Method for preparing covalent organic framework material by high-pressure homogenization

A covalent organic framework, high-pressure homogenization technology, applied in chemical instruments and methods, other chemical processes, etc., can solve the problems of large amount of organic solvent, long synthesis time, complex process, etc., and achieve short reaction time and low cost. , the effect of simple operation

Active Publication Date: 2021-06-25
NANKAI UNIV
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  • Abstract
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  • Claims
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Problems solved by technology

[0005] In view of the deficiencies in the prior art, the purpose of the present invention is to provide a method for preparing covalent organic framework materials using high pressure homogenization (high pressure homogenization, HPH), to solve the problems of long synthesis time, complicated process and high energy consumption in the prior art. , low yield, and many problems in the use of organic solvents

Method used

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  • Method for preparing covalent organic framework material by high-pressure homogenization
  • Method for preparing covalent organic framework material by high-pressure homogenization
  • Method for preparing covalent organic framework material by high-pressure homogenization

Examples

Experimental program
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Effect test

Embodiment 1

[0033] S1. At normal temperature and pressure, add 2,4,6-trihydroxy-1,3,5-benzenetricarbaldehyde (1mmol) and p-phenylenediamine (1.5mmol) into a 500mL beaker at a molar ratio of 1:1.5 , add 300mL water, 150mL glacial acetic acid, and stir for 5min with a mechanical mixer;

[0034] S2. Under normal temperature and pressure, turn on the circulating condensed water of the high-pressure homogenizer, and adjust the temperature to 0°C, add the above-mentioned suspension to the high-pressure homogenizer, and circulate the homogeneous reaction for 30 minutes at a homogenization pressure of 100 MPa;

[0035] S3. After the reaction is over, use a 500mL beaker to take the reaction suspension, and vacuum filter to obtain a solid product. The filtrate is recovered and stored. After the product is washed with water, ethanol, and acetone in sequence, it is dried at 150°C for 12 hours to obtain a high-pressure average product. The HPH-TpPa-1 prepared by mass method has an isolated yield of 81...

Embodiment 2

[0041] S1. At normal temperature and pressure, add 2,4,6-trihydroxy-1,3,5-benzenetricarbaldehyde (1mmol) and p-phenylenediamine (1.5mmol) into a 500mL beaker at a molar ratio of 1:1.5 , add 300mL water, 150mL glacial acetic acid, and stir for 5min with a mechanical mixer;

[0042] S2. Under normal temperature and pressure, turn on the circulating condensed water of the high-pressure homogenizer, and adjust the temperature to 0°C, add the above-mentioned suspension to the high-pressure homogenizer, and circulate the homogeneous reaction at a homogenization pressure of 100 MPa for 120 minutes;

[0043] S3. After the reaction is over, use a 500mL beaker to take the reaction suspension, and vacuum filter to obtain a solid product. The filtrate is recovered and stored. After the product is washed with water, ethanol, and acetone in sequence, it is dried at 150°C for 12 hours to obtain a high-pressure average product. The HPH-TpPa-1 prepared by mass method has an isolated yield of 82%...

Embodiment 3

[0045] S1. At normal temperature and pressure, add 2,4,6-trihydroxy-1,3,5-benzenetricarbaldehyde (1mmol) and p-phenylenediamine (2mmol) into a 500mL beaker at a molar ratio of 1:2, Add 300mL of water and 150mL of glacial acetic acid, and stir for 5min with a mechanical stirrer;

[0046] S2. Under normal temperature and pressure, turn on the circulating condensed water of the high-pressure homogenizer, and adjust the temperature to 0°C, add the above-mentioned suspension to the high-pressure homogenizer, and circulate the homogeneous reaction at a homogenization pressure of 100 MPa for 120 minutes;

[0047] S3. After the reaction is over, use a 500mL beaker to take the reaction suspension, and vacuum filter to obtain a solid product. The filtrate is recovered and stored. After the product is washed with water, ethanol, and acetone in sequence, it is dried at 150°C for 12 hours to obtain a high-pressure average product. The HPH-TpPa-1 prepared by mass method has an isolated yiel...

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Abstract

The invention relates to a method for preparing a covalent organic framework material by high-pressure homogenization. According to the synthesis method, at normal temperature and normal pressure, a common organic ligand is used as a raw material, water or an organic reagent is used as a solvent and a template agent, organic acid and inorganic acid are used as catalysts, and the corresponding COFs are obtained by homogenizing for a certain time through a high-pressure homogenizer. The method comprises the following steps of: adding 2, 4, 6-trihydroxy-1, 3, 5-benzenetricarboxaldehyde and p-phenylenediamine into a beaker, adding a proper amount of water and acetic acid, uniformly mixing, adding the mixture into a high-pressure homogenizer, and homogenizing for a certain time; and carrying out suction filtration on the product powder after the homogenizing reaction, recycling the filtrate, washing the product powder, and carrying out vacuum drying to obtain the covalent organic framework material HPH-Tp-Pa-1. Compared with other COFs preparation methods, the method provided by the invention has the advantages of continuous reaction, simple operation, low cost, high yield, environmental protection, energy saving, short reaction time and the like, has the potential of large-scale production, and can greatly promote the industrial production process of the COFs material.

Description

technical field [0001] The invention belongs to the technical field of macromolecular organic porous materials, and in particular relates to a method for homogeneously preparing covalent organic framework materials by using high pressure. Background technique [0002] Covalent organic framework (COFs) is a kind of light elements such as C, H, O, N, B connected by reversible covalent bonds (such as C-N, C-O, B-O, C-N, etc.) Crystalline and periodic 2D or 3D organic porous materials. Due to the advantages of low density, easy functional modification, regular structure, adjustable pore structure, and large specific surface area, this type of material has attracted extensive attention from scientific researchers. It has broad application prospects. [0003] Covalent organic frameworks are ordered porous crystalline materials formed by thermodynamically controlled reversible or irreversible polymerization, often prepared by thermodynamic reactions. At present, the main prepara...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G83/00B01J20/22B01J20/30
CPCC08G83/008B01J20/226
Inventor 李柏延刘雄利
Owner NANKAI UNIV
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