Clay load palladium catalyst and preparation method thereof
A palladium catalyst, a catalyst technology, which is applied in the directions of catalyst activation/preparation, carbon-based compound preparation, chemical instruments and methods, etc., can solve the problems of high calcination temperature, expensive reagents, limited industrial application, etc., and achieves low energy consumption, simple composition, Simple preparation method
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Embodiment 1
[0020] Weigh 0.444g PdCl 2 Add 20mL of distilled water, then add 0.49g of concentrated hydrochloric acid, stir to dissolve, then dilute to 50mL with distilled water to make H2O with a concentration of 0.05M 2 PdCl 4 solution. Pipette the above H 2 PdCl 4 Add 2 mL of the solution into 25 mL of distilled water, add 1 g of organoclay (montmorillonite modified by alkyl quaternary ammonium surfactant exchange) into the above solution, and stir at room temperature for 10 min. The above mixture was filtered and washed, and then the filter cake was dried in an oven at 60°C for 24 hours. After the dried solid was ground into powder, freshly prepared 2.0wt% NaBH was added dropwise 4 solution until no more bubbles are produced. After the reaction, the above mixture was filtered, washed with a large amount of distilled water, and washed with 1mol / LAgNO 3 Check whether the chloride ion is removed, and add AgNO to the filtrate 3 The solution no longer formed a white precipitate. Th...
Embodiment 2
[0025] For the 1.0 wt% Pd-DK1-RE catalyst prepared in the above column. Pipette 1 mL (9.7 mmol) of benzyl alcohol, put it into a 50 mL glass flask, then add 10 mL of toluene, then weigh 0.05 g of catalyst and 0.1 g of K 2 CO 3 into the above mixture. At the beginning of the reaction, oxygen was passed into the reaction liquid below the liquid level through the gas guide tube, and the flow rate of oxygen was controlled at 25 mL / min. The reaction temperature was controlled at 100±1°C by an oil bath. After reacting for 2 hours, the temperature was lowered to room temperature, 0.2 g of naphthalene was added as an internal standard, and after shaking well, the catalyst was centrifuged, and the liquid product was analyzed by a Grockway GC7800 gas chromatograph. The catalytic reaction results are listed in Table 2. The catalytic performance of the catalyst remained basically unchanged after 3 cycles.
[0026] Table 2 Table 11.0wt%Pd / DK1-RE Catalyst Selective Oxidation Performanc...
Embodiment 3
[0029] For the 1.0 wt% Pd-DK1-RE catalyst prepared in the above example. Pipette 5 mL (48.5 mmol) of benzyl alcohol and put it into a 50 mL glass flask, then weigh 0.1 g of catalyst and put it into the above mixed solution. At the beginning of the reaction, oxygen was passed into the reaction liquid below the liquid level through the gas guide tube, and the flow rate of oxygen was controlled at 25 mL / min. The reaction temperature was controlled at 100±1°C by an oil bath. After reacting for 2 hours, the temperature was lowered to room temperature, 0.2 g of naphthalene was added as an internal standard, and after shaking well, the catalyst was centrifuged, and the liquid product was analyzed by a Grockway GC7800 gas chromatograph. The results of the catalytic reactions are listed in Table 3.
[0030] Table 31.0wt%Pd / DK1-RE Catalyst Selective Oxidation Performance of Benzyl Alcohol
[0031] Reaction time (h)
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