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Novel snowflake-shaped bionic covalent organic framework COFs photocatalyst and preparation method thereof

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

Active Publication Date: 2021-10-19
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 0.351 g of 1,3,5-tris(4-aminophenyl)benzene, 0.210 g of trialdehyde phloroglucinol to 7 mL of 1,3,5-trimethylbenzene and 7 mL of 1,4-dioxane Add 1mL of 3mol / L glacial acetic acid dropwise to the mixed solution, and sonicate for 30min until 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. After washing with 1,4-dioxane three times and drying at 80°C for 7 hours, a three-dimensional COFs structure material with ketone groups was obtained.

[0029] Add 50mg of three-dimensional COFs structure material to 20mL of water, drop 0.5mL of 3mol / L acetic anhydride solution into the above reaction solution, stir at 75°C for 26h for ketone addition, cool the reaction to room temperature, wash 3 times, and dry After that, the double hydroxyl structure material is obtained.

[0030] Add 0.076g glycine, 0.088g dihydroxy structural material and 0.191g 4-toluenesulfonyl ...

Embodiment 2

[0034] Add 0.290g tris(4 aminophenyl)amine and 0.210g trialdehyde phloroglucinol to the mixed solution of 12mL 1,3,5-trimethylbenzene and 6mL 1,4-dioxane, dropwise The mixture of 0.5mL 3mol / L glacial acetic acid and 0.5mL 3mol / L phosphoric acid was sonicated for 20min until it was completely dissolved, and reacted under vacuum at 140°C for 48h, and then 5mL N,N-dimethylformamide was added to the reaction solution, and continued After reacting for 24 hours, washing with 1,4-dioxane for 3 times and dichloromethane for 3 times, drying at 60°C for 8 hours, a three-dimensional COFs structure material with ketone groups was obtained.

[0035]Add 50 mg of three-dimensional COFs structural material to 15 mL of water, add 0.5 mL of 3 mol / 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 After drying, the double hydroxyl structure material is obtained.

[...

Embodiment 3

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

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

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Abstract

The invention discloses a novel snowflake-like bionic covalent organic framework COFs photocatalyst and a preparation method thereof. According to the preparation method, firstly, a three-dimensional COFs structure is formed by utilizing a reaction between an amino group and an aldehyde group in raw materials, and a keto group is formed by virtue of enol interconversion to provide a basis for subsequent electrophilic addition; and secondly, a dihydroxyl structure is formed through an electrophilic addition reaction of water molecules to ketone groups, the dihydroxyl structure and carboxyl in amino acid are subjected to a dehydration reaction to form the novel snowflake-shaped bionic COFs material. Pore diameter regulation and control can be further conducted by changing reactant molecules and amino acid types, and the covalence effect of amino lone pair electrons on the snowflake shape and the empty orbital of the promoter Pt is utilized to realize the uniform dispersion of the promoter. Amino acid is introduced into the COFs material, the COFs material is low in cost, easy to obtain and environmentally friendly, and the hydrophilic performance of the snowflake-shaped material is beneficial to accelerating hydrogen production through water photolysis. The porosity, crystallinity and pi-pi conjugated system of the COFs material 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-like biomimetic covalent organic framework COFs photocatalyst and a preparation method thereof. Background technique [0002] With the rapid development of the economy, the problem of sustainable development of human society follows. The problem of excessive consumption of fossil energy is particularly prominent. Energy shortage and environmental problems have become constraints for the sustainable development of human society. Therefore, it is necessary to develop some alternatives. Clean energy alternatives to fossil fuels. Hydrogen energy has been widely concerned as a clean and renewable energy source. Photocatalytic hydrogen production technology may provide abundant clean energy in the future to alleviate the environmental crisis. At present, many inorganic semiconductor materials, including cadmium sulfide and zinc oxide, have been stu...

Claims

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Application Information

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Patent Type & Authority Applications(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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