Phosphorus-doped cerium-iron composite oxide catalyst and its preparation method and application
A technology of composite oxides and catalysts, applied in the direction of carbon-based compound preparation, physical/chemical process catalysts, chemical instruments and methods, etc., can solve low conversion rate and/or selectivity, benzaldehyde yield and purity reduction, catalyst Complicated preparation methods and other issues, to achieve the effects of simple preparation methods, improved safety factor, and improved atomic economic benefits
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Embodiment 1
[0052] Preparation of Example 1 phosphorus-doped cerium-iron composite oxide catalyst samples 1-6
[0053] S1. Under magnetic stirring, Ce(NO 3 ) 3 ·6H 2 O, Fe(NO 3 ) 2 9H 2 O and KH 2 PO 4 Dissolve in 200ml deionized water to prepare solution II;
[0054] S2. Under magnetic stirring, use a dropping funnel to add triethylamine dropwise to the above solution II until the pH of the solution is 9; then keep the stirring conditions unchanged, and age in an oil bath at a constant temperature of 90°C for 18 hours;
[0055] S3. Pour the aged suspension into a sand core funnel for suction filtration to obtain a filter cake, fully wash the filter cake with deionized water to neutrality, and then wash with absolute ethanol; after washing, the gained filter cake is Drying at 110 °C for 12 h, grinding, and calcining at 400 °C for 4 h in air atmosphere to obtain Ce 2 FeP X o Y Catalyst samples 1-6.
[0056] Ce(NO 3 ) 3 ·6H 2 O (referred to as cerium salt), Fe (NO 3 ) 2 9H ...
Embodiment 7
[0061] Example 7 Samples 1-6 and comparative sample D1 are used for the performance test of benzyl alcohol selective oxidation reaction
[0062] 1) Set the reaction temperature of the parallel reactors, and control the temperature at the reaction preset temperature of 59-61°C;
[0063] 2) Add 80 mg of catalyst, 0.5 mmol of benzyl alcohol, and 5 ml of toluene as a solvent in the glass tube;
[0064] 3) Put the glass tube containing the reaction mixture into the parallel reactor, and under the air (open) atmosphere, the magnetic sub-stirring (rotating speed 900rpm) continues to react for 10h;
[0065] 4) After the reaction time is up, take out the glass tube, quickly cool it to room temperature with an ice-water bath, draw the reaction solution in the glass tube with a syringe and filter it with a 0.45 micron filter head;
[0066] 5) Quantitative analysis was performed using a Trace 1310 gas chromatograph from Thermo Fisher Scientific Co., Ltd., using an external standard metho...
Embodiment 8
[0077] Embodiment 8: Catalytic cycle experiment of samples 1-6
[0078] 1) The catalyst after completing one catalytic reaction in Example 2 was recovered by centrifugation, washed alternately with ethanol and deionized water for 3 times, and vacuum-dried at 60° C. for 6 hours to obtain a catalyst with a use number of 1, which was used for subsequent Catalytic cycle test.
[0079] 2) Set the reaction temperature of the parallel reactor, and control the temperature at the reaction preset temperature of 60±1°C;
[0080] 3) Then add 80 mg of catalyst, 0.5 mmol of benzyl alcohol, and 5 ml of toluene in the glass tube as a solvent;
[0081] 4) Put the glass tube containing the reaction mixture into the parallel reactor, and in the air (open) atmosphere, the magnetic sub-stirring (rotating speed 900rpm) continued to react for 10h;
[0082] 5) After the reaction time is up, take out the glass tube, quickly cool it to room temperature with an ice-water bath, draw the reaction soluti...
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