Preparation method of lamellar two-dimensional porous covalent organic framework material

A covalent organic framework and lamellar technology, applied in chemical instruments and methods, organic compound/hydride/coordination complex catalysts, inorganic chemistry, etc., can solve the problem of slow proton reduction process, low photostability and low crystallinity and other problems, to achieve the effects of high visible light catalytic hydrogen production performance, high responsiveness, and mild reaction conditions

Active Publication Date: 2021-03-16
XIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the limited photostability of the catalyst, low crystallinity, and the slowness of the multi-electron diffusion-controlled proton reduction process, it is often challenging to prepare a COFs material with high catalytic efficiency and simple synthesis method.

Method used

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  • Preparation method of lamellar two-dimensional porous covalent organic framework material
  • Preparation method of lamellar two-dimensional porous covalent organic framework material
  • Preparation method of lamellar two-dimensional porous covalent organic framework material

Examples

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Effect test

Embodiment 1

[0029] A preparation method of a lamellar two-dimensional porous covalent organic framework material of the present invention is specifically implemented according to the following steps:

[0030] Step 1: carry out dehydrochloric acid treatment on 4,6-diaminoresorcinol dihydrochloride to obtain 4,6-diaminoresorcinol; specifically:

[0031] Step 1.1: Weigh 95.8 mg of raw material 4,6-diaminoresorcinol dihydrochloride;

[0032] Step 1.2: Put the raw materials weighed in step 1.1 into a pressure tube, and add 50 mL of polyphosphoric acid;

[0033] Step 1.3: degas the pressure tube containing the raw materials and solvent in step 1.2 with nitrogen gas for three times to ensure that the reaction is carried out under anhydrous and oxygen-free conditions;

[0034] Step 1.4: Stir the pressure tube of Step 1.3 at 70°C for 8h;

[0035] Step 2: Using 4,6-diaminoresorcinol and 2,4,6-tris(4-aldophenyl)-1,3,5-triazine as raw materials to prepare COFs material;

[0036] Step 2.1: Weigh 11...

Embodiment 2

[0048] A preparation method of a lamellar two-dimensional porous covalent organic framework material of the present invention is specifically implemented according to the following steps:

[0049] In step 1, 4,6-diaminoresorcinol dihydrochloride is subjected to dehydrochloric acid treatment to obtain 4,6-diaminoresorcinol;

[0050] Specifically: 4,6-diaminoresorcinol and polyphosphoric acid were added to the pressure tube, after three nitrogen degassing treatments, and then under nitrogen protection, the reaction was carried out in an oil bath at 80 °C for 8 hours, and the removal of hydrochloric acid;

[0051] Wherein, every 9mmol of 4,6-diaminoresorcinol corresponds to 1L of polyphosphoric acid;

[0052] Step 2, add 2,4,6-tris(4-aldolphenyl)-1,3,5-triazine to 4,6-diaminoresorcinol, then carry out temperature-programmed reaction, wait for the end of the reaction after cooling to room temperature, adding distilled water to the reaction solution, suction filtration, repeatedl...

Embodiment 3

[0056] A preparation method of a lamellar two-dimensional porous covalent organic framework material of the present invention is specifically implemented according to the following steps:

[0057] In step 1, 4,6-diaminoresorcinol dihydrochloride is subjected to dehydrochloric acid treatment to obtain 4,6-diaminoresorcinol;

[0058] Specifically: 4,6-diaminoresorcinol and polyphosphoric acid were added to the pressure tube, after three nitrogen degassing treatments, and then under nitrogen protection, the reaction was carried out in an oil bath at 80 °C for 8 hours, and the removal of hydrochloric acid;

[0059] Wherein, every 10mmol of 4,6-diaminoresorcinol corresponds to 1L of polyphosphoric acid;

[0060] Step 2, add 2,4,6-tris(4-aldolphenyl)-1,3,5-triazine to 4,6-diaminoresorcinol, then carry out temperature-programmed reaction, wait for the end of the reaction after cooling to room temperature, adding distilled water to the reaction solution, suction filtration, repeated...

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Abstract

The invention discloses a preparation method of a lamellar two-dimensional porous covalent organic framework material, which comprises the following steps of: carrying out hydrochloric acid removal treatment on 4, 6-diamino resorcinol dihydrochloride to obtain 4, 6-diamino resorcinol; and adding 2, 4, 6-tri (4-aldehyde phenyl)-1, 3, 5-triazine into the 4, 6-diamino resorcinol, carrying out programmed heating reaction, cooling to room temperature after the reaction is finished, adding distilled water into the reaction liquid, carrying out suction filtration, washing to be neutral, and drying toobtain the lamellar two-dimensional porous covalent organic framework (COFs) material. The COFs material with the lamellar structure prepared by the method disclosed by the invention has a high conjugate structure, has relatively high response capability to visible light and has relatively high visible light catalytic hydrogen production performance.

Description

technical field [0001] The invention belongs to the technical field of preparation of organic framework materials, in particular to a preparation method of a lamellar two-dimensional porous covalent organic framework material. Background technique [0002] For nearly two centuries, energy shortage and environmental pollution are the two major challenges facing human existence. Hydrogen energy has high energy density and no pollution, and is an ideal clean energy. At present, with the rapid development of materials science, photocatalytic water splitting for hydrogen production is an ideal method for obtaining hydrogen energy. Among them, covalent organic frameworks (COFs) have increasingly become a research hotspot in the field of heterogeneous catalysts due to their orderly pore structure, adjustable diameter, relatively high specific surface area, various preparation methods, and easy functional modification. These COFs have tunable chemical and physical properties, and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G8/16B01J31/06C01B3/04
CPCC08G8/16B01J31/06B01J35/004C01B3/042Y02E60/36
Inventor 何仰清师静马占营杨谦姚秉华
Owner XIAN UNIV OF TECH
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