A method for the homogeneous preparation of covalent organic framework materials using high pressure

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

Active Publication Date: 2022-05-06
NANKAI UNIV
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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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  • A method for the homogeneous preparation of covalent organic framework materials using high pressure
  • A method for the homogeneous preparation of covalent organic framework materials using high pressure
  • A method for the homogeneous preparation of covalent organic framework materials using high pressure

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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

A method for homogeneously preparing covalent organic framework materials under high pressure. The synthesis method is at normal temperature and pressure, using common organic ligands as raw materials, water or organic reagents as solvents and templates, and organic acids and inorganic acids as catalysts. , the method of obtaining the corresponding COFs by homogenizing with a high-pressure homogenizer for a certain period of time. Add 2,4,6-trihydroxy-1,3,5-benzenetricarbaldehyde and p-phenylenediamine in a beaker, add appropriate amount of water and acetic acid, mix well and add to a high-pressure homogenizer to homogenize for a certain period of time; After the qualitative reaction, the product powder was suction-filtered, and the filtrate was recycled for reuse. The product powder was washed and vacuum-dried to obtain the covalent organic framework material HPH-Tp-Pa-1. Compared with other COFs preparation methods, the present invention has the advantages of continuous reaction, simple operation, low cost, high yield, environmental protection and energy saving, short reaction time, etc., has the potential for large-scale production, and will greatly promote the industrial production process of COFs materials.

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 Patents(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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