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Method for rapidly preparing two-dimensional covalent organic framework material at low temperature and two-dimensional covalent organic framework material

A covalent organic framework, room temperature technology, applied in the field of two-dimensional covalent organic framework materials, low-temperature rapid preparation of two-dimensional covalent organic framework materials, can solve complex operation process, high reaction temperature, long reaction time and other problems

Pending Publication Date: 2020-10-23
CHINA UNIV OF GEOSCIENCES (BEIJING)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These methods generally require conditions such as higher reaction temperature (≥90°C), longer reaction time (ranging from several hours to several days) or complicated operation process.

Method used

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  • Method for rapidly preparing two-dimensional covalent organic framework material at low temperature and two-dimensional covalent organic framework material
  • Method for rapidly preparing two-dimensional covalent organic framework material at low temperature and two-dimensional covalent organic framework material
  • Method for rapidly preparing two-dimensional covalent organic framework material at low temperature and two-dimensional covalent organic framework material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] This example provides a method for rapidly preparing a two-dimensional covalent organic framework material at low temperature, as follows.

[0044] Step 1: In the reaction vessel, sequentially add 1 mL of dioxane and mesitylene with a volume ratio of 4:1 mixed solvent, 0.08 mmol 4,4',4"-(1,3,5-triazine-2 ,4,6-triyl)trianiline (4,4',4"-(1,3,5-triazine-2,4,6-triyl)trianiline, TTA) and 0.12 mmol 3,3'-bipyridine -6,6'-dicarbaldehyde ([3,3'-bipyridine]-6,6'-dicarbaldehyde, BPA), ultrasonically dispersed to obtain a mixed solution 1. Wherein, the reaction container may be a glass vessel with a lid. Specifically, the ultrasonic dispersion can be 60W for 10 seconds.

[0045] Step 2: Add 0.08 mmol of Lewis acid and 0.4 mL of acetic acid solution with a concentration of 6 mol / L into the mixed solution 1, and disperse uniformly by ultrasonic to obtain the mixed solution 2. Specifically, the ultrasonic dispersion can be 60W for 5 seconds.

[0046] Step 3: Seal the reaction vess...

Embodiment 2

[0055] This example provides a method for rapidly preparing a two-dimensional covalent organic framework material at low temperature, as follows.

[0056] Step 1: In the reaction vessel, sequentially add 1 mL of dioxane and mesitylene with a volume ratio of 4:1 mixed solvent, 0.08 mmol of 1,3,5-tris(4-aminophenyl)benzene (1,3, 5-tris(4-aminophenyl)benzene, TAPB) and 0.12mmol 3,3'-bipyridine-6,6'-dicarbaldehyde (BPA) were dispersed uniformly by ultrasonic to obtain a mixed solution 1.

[0057] Step 2: Add 0.08 mmol of Lewis acid and 0.4 mL of acetic acid solution with a concentration of 6 mol / L into the mixed solution 1, and disperse uniformly by ultrasonic to obtain the mixed solution 2.

[0058] Step 3: Seal the reaction vessel containing the mixed solution 2 at normal temperature and pressure, or seal it under vacuum after quick freezing with liquid nitrogen.

[0059] Step 4: Reacting the closed reaction vessel at a relatively low temperature (0-25° C.) for 1-30 minutes to ...

Embodiment 3

[0067] This example provides a method for rapidly preparing a two-dimensional covalent organic framework material at low temperature, as follows.

[0068] Step 1: In the reaction vessel, sequentially add 1 mL of dioxane and mesitylene with a volume ratio of 4:1 mixed solvent, 0.08 mmol 4,4',4"-(1,3,5-triazine-2, 4,6-triyl)triphenylamine (TTA) and 0.12 mmol 2,5-dicarboxyphenazine (pyrazine-2,5-dicarbaldehyde, PDA) were dispersed uniformly by ultrasonic to obtain a mixed solution 1.

[0069] Step 2: Add 0.08 mmol of Lewis acid and 0.4 mL of acetic acid solution with a concentration of 6 mol / L into the mixed solution 1, and disperse uniformly by ultrasonic to obtain the mixed solution 2.

[0070] Step 3: Seal the glass reaction container containing the mixed solution 2 at normal temperature and pressure, or seal it under vacuum after quick freezing with liquid nitrogen.

[0071] Step 4: Reacting the closed reaction vessel at a relatively low temperature (0-25° C.) for 1-30 minut...

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Abstract

The invention relates to the technical field of organic material preparation, in particular to a method for rapidly preparing a two-dimensional covalent organic framework material at a low temperatureand the two-dimensional covalent organic framework material. The material is obtained by reacting aromatic amine with aromatic aldehyde at the temperature of 0 DEG C to room temperature, wherein thearomatic amine is one or more of 1, 4-phenylenediamine, 1, 4-biphenyl diamine, 4, 4', 4''-(1, 3, 5-triazine-2, 4, 6-triyl)triphenylamine, 1, 3, 5-tri(4-aminophenyl)benzene, tri(4-aminophenyl)amine, tetra(4-aminophenyl)porphyrin and tetra (4-aminophenyl)methane, the aromatic aldehyde is one or more of aromatic aldehyde containing pyridine and phenazine structures, 3, 3'-dipyridine-6, 6'-diformaldehyde, 2, 2'-dipyridine-5, 5'-diformaldehyde, 5,5',5''-(phenyl-1, 3, 5-triyl)tripyridylaldehyde, 6,6',6'''-(phenyl-1, 3, 5-triyl)tripyridylaldehyde, and the molar ratio of the aromatic amine to the aromatic aldehyde is (0.1-10): 1.

Description

technical field [0001] The invention relates to the technical field of organic material preparation, in particular to a method for rapidly preparing a two-dimensional covalent organic framework material at low temperature and the two-dimensional covalent organic framework material. Background technique [0002] Two-dimensional covalent organic framework (COF) is a kind of material formed by the connection of organic monomer molecules in the form of covalent bonds, which has a certain topology and high crystallinity. Due to the diversity and designability of organic molecular structures, through the design and selection of organic monomer molecules, two-dimensional covalent organic framework materials with rich topological structures, adjustable pore structures, modifiable channels, and functional diversification can be realized. Regulate synthesis. Compared with molecular assembly systems, two-dimensional covalent organic framework materials connected by covalent bonds have...

Claims

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Application Information

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IPC IPC(8): C08G73/06
CPCC08G73/0627C08G73/0644C08G73/065
Inventor 孙兵冯甜甜
Owner CHINA UNIV OF GEOSCIENCES (BEIJING)
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