Synthesis method of porous organic covalent frame material with triazine structure

A frame material and synthesis method technology, which is applied in the field of synthesis of organic porous frame materials, can solve the problems of high cost, complicated experimental process, and high technical requirements, and achieve the effects of low synthesis cost, simple synthesis process, and good application prospects

Inactive Publication Date: 2018-06-05
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 experimen

Method used

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  • Synthesis method of porous organic covalent frame material with triazine structure
  • Synthesis method of porous organic covalent frame material with triazine structure
  • Synthesis method of porous organic covalent frame material with triazine structure

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Dissolve 0.9733g of p-phenylenediamine and 1.107g of cyanuric chloride (the molar ratio of substances is 3:2) in 35 ml and 11ml of dioxane-mesitylene-acetic acid mixed solvents respectively (the volume ratio of the three solvents 5:5:1), then mix the two reactant solutions evenly, transfer to a stainless steel autoclave, keep at 120°C for 70 hours, and wash the product repeatedly with tetrahydrofuran and methanol. After washing, vacuum dry at 120°C for 24 hours , the khaki powder obtained after grinding is the target product. The yield is about 82%, and the specific surface area of ​​the product is 33.6447 m 2 ∙g -1 , with a pore size of about 1.37 nm.

Embodiment 2

[0033] Dissolve 0.9733g p-phenylenediamine and (0.5535g) cyanuric chloride (ratio of substance is 3:1) in 35ml and 10ml dioxane-mesitylene-acetic acid mixed solvent respectively (three solvents The volume ratio is 4.5:4.5:1), and then the two reactant solutions are mixed evenly, transferred to a stainless steel high-pressure reactor, and kept at 120°C for 70 hours. The product is washed repeatedly with tetrahydrofuran and methanol. After washing, it is vacuum-dried at 120°C After 24 hours, the yellow powder obtained after grinding was the target product. The yield is about 80%, and the specific surface area of ​​the product is 15m 2 ∙g -1 , with a pore size of about 1.5 nm.

[0034] Compared with Example 1, when other conditions are constant, increasing the ratio of p-phenylenediamine and cyanuric chloride will make the specific surface area of ​​the product smaller, because unreacted p-phenylenediamine is more difficult to It is separated from the reaction product and atta...

Embodiment 3

[0036] Dissolve 0.9733g p-phenylenediamine and 1.107g cyanuric chloride (mass ratio is 3:2) in 35ml and 10ml dioxane-mesitylene-acetic acid mixed solvent respectively (three kinds of solvent volume ratio 4:4:1), then mix the two reactant solutions evenly, transfer them to a stainless steel autoclave, keep at 120°C for 70 hours, and wash the product repeatedly with tetrahydrofuran and methanol. After washing, dry it under vacuum at 120°C for 24 hours , the khaki powder obtained after grinding is the target product. The yield is about 87%, and the specific surface area of ​​the product is 9 m 2 ∙g -1 , with a pore size of about 1.8 nm.

[0037] Compared with Example 1, under the condition that other conditions are constant, the ratio of three kinds of solvents is adjusted, and it is found that the solubility of the reactant decreases, and the specific surface area of ​​the product decreases. It is not conducive to the production of qualified products.

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Abstract

The invention provides a synthesis method of a porous organic covalent frame material with a triazine structure. The synthesis method comprises the steps of in a 1,4-dioxane-mesitylene-acetic acid mixed solvent, carrying out solvothermal reaction on p-phenylenediamine and cyanuric chloride for 70 to 72h at 115 to 120 DEG C, repetitively washing a product through tetrahydrofuran and methyl alcohol,drying, grinding, and obtaining earthy yellow powder which is a target object. The synthesis method provided by the invention has the characteristics of cheap and easy-to-get raw materials, simple synthesis process, mild reaction conditions, low synthesis cost, high yield and the like; the synthesized COF material is large in specific surface area, low in density, and high in nitrogen content, and has a better application prospect in the fields of adsorption, drug release, photoelectricity functions, 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 dehydration condensation of 1,4-p-diphenylboronic acid itself. Actively engage in research in this field. In terms of the synthesis and application of COFs, the United States, Japan, Germany and other countries are at the forefront, and Spain, France, South Korea, India a...

Claims

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Application Information

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IPC IPC(8): C08G83/00
CPCC08G83/008
Inventor 郭昊薛瑞王婷王笑岳利国杨武
Owner NORTHWEST NORMAL UNIVERSITY
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