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Preparation method of porous covalent organic framework material with triazine structure

A technology of covalent organic framework and triazine is applied in the field of preparation of porous covalent organic framework materials, which can solve the problems to be improved, and achieve the effects of good spatial structure stability, high yield and mild reaction conditions.

Active Publication Date: 2021-06-04
XIAN UNIV OF SCI & TECH
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  • Abstract
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Problems solved by technology

[0003] The Chinese invention patent with the publication number CN108117651A discloses a method for synthesizing a porous organic covalent framework material with a triazine structure. The invention is carried out in a mixed solvent of 1,4-dioxane-mesitylene-acetic acid, p-Phenylenediamine and cyanuric chloride react solvothermally at 115~120°C for 70~72h, and the product is repeatedly washed with tetrahydrofuran and methanol, dried and ground to obtain a khaki powder, which is a porous organic compound with a triazine structure. Covalent framework material; although the synthesis method of the invention has the advantages of cheap and easy-to-obtain raw materials, simple synthesis process, mild reaction conditions, low synthesis cost, and high yield, the organic covalent framework material prepared by this method has low crystallinity and Specific surface area still needs to be improved

Method used

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  • Preparation method of porous covalent organic framework material with triazine structure
  • Preparation method of porous covalent organic framework material with triazine structure
  • Preparation method of porous covalent organic framework material with triazine structure

Examples

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Embodiment 1

[0038] Example 1 Preparation method of a porous covalent organic framework material with a triazine structure

[0039] The synthetic reaction formula of present embodiment is as figure 1 As shown, it proceeds in the following steps:

[0040] S1. Mix 0.01772 g (5 mmol) 2,4,6-tris(4-aminophenyl)-1,3,5-triazine with 0.01967 g (5 mmol) 2,4,6-tris(4-formylbenzene base)-1,3,5-triazine (molar ratio 1 : 1) was dissolved in 11 mL of dioxane-mesitylene-acetic acid mixed solvent (the volume ratio between the three solvents was 5 : 5 : 1 ) and sonicate for 30 min to obtain system A1;

[0041] S2. Add 0.002775g of anhydrous calcium chloride (water removal agent) to system A1 for dehydration, then transfer to a stainless steel autoclave, pass in argon, and conduct a solvothermal reaction at 120°C for 72 h under an argon atmosphere , to obtain product B1;

[0042] S3. The product B1 was washed with N,N-dimethylformamide first, then with ethanol, and repeated washing three times. After th...

Embodiment 2~8

[0055] Examples 2-8 Preparation method of porous covalent organic framework material with triazine structure

[0056] Examples 2 to 8 are respectively a preparation method of a porous covalent organic framework material with a triazine structure, and their preparation steps are basically the same as in Example 1, the only difference lies in the amount of raw materials and process parameters. For details, see The following table:

[0057]

[0058] Among the F2~F8 materials, three kinds were randomly selected for morphology characterization analysis. Figure 9 For the scanning electron micrograph of the F3 material prepared in Example 3, the magnification is 20000 times; Figure 10 For the scanning electron micrograph of the F5 material prepared in Example 5, the magnification is 20000 times; Figure 11 The scanning electron microscope image of the F7 material prepared for Example 7 has a magnification of 20,000 times; it can be seen that the COF materials prepared by the m...

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Abstract

The invention discloses a preparation method of a porous covalent organic framework material with a triazine structure, which comprises the following steps: by taking 2,4,6-tris(4-formylphenyl)-1,3,5-triazine and 2,4,6-tris (4-aminophenyl)-1,3,5-triazine as raw materials and a mixed solution of 1,4-dioxane, mesitylene and acetic acid as a solvent, adding a water removal agent, and synthesizing the compound by a preparation method combining ultrasonic and solvothermal reaction. The method is simple in process, mild in reaction condition and relatively high in yield; the prepared material has a relatively large specific surface area, relatively high nitrogen content and good thermal stability and crystallinity. The method is suitable for preparing the porous covalent organic framework material with the triazine structure.

Description

technical field [0001] The invention belongs to the synthesis technology of organic materials, and relates to a preparation method of a porous covalent organic framework material, specifically a preparation method of a porous covalent organic framework material with a triazine structure. Background technique [0002] Covalent organic frameworks (COFs) are a class of porous organic polymer materials with crystallinity and periodicity, which have the advantages of large specific surface area, rich pore structure, light weight, ordered structure, and adjustable pore size. It has good application prospects in the fields of photovoltaic materials, guest molecular adsorption, material transport, energy storage, photoelectric functions, and nanoreactors, so it has received extensive attention. [0003] The Chinese invention patent with the publication number CN108117651A discloses a method for synthesizing a porous organic covalent framework material with a triazine structure. The ...

Claims

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Application Information

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IPC IPC(8): C08G12/30
CPCC08G12/30
Inventor 熊善新刘健刘娟娟
Owner XIAN UNIV OF SCI & TECH
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