A kind of terbium organic framework complex and preparation method thereof
A technology of organic frameworks and complexes, applied in the field of terbium complexes with luminescent properties and its preparation, achieving the effects of good crystal quality, simple preparation method, and high yield
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Embodiment 1
[0021] Embodiment 1. Weigh 0.1mmol H 3 L with 0.15mmolTb(NO 3 ) 3 ·6H 2 O was added to a 15ml polytetrafluoroethylene tube, and 5ml DMF was added, and stirred at room temperature for 30 minutes. The polytetrafluoroethylene tube was sealed in a stainless steel reaction kettle, the temperature was controlled at 120°C and heated for 72 hours, and the temperature was naturally lowered. Colorless blocky crystals were precipitated overnight, washed and dried in vacuum. The yield of the obtained terbium complex was 84%.
[0022] Structure determination of terbium organic framework complexes:
[0023] Select a single crystal with a suitable size under a microscope, and use X-ray diffraction to monochromatize Mo-Kα rays through a graphite monochromator with a Bruker Smart Apex II detector, scan mode ω, and collect data at a temperature of 293K. All diffraction data were subjected to semi-empirical absorption correction using the SADABS program after SAINT reduction. The crystal st...
Embodiment 2
[0029] Embodiment 2. Weigh 0.1mmol H 3 L with 0.15mmolTb(NO 3 ) 3 Add to a 15ml Teflon tube and add 5ml H 2 O, stirred at room temperature for 30 minutes. The polytetrafluoroethylene tube was sealed in a stainless steel reaction kettle, and after heating at 120°C for 72 hours, the temperature was naturally lowered, and no crystals were precipitated overnight, and a large amount of white powder was obtained.
Embodiment 3
[0030] Embodiment 3. Weigh 0.1mmol H 3 L with 0.15mmolTb(NO 3 ) 3 Add to a 15ml polytetrafluoroethylene tube, and add 5ml of H at a volume ratio of 1:1 2A mixed solvent of O and DMF was stirred at room temperature for 30 minutes. Seal the polytetrafluoroethylene tube in a stainless steel reaction kettle, heat it at 120°C for 72 hours, cool down naturally, and precipitate colorless blocky crystals overnight, wash them, and dry them in vacuum. was 43%.
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