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Preparation method of two-dimensional covalent organic framework material with spherical porous structure

A covalent organic framework and porous structure technology, applied in the field of photocatalytic materials, can solve the problems of light stability, low crystallinity, slow multi-electron diffusion-controlled proton reduction process, etc., to achieve enhanced absorption capacity and electron transport capacity , high visible light catalytic hydrogen production performance, and mild reaction conditions

Active Publication Date: 2021-03-16
XIAN UNIV OF TECH
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Problems solved by technology

However, the synthesis of an efficient photocatalytic COFs is often challenging due to the limited photostability of the catalyst, low crystallinity, and slow multi-electron diffusion-controlled proton reduction process.

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  • Preparation method of two-dimensional covalent organic framework material with spherical porous structure
  • Preparation method of two-dimensional covalent organic framework material with spherical porous structure
  • Preparation method of two-dimensional covalent organic framework material with spherical porous structure

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preparation example Construction

[0030] The invention discloses a method for preparing a two-dimensional covalent organic framework material with a spherical porous structure, which specifically includes the following steps:

[0031] Step 1, using 1,10-phenanthroline-2,9-dicarbaldehyde and 2,4,6-tris(4-aminophenyl)-1,3,5-triazine as raw materials to prepare organic framework COFs,

[0032] Specifically: 1,10-phenanthroline-2,9-dicarbaldehyde, 2,4,6-tris(4-aminophenyl)-1,3,5-triazine, mesitylene, 1,4 - Dioxane and glacial acetic acid were added to the pressure tube and subjected to nitrogen degassing treatment three times, then reacted at 100-120°C for 3 days, and washed with tetrahydrofuran after the reaction to obtain organic framework material COFs.

[0033] Wherein, the mass ratio of 1,10-phenanthroline-2,9-dimethylaldehyde to 2,4,6-tris(4-aminophenyl)-1,3,5-triazine is 1:1-2.

[0034] Among them, the mass volume ratio of 1,10-phenanthroline-2,9-dimethylaldehyde to glacial acetic acid is 420-460 mg / mL, an...

Embodiment 1

[0052] Step 1: Preparation of organic framework material COFs

[0053] Step 1.1: Weigh 92 mg of 1,10-phenanthroline-2,9-dicarbaldehyde and 92 mg of 2,4,6-tris(4-aminophenyl)-1,3,5-triazine (TTA);

[0054] Step 1.2: Put the raw materials weighed in step 1.1 into a pressure tube, and add 5.1 mL of mesitylene, 0.9 mL of 1,4-dioxane and 0.2 mL of 3 g / mol glacial acetic acid;

[0055] Step 1.3: Degas the pressure tube containing the raw materials and solvent in step 1.2 three times with nitrogen to ensure that the reaction is carried out under anhydrous and oxygen-free conditions;

[0056] Step 1.4: react the pressure tube in step 1.3 at a temperature of 120° C. for three days;

[0057] Step 1.5: washing the product after the reaction in step 1.4 with tetrahydrofuran to obtain a two-dimensional COFs material with a spherical porous structure, which is an organic framework material COFs. Its infrared spectrum and solid NMR diagram are shown in figure 1 and figure 2 .

[0058] ...

Embodiment 2

[0072] Step 1: Preparation of organic framework material COFs

[0073] Step 1.1: Weigh 92 mg of 1,10-phenanthroline-2,9-dicarbaldehyde and 184 mg of 2,4,6-tris(4-aminophenyl)-1,3,5-triazine (TTA);

[0074] Step 1.2: Put the raw materials weighed in step 1.1 into a 25mL pressure tube, and add 4.2mL of mesitylene, 0.84mL of 1,4-dioxane and 0.21mL of 3g / mol glacial acetic acid;

[0075] Step 1.3: Degas the pressure tube containing the raw materials and solvent in step 1.2 three times with nitrogen to ensure that the reaction is carried out under anhydrous and oxygen-free conditions;

[0076] Step 1.4: React the pressure tube in step 1.3 at a temperature of 100°C for three days;

[0077] Step 1.5: washing the product after the reaction in step 1.4 with tetrahydrofuran to obtain a two-dimensional COFs material with a spherical porous structure, which is an organic framework material COFs.

[0078] Step 2: Modification of organic framework material COFs with iridium complex LX1

...

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Abstract

The invention discloses a preparation method of a two-dimensional covalent organic framework material with a spherical porous structure, which comprises the following steps: preparing an organic framework material COFs by using 1,10-phenanthroline-2,9-dicarbaldehyde and2,4,6-tris(4-aminophenyl)-1,3,5-triazine as raw materials, and modifying the organic framework material COFs by using an iridium complex LX1 to obtain the two-dimensional covalent organic framework material with the spherical porous structure. According to the preparation method disclosed by the invention, the organic frameworkmaterial COFs are successfully synthesized by utilizing a solvothermal method, reaction conditions are mild, and a synthesis process is simple and easy to realize. The iridium-containing transition metal complex LX1 is used for carrying out functional modification on the organic framework material COFs, so that the light absorption capability and the electron transmission capability of the organicframework material COFs and the stability of the COFs material can be enhanced; and the obtained COFs material with the spherical porous structure has relatively high visible light catalytic hydrogenproduction performance.

Description

technical field [0001] The invention belongs to the field of photocatalytic materials, and in particular relates to a method for preparing a two-dimensional covalent organic framework material with a spherical porous structure. Background technique [0002] With the natural reserves of petroleum fuels decreasing day by day, seeking new, clean and sustainable alternative energy sources is a major scientific problem that mankind urgently needs to solve. Converting solar energy into storable "solar fuels" such as hydrogen through artificial photosynthesis is one of the most feasible and sustainable solutions to this challenge. Therefore, the development of highly efficient photocatalytic systems to generate hydrogen energy through light-induced water splitting has aroused widespread interest among scientists in the field of energy research. Covalent organic frameworks (Covalent Organic Frameworks, COFs) are similar to semiconductor nitrogen carbide and are composed of light el...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G12/40C08G12/30B01J31/22B01J35/10B01J35/08C01B3/04
CPCC08G12/40C08G12/30B01J31/2295B01J31/1691B01J31/165C01B3/042B01J2531/827B01J35/39B01J35/51B01J35/60Y02E60/36
Inventor 何仰清王雪婷杨谦姚秉华
Owner XIAN UNIV OF TECH
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