Non-precious metal-metal organic framework composite material, its preparation method and application
A metal-organic framework, non-precious metal technology, applied to non-precious metal-metal-organic framework composite materials, and its preparation field, can solve the problems of cumbersome catalyst synthesis process, harsh reaction conditions, unfavorable industrial production and the like, and is beneficial to the research of catalytic mechanism. , the preparation is simple, the structure is clear
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Embodiment 1
[0062] Example 1: Synthesis of non-noble metal-MOFs composites
[0063] Synthesis of MOFs material (i.e. UiO-67-BPY): zirconium tetrachloride (25 mg), 2,2'-bipyridine-5,5'-dicarboxylic acid (H 2 BPY, 25mg), benzoic acid (1.1735g) and DMF (10mL) were placed in a polytetrafluoroethylene kettle, ultrasonicated for 10 minutes, sealed, and heated at 120°C for 3 days. After cooling to room temperature, the crystals were collected, washed successively with a large amount of DMF and methanol, and vacuum-dried at 150° C. for 10 hours to obtain a white microcrystalline powder, which was set aside.
[0064] Zn(BF 4 ) 2 ·xH 2 After ultrasonically dissolving O (11 mg) in DMF (2 mL), the solution was injected into a vial containing 100 mg of UiO-67-BPY powder under argon atmosphere, and heated at 45°C overnight. After cooling to room temperature, they were washed three times with DMF and methanol respectively, and then vacuum-dried at 150°C for 10 hours to obtain non-noble metal-MOFs co...
Embodiment 2
[0066] Example 2: Zn-UiO-67-BPY catalyzes the intramolecular hydroamination of 2-(2-phenylethynyl) aniline
[0067] Add catalyst (Zn-UiO-67-BPY prepared in Example 1, 25 mg), 2-(2-phenylethynyl) aniline (10 mg) successively in the pressure-resistant bottle, seal, and go through vacuum-filling argon circulation After three operations, 0.2 mL of ultra-dry methanol was injected under an argon atmosphere, and the reaction was heated at 100° C. for 24 hours. The reaction was cooled to room temperature, methanol was added, centrifuged, and the separated clear liquid was spun to remove the solvent to obtain a crude product, which was separated by column chromatography (the eluent was a mixture of petroleum ether and ethyl acetate) to obtain the final product. The rate is 98%.
[0068] NMR data of the final product: 1 H NMR (400MHz, DMSO-d6): δ11.54(s,1H), 7.88-7.86(m,2H), 7.54-7.30(m,5H), 7.12-6.98(m,2H), 6.91(s, 1H).
Embodiment 3
[0069]Example 3: Zn-UiO-67-BPY catalyzes the intramolecular hydroamination of 2-((4-chlorophenyl)ethynyl)-aniline
[0070] The catalyst (Zn-UiO-67-BPY prepared in Example 1, 25 mg), 2-((4-chlorophenyl) ethynyl)-aniline (11 mg) was added sequentially in the pressure bottle, sealed, and vacuum- After three cycles of argon gas filling, 0.2 mL of ultra-dry toluene was injected under an argon atmosphere, and the reaction was heated at 100° C. for 24 hours. The reaction was cooled to room temperature, toluene was added, centrifuged, and the clear liquid obtained by separation was evaporated to remove the solvent to obtain a crude product, which was separated by column chromatography (the eluent was a mixture of petroleum ether and ethyl acetate) to obtain the final product. The rate is 92%.
[0071] NMR data of the final product: 1 H NMR (400MHz, DMSO-d6): δ11.59(s, 1H), 7.89-7.87(m, 2H), 7.54-7.39(m, 4H), 7.12-7.01(m, 2H), 6.94(s, 1H).
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