Novel porous titanium metal-organic framework material for visible-light photocatalytic hydrogen generation and preparation method thereof
An organic framework, photocatalytic technology, applied in catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc., to achieve novel structure, good absorption, and good stability.
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Embodiment 1
[0024] (1) the desired tricarboxylic acid organic ligand 4,4',4"-tricarboxylic acid triphenylamine (H 3 TCA) was added to a 25mL polytetrafluoroethylene hydrothermal reaction kettle, 5mL N,N-dimethylformamide (hereinafter referred to as DMF) was added, and ultrasonically dissolved to obtain a clear solution;
[0025] (2) Add isopropyl titanate to the clarified solution obtained in step (1) according to the molar ratio of isopropyl titanate to tricarboxylic acid organic ligand 1:1, stir well, and place in a constant temperature oven at 180°C After 24 hours of reaction, during the hydrothermal reaction, the carboxylic acid oxygen of the organic ligand and the titanium ion rearrangement reaction became Ti 6 o 6 metal clusters, and carry out a coordination reaction with organic ligands to obtain a suspension after hydrothermal reaction;
[0026] (3) Naturally cool the hydrothermally reacted suspension obtained in step (2) to room temperature, centrifuge and wash, wash with DMF a...
Embodiment 2
[0028] (1) the required tribasic carboxylic acid organic ligand 1,3,5-three (4-carboxyphenyl) benzene (H 3 BTB) was added to a 25mL polytetrafluoroethylene hydrothermal reaction kettle, and 5mL N,N-dimethylformamide (hereinafter referred to as DMF) was added, and ultrasonically dissolved to obtain a clear solution;
[0029] (2) Add isopropyl titanate to the clarified solution obtained in step (1) according to the molar ratio of isopropyl titanate to tricarboxylic acid organic ligand 1:1.5, stir well, and place in a constant temperature oven at 180°C After 18 hours of reaction, during the hydrothermal reaction, the carboxylic acid oxygen of the organic ligand and the titanium ion rearrangement reaction become Ti6O6 metal clusters, and carry out a coordination reaction with the organic ligand to obtain a suspension after the hydrothermal reaction;
[0030] (3) Naturally cool the hydrothermally reacted suspension obtained in step (2) to room temperature, centrifuge, wash with DMF...
Embodiment 3
[0032] (1) the desired tricarboxylic acid organic ligand H 3Add BTCA to a 25mL polytetrafluoroethylene hydrothermal reaction kettle, add 5mL N,N-dimethylformamide (hereinafter referred to as DMF), and ultrasonically dissolve it fully to obtain a clear solution;
[0033] (2) Add isopropyl titanate to the clarified solution obtained in step (1) according to the molar ratio of isopropyl titanate to tricarboxylic acid organic ligand 1:2, stir well, and place in a constant temperature oven at 180°C After 30 hours of reaction, during the hydrothermal reaction, the carboxylic acid oxygen of the organic ligand and the titanium ion rearrangement reaction became Ti 6 o 6 metal clusters, and carry out a coordination reaction with organic ligands to obtain a suspension after hydrothermal reaction;
[0034] (3) Naturally cool the hydrothermally reacted suspension obtained in step (2) to room temperature, centrifuge and wash, wash with DMF and methanol for 5 times, then reflux with DMF at...
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