A kind of supported PD catalyst and its preparation method for benzyl alcohol oxidation synthesis benzaldehyde under solvent-free system
A technology of oxidative synthesis and catalyst, applied in catalyst activation/preparation, preparation of organic compounds, preparation of carbon-based compounds, etc., can solve environmental problems
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Embodiment 1
[0025](1) Take 0.2 parts of NOMC samples to 10 parts by mass of deionized water, ultrasonic 30min;
[0026](2) Take a PDCL under stirring2The dilute solution (controlled its PD accounting for 1% of the mass percentage of NOMC), continued to be 30 min, stirred for 2 h;
[0027](3) Add an excess NABH to the mixed liquid4Dilute solution. The mixture was filtered and washed several times, dried at 40 ° C to give a catalyst to be 1 pd / NOMC.
[0028](4) Put 100 parts by mass of benzyl alcohol and 1 pd / NOMC catalyst into the flask, oxygen (30 ml of flow rate)-1), Reacting at 90 ° C for 4 h;
[0029](5) Centrifugation of the catalyst after the reaction was completed. The product was analyzed by gas chromatography, and the yield of benzaldehyde was 60%, and the selectivity was greater than 99%.
Embodiment 2
[0031](1) Take 0.2 parts of NOMC sample to disperse 20 parts by mass of deionized water, ultrasonic 30min;
[0032](2) Take a PDCL under stirring2The dilute solution (controlled its PD accounting for 2% of the mass percentage of NOMC), continuing to ultrason for 30 min, stirred for 2 h;
[0033](3) Add an excess NABH to the mixed liquid4Dilute solution. The mixture was filtered and washed with water, dried at 60 ° C to give a catalyst to be 2 pd / NOMC.
[0034](4) 100 parts by mass of benzyl alcohol and 1 part of 2 pd / NOMC catalyst are placed in a flask, and oxygen (flow rate 30ml min)-1), Reacting at 90 ° C for 4 h;
[0035](5) Centrifugation of the catalyst after the reaction was completed. The product was analyzed by gas chromatography, and the yield of benzaldehyde was 75%, and the selectivity was greater than 99%.
Embodiment 3
[0037](1) Take 0.2 parts by mass of NOMC samples to disperse 30 parts by mass of deionized water, ultrasonic 30min;
[0038](2) Take a PDCL under stirring2The dilute solution (controlled the mass percentage of the NOMC of NOMC), continued to ultrason for 30 min, stirred for 2 h;
[0039](3) Add an excess NABH to the mixed liquid4Dilute solution. The mixture was filtered and washed with water, dried at 80 ° C to give a catalyst to be 3 pd / NOMC.
[0040](4) 100 parts by mass of benzyl alcohol and 1 part of 3 pd / NOMC catalyst were placed in a flask, and an oxygen (flow rate 30 ml min)-1), Reacting at 90 ° C for 4 h;
[0041](5) Centrifugation of the catalyst after the reaction was completed. The product was analyzed by gas chromatography, and the yield of benzaldehyde was 85%, and the selectivity was greater than 99%.
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