Composite catalytic material, preparation method and application thereof in controllable preparation of dihydroxy/dimethylfuran compound
A technology of catalytic materials and polymers, applied in chemical instruments and methods, chemical/physical processes, organic compound/hydride/coordination complex catalysts, etc., can solve complex catalyst preparation process, numerous operation steps, complex composition, etc. Problems, to achieve good industrial application prospects, improve the effect of economic efficiency
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[0047] The preparation method of above-mentioned catalytic material, comprises the steps:
[0048] Preparation of the carrier: mixing the first metal chloride with an organic solvent to obtain a first mixed solution; mixing an organic phosphonic acid ligand with an organic solvent to obtain a second mixed solution; adding the first mixed solution to the second mixed solution , adding triethylamine, reacting, aging, washing, drying and pulverizing the generated precipitate to obtain an amorphous mesoporous metal phosphonic acid polymer carrier;
[0049] Active center loading: Disperse the amorphous mesoporous metal phosphonic acid polymer carrier in the solution containing the second metal chloride, then add NaBH 4 The aqueous solution is reacted, and the generated precipitate is washed, dried and pulverized to obtain an active metal-loaded amorphous mesoporous metal phosphonic acid polymer catalyst.
[0050] In one embodiment, the molar ratio of the first metal chloride, orga...
Embodiment 1
[0066] Add 10mmol of zirconium tetrachloride and 10mmol of biphenyl-4,4-diphosphonic acid ligand to 400mL of dimethylformamide solvent, stir well until completely dissolved; slowly add the zirconium tetrachloride solution to the organic phosphonic acid In the ligand solution, add 60 mmol of triethylamine dropwise to the above mixed solution, continue to stir for 4 hours at room temperature, raise the temperature to 80°C and let it stand for 4 hours; after the solid precipitate is separated by filtration, use dimethylformamide Repeated washing with 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 about 200 mesh to obtain an amorphous mesoporous metal phosphonic acid polymer carrier; Take 1g of amorphous mesoporous metal phosphonic acid polymer carrier and disperse it in 300mL containing CuCl 2 In deionized water, ultrasonically stirred for 30 min and then continued to stir at room te...
Embodiment 2
[0070]Add 10mmol of hafnium tetrachloride and 10mmol of hydroxyethylidene diphosphonic acid ligand into 400mL of dimethylformamide solvent, stir well until completely dissolved; slowly add the hafnium tetrachloride solution into the organic phosphonic acid ligand solution , and then add 60mmol of triethylamine dropwise to the above mixed solution, continue to stir for 4h at room temperature, raise the temperature to 80°C and let it stand for 4h; after the solid precipitate is separated by filtration, it is washed repeatedly with dimethylformamide 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 about 200 meshes to obtain an amorphous mesoporous metal phosphonic acid polymer carrier; take 1g of amorphous The mesoporous metal phosphonic acid polymer support was dispersed in 300mL containing CuCl according to the loading 2 In deionized water, ultrasonically stirred for 30 min and t...
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