or its pores, so that the specific surface area is reduced. Therefore, the ratio of the amount of melamine to cyanuric chloride should be strictly controlled at 1:1~1:1.1.

Embodiment 3

[0030] Keeping other conditions unchanged in Example 1, and increasing the reaction temperature to 180° C., it was found that the reaction was completed more rapidly, but as the reaction progressed further, the product would appear yellow and larger particles of precipitates would appear. It has been determined that the specific surface area decreases. This is because the reaction at a higher temperature for a long time will change or even destroy the formed microporous particle structure, which is not conducive to the production of qualified products. Therefore, the reaction temperature should be controlled at 130-150°C.

[0031] In each of the above examples, white gas will be emitted when the reaction is carried out for nearly two hours, and it is recommended to lower the reaction temperature to 130°C.

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Abstract

The invention provides a synthesis method of a porous organic covalent framework material having a triazine structure. According to the present invention, the porous organic covalent framework material COF is synthesized by using melamine and cyanuric chloride as raw materials using dimethyl sulfoxide as a solvent through a hot melt method; the synthesis method has characteristics of cheap and easily available raw materials, simple synthesis process, mild reaction condition, low synthesis cost, high yield and the like; and the synthesized COF material has advantages of high specific surface area, low density and high nitrogen content, and has good application prospects in the fields of adsorption, electrode materials, catalysis and the like.

Description

technical field [0001] The invention relates to the synthesis of an organic covalent framework material, in particular to a synthesis method of a porous organic covalent framework material with a triazine structure, and belongs to the technical field of synthesis of organic porous framework materials. Background technique [0002] Covalent organic frameworks (COFs) are a new class of porous organic materials, which have the advantages of large specific surface area, rich pore structure, light weight, orderly structure, and adjustable structure and pore size. In 2005, the Yaghi team at the University of Michigan in the United States successfully prepared the first covalent organic framework polymer COF-1 by using 1,4-p-diphenylboronic acid self-dehydration condensation, and published it in the top international journal Science, which has attracted the attention of researchers from all over the world. Chinese scientists are also actively engaged in research in this field. In ...

Claims

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Application Information

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IPC IPC(8): C08G83/00
CPCC08G83/008
Inventor 杨武薛瑞郭昊王婷黄冬冬
Owner NORTHWEST NORMAL UNIVERSITY
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