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Snowflake-like biomimetic covalent organic framework cofs photocatalyst and its preparation method

A covalent organic framework, photocatalyst technology, applied in the field of photocatalysis, can solve the problems of high operational safety requirements, difficulty in achieving green environmental protection, poor chemical stability, etc. The effect of improving the activity of photo-splitting water for hydrogen production

Active Publication Date: 2022-06-03
SOUTHEAST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The photocatalyst has a long service life, but its disadvantage is that the reaction process requires super acid trifluoromethanesulfonic acid, which requires high equipment and operation safety, and the existing photocatalysts generally have the problem of poor chemical stability. Difficult to be green in the process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Add 0.351g 1,3,5-tris(4-aminophenyl)benzene, 0.210g trialdehyde phloroglucinol to 7mL 1,3,5-trimethylbenzene and 7mL 1,4-dioxane 1 mL of 3 mol / L glacial acetic acid was added dropwise to the mixed solution, and it was sonicated for 30 min until it was completely dissolved. Under vacuum, react at 150 °C for 60 h, then add 6 mL of N,N-dimethylformamide to the reaction solution, and continue the reaction for 24 h. Washed with 1,4-dioxane for 3 times and dried at 80 °C for 7 h to obtain a three-dimensional COFs structure material with ketone groups.

[0029] 50mg of three-dimensional COFs structure material was added to 20mL of water, 0.5mL of 3mol / L acetic anhydride solution was added dropwise to the above reaction solution, stirred at 75°C for 26h for ketone group addition, the reaction was cooled to room temperature, washed 3 times, and dried. Then the double hydroxyl structure material is obtained.

[0030] 0.076g of glycine, 0.088g of dihydroxy structural material an...

Embodiment 2

[0034] 0.290g of tris(4aminophenyl)amine and 0.210g of trialdehyde-based phloroglucinol were added to the mixed solution of 12mL of 1,3,5-trimethylbenzene and 6mL of 1,4-dioxane, and added dropwise. A mixture of 0.5mL of 3mol / L glacial acetic acid and 0.5mL of 3mol / L phosphoric acid, ultrasonicated for 20min until completely dissolved, reacted under vacuum at 140°C for 48h, then added 5mL of N,N-dimethylformamide to the reaction solution, and continued The reaction was carried out for 24 h, washed with 1,4-dioxane for 3 times, washed with dichloromethane for 3 times, and dried at 60 °C for 8 h to obtain a three-dimensional COFs structure material with a ketone group.

[0035]Add 50 mg of three-dimensional COFs structure material to 15 mL of water, add 0.5 mL of 3mol / L glacial acetic acid solution to the above reaction solution, stir at 80 °C for 24 h for ketone addition, cool the reaction to room temperature, and wash with deionized water for 3 Second, the double-hydroxyl stru...

Embodiment 3

[0040] Add 0.354g 2,4,6-tris(4-aminophenyl)-1,3,5-triazine, 0.210g trialdehyde phloroglucinol to 8mL 1,3,5-trimethylbenzene and To the mixed solution of 8mL 1,4-dioxane, add 1mL 3mol / L sulfurous acid dropwise, ultrasonicate for 25min to completely dissolve, react under vacuum at 135°C for 48h, and then add 7mL N,N-dimethylformamide to In the reaction solution, the reaction was continued for 24 h, washed three times with 1,4-dioxane, washed three times with acetone, and dried at 55 °C for 8 h to obtain a three-dimensional COFs structure material with a ketone group.

[0041] 50mg of three-dimensional COFs structural material was added to 18mL of water, and a mixture of 0.25mL of 3mol / L glacial acetic acid solution and 0.25mL of 3mol / L acetic anhydride solution was added to the above reaction solution, and stirred at 65 ° C for 22h to carry out ketone addition. The reaction was cooled to room temperature, washed three times with deionized water, and dried to obtain a dihydroxy s...

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Abstract

The invention discloses a snowflake-like biomimetic covalent organic framework COFs photocatalyst and a preparation method thereof. The steps are as follows: first, the three-dimensional COFs structure is formed by the reaction between the amino group and the aldehyde group in the raw material, and the enol formula Interconversion to form a keto group provides the basis for subsequent electrophilic addition. Secondly, the electrophilic addition reaction of water molecules to the ketone group is used to form a dihydroxy structure, and the dehydration reaction between the dihydroxy structure and the carboxyl group in the amino acid is used to form a new snowflake-like biomimetic COFs material. The pore size can be further adjusted by changing the reactant molecule and the type of amino acid. Controlling, using the covalent interaction between the amino lone pair electrons on the snowflake and the empty orbital of the co-catalyst Pt to achieve uniform dispersion of the co-catalyst. The COFs material of the present invention introduces amino acids, is cheap and easy to obtain, and is environmentally friendly, and the hydrophilic property of the snowflake-like material is conducive to accelerating the process of hydrogen production by photolysis of water. The porosity, crystallinity and π-π conjugated system of COFs materials endow the material with excellent physical and chemical properties.

Description

technical field [0001] The invention belongs to the technical field of photocatalysis, and in particular relates to a novel snowflake-shaped biomimetic covalent organic framework COFs photocatalyst and a preparation method thereof. Background technique [0002] With the rapid development of the economy, the sustainable development of human society comes along with it. The problem of excessive consumption of fossil energy is particularly prominent. Energy shortage and environmental problems have become constraints on the sustainable development of human society. Therefore, it is necessary to develop some alternatives. Clean energy alternatives to fossil fuels. Hydrogen energy has received extensive attention as a clean and renewable energy source, and photocatalytic hydrogen production technology may provide abundant clean energy in the future to alleviate the environmental crisis. At present, many inorganic semiconductors, including cadmium sulfide, zinc oxide and other ino...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G14/073C08G14/12B01J31/06C01B3/04
CPCC08G14/06C08G14/12B01J31/06C01B3/042B01J35/39Y02E60/36
Inventor 张一卫费婷毛春峰王东东周钰明董国盟
Owner SOUTHEAST UNIV
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