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 the above-mentioned catalytic material includes the following 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 , And then add triethylamine, after the reaction, 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, and then add NaBH 4 The resulting precipitate is washed, dried and pulverized to obtain an active metal-supported amorphous mesoporous metal phosphonic acid polymer catalyst.
[0050] In one embodiment, the molar ratio of the first metal chloride, organic phosp...
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[0065] Example 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 60mmol of triethylamine dropwise to the above mixed solution, continue to stir at room temperature for 4h, warm up to 80℃ and let stand for 4h; after the solid precipitate is separated by filtration, use dimethylformamide Repeated washing with ethanol until no chloride ion is detected; vacuum drying the washed solid precipitate at 80°C for 12 hours, grinding and pulverizing it to about 200 meshes 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 according to the loading amount 2 In deionized water, ultrasonically stirred for 30 minutes and then continue ...
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[0069] Example 2
[0070] Add 10mmol of hafnium tetrachloride and 10mmol of hydroxyethylidene diphosphonic acid ligand to 400mL of dimethylformamide solvent, stir thoroughly until completely dissolved; slowly add the hafnium tetrachloride solution to the organic phosphonic acid ligand solution , And then add 60mmol of triethylamine dropwise to the above mixed solution, continue to stir at room temperature for 4 hours, warm to 80 ℃ and stand for 4 hours; the solid precipitate is separated by filtration and washed repeatedly with dimethylformamide and ethanol Until the presence of chloride ions is not detected; the washed solid precipitate is vacuum dried at 80°C for 12 hours, and then ground and crushed to about 200 meshes to obtain an amorphous mesoporous metal phosphonic acid polymer carrier; take 1 g of amorphous The mesoporous metal phosphonic acid polymer carrier is dispersed in 300mL containing CuCl according to the loading amount 2 In deionized water, ultrasonically stirred...
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