Photosensitive covalent organic framework material as well as preparation method and application thereof
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A covalent organic framework and photosensitivity technology, applied in the field of preparation of covalent organic framework materials, can solve the problems of cumbersome operation, harsh synthesis conditions and long reaction time.
Active Publication Date: 2021-07-06
YUNNAN UNIV
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In the above-mentioned synthesis process, the operation is very cumbersome, the synthesis conditions are relatively harsh, the reaction time is long, and mass production is not possible.
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[0038] The invention provides a method for preparing a photosensitive covalent organic framework material, comprising the following steps:
[0039] Mix 4,7-bis(4-aminophenyl)-2,1,3-benzothiadiazole, trialdehyde phloroglucinol and a solvent for condensation reaction to obtain the photosensitive covalent organic framework Material.
[0040] In the present invention, unless otherwise specified, the raw materials used are all preferably commercially available products.
[0041]In the present invention, the molar ratio of 4,7-bis(4-aminophenyl)-2,1,3-benzothiadiazole to trialdehyde phloroglucinol is preferably (1-10): 1, more preferably 3:2.
[0042] In the present invention, the solvent is preferably a mixture of o-dichlorobenzene, n-butanol and aqueous acetic acid; the concentration of the aqueous acetic acid is preferably 6mol / L; The volume ratio is preferably 1:(0.25-4):(0.1-0.3), more preferably 1:1:0.2.
[0043] In the present invention, the amount ratio of the solvent to...
Embodiment 1
[0058] A method for preparing a photosensitive COFs material, comprising the steps of:
[0059] Add organic monomer 4,7-bis(4-aminophenyl)-2,1,3-benzothiadiazole (238 mg, 0.75 mmol) and trialdehyde phloroglucinol ( 105mg, 0.5mmol), add 10mL o-dichlorobenzene, 10mL n-butanol, 2mL 6mol / L acetic acid aqueous solution, disperse evenly in 100W ultrasonic for 5min, then carry out condensation reaction at 25℃, 0.101MPa, 300rpm for 3 days .
[0060] The obtained condensation reaction feed liquid was centrifuged (12000 rpm), and the obtained precipitate was washed 5 times with tetrahydrofuran and 3 times with acetone, and vacuum-dried at 120° C. for 1 day to obtain a photosensitive COFs material.
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Abstract
The invention belongs to the technical field of preparation of covalent organic framework materials, and provides a photosensitive covalent organic framework material as well as a preparation method and application thereof. The organic monomers 4, 7-bis (4-aminophenyl)-2, 1, 3-benzothiadiazole and trialdehyde phloroglucinol are connected through a covalent bond at room temperature to form a photosensitive covalent organic framework material (COFs), and the photosensitive COFs material has an enol type structure and a ketone type structure at the same time, has excellent photosensitive property, and can generate I-type and II-type active oxygen at the same time under the irradiation of visible light. The preparation method only needs one-step simple reaction, the synthesis method is simple and convenient, the synthesis condition is mild, the consumed time is short, and large-scale synthesis is facilitated. Furthermore, the preparation method provided by the invention is easy to separate and purify, and the photosensitive COFs material can be obtained only by washing with an organic solvent.
Description
technical field [0001] The invention relates to the technical field of preparation of covalent organic framework materials, in particular to a photosensitive covalent organic framework material and its preparation method and application. Background technique [0002] Photosensitizer (photosensitizer, abbreviated as PS), also known as photoinitiator, is a kind of substance that can absorb radiation energy and undergo photochemical changes after excitation, thereby generating free radicals or cations. Among them, reactive oxygen species (ROS) induced by photosensitizers are considered to be a class of clean and efficient oxidants. According to their production pathways, they can be divided into two types: type I ROS and type II ROS. Among them, type I ROS are free radicals directly generated by electron-excited photosensitizers (PS) from substrates to obtain electrons or hydrogen atoms, including superoxide radicals (O 2 ·- ), hydroxyl radicals (·OH) and hydrogen peroxide (...
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