Preparation method and application of sulfonic acid functionalized inorganic-organic hybrid polymer catalyst
A technology of sulfonic acid functionalization and organic hybridization, which can be used in organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, organic chemistry, etc. High price and other problems, to achieve good industrial application potential, improve selectivity and yield, and avoid the use of precious metals
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Embodiment 1
[0025] Add 20mmol of zirconium tetrachloride and 20mmol of 3,5-diphosphonophenylsulfonic acid into 400mL of dimethylformamide solvent respectively, and stir until completely dissolved with the assistance of ultrasound; slowly add the zirconium tetrachloride solution into In the 3,5-diphosphonophenylsulfonic acid solution, continue to stir for 5 hours at room temperature, raise the temperature to 80°C and let it stand for 6 hours; after the solid precipitate is separated by filtration, it is washed repeatedly with dimethylformamide and ethanol until Until the presence of chloride ions is no longer detected; vacuum-dry the washed solid precipitate at 80°C for 12 hours, and grind it to 200 mesh to obtain the sulfonic acid functionalized inorganic-organic hybrid polymer catalyst 1, abbreviated as Zr- DPBS-SO 3 H; through NH 3 -TPD, CO 2 -TPD and Py-IR characterization analysis shows that Zr-DPBS-SO 3 The Lewis acidic site content of H is 0.923 mmol / g, the Lewis basic site conte...
Embodiment 2
[0027]Add 15mmol of zirconium tetrachloride and 10mmol of 2,5-diphosphonophenyl-1,4-disulfonic acid into 500mL of dimethylformamide solvent, stir until completely dissolved with the assistance of ultrasound; Slowly add the zirconium chloride solution into the 2,5-diphosphonophenyl-1,4-disulfonic acid solution, continue to stir for 5 hours at room temperature, raise the temperature to 80°C and let it stand for 6 hours; after the solid precipitate is separated by filtration , washed repeatedly with dimethylformamide and ethanol until the presence of chloride ions is no longer detected; the washed solid precipitate was vacuum-dried at 80°C for 12 hours, and ground and crushed to 300 mesh to obtain sulfonic acid functionalized inorganic Organic hybrid polymer catalyst 2, abbreviated as Zr-DPBDS-SO 3 H; through NH 3 -TPD, CO 2 -TPD and Py-IR characterization analysis shows that Zr-DPBDS-SO 3 The Lewis acidic site content of H is 0.857 mmol / g, the Lewis basic site content is 1.42...
Embodiment 3
[0029] Add 20mmol of zirconium tetrachloride and 40mmol of 5-sulfonic acid-1,2,4-benzenetricarboxylic acid into 500mL of dimethylformamide solvent, and stir until completely dissolved with the assistance of ultrasound; the zirconium tetrachloride solution Slowly add to 5-sulfonic acid-1,2,4-benzenetricarboxylic acid solution, continue stirring at room temperature for 5 hours, raise the temperature to 80°C and let it stand for 6 hours; after the solid precipitate is separated by filtration, use dimethyl formaldehyde Repeated washing with amide and ethanol until the presence of chloride ions is no longer detected; vacuum-dry the washed solid precipitate at 80°C for 12 hours, and grind it to 200 mesh to obtain a sulfonic acid functionalized inorganic-organic hybrid polymer catalyst 3, abbreviated as Zr-SBTC-SO 3 H; through NH 3 -TPD, CO 2 -TPD and Py-IR characterization analysis shows that Zr-SBTC-SO 3 The Lewis acidic site content of H is 0.795 mmol / g, the Lewis basic site co...
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