Molybdenum carbide-molybdenum oxide catalyst, and preparation method and application thereof
A molybdenum carbide and catalyst technology, which is applied in the field of molybdenum carbide-molybdenum oxide catalyst and its preparation, can solve the problems of high cost and harsh reaction conditions, and achieve the effect of enhancing the activity of metal breaking carbon-carbon bonds and changing the distribution of electronic states
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Embodiment 1
[0054] The embodiment of the present application provides a molybdenum carbide-molybdenum oxide catalyst, the preparation method comprising:
[0055] 1. 10g ammonium paramolybdate (NH 4 ) 6 Mo 7 o 24 4H 2 O was loaded into a 200ml crucible, heated to 500°C in a muffle furnace at a rate of 10°C / min and kept at this temperature for 4h to prepare MoO 3 .
[0056] Get the 2.4000g MoO obtained above 3 Put 150ml / min of 20% CH 4 / H 2 in a quartz tube. Then it was heated from room temperature (RT) to 300°C at a rate of 5°C / min, then increased from 300°C to 700°C at a rate of 1°C / min, and kept at 700°C for 2 h. Cooling to room temperature yields Mo 2 C precursor. Take Mo 2 C precursor in 1% O at 15ml / min 2 / Ar gas passivation at 350°C for 2 hours and recorded as MoO x -Mo 2 c.
[0057] 2. Take 6.5g of MoO prepared in step 1 x -Mo 2 C was added to 3.5135ml of ruthenium trichloride solution containing 3.7wt% Ru, soaked for 10h, dried at 100°C for 10h, calcined at 350°C ...
Embodiment 2
[0059] The embodiment of the present application provides a molybdenum carbide-molybdenum oxide catalyst, the preparation method comprising:
[0060] 1. 10g ammonium paramolybdate (NH 4 ) 6 Mo 7 o 24 4H 2 O was loaded into a 200ml crucible, heated to 500°C in a muffle furnace at a rate of 10°C / min and kept at this temperature for 4h to prepare MoO 3 .
[0061] Get the 0.8000g MoO obtained above 3 NH at 150mL / min 3 Under the atmosphere, the temperature was programmed to rise to 700°C at 5°C / min and kept for 2h for ammoniation treatment. Cool to room temperature. Switch the reaction atmosphere to 20% CH at 150mL / min 4 / H 2 Mix the atmosphere, set the temperature rise program at 5°C / min to 700°C and keep it for 2h. Cool down to room temperature to obtain a MoC catalyst sample. Take the MoC catalyst sample at 15ml / min1%O 2 / Ar atmosphere at 5°C / min to 350°C and keep it for 2h as MoO x -MoC.
[0062] 2. Take 6.5g of MoO prepared in step 1 x -Mo 2 C was added to 3.5...
Embodiment 3
[0098] The embodiment of the present application provides an activity evaluation test using Cat1-Cat12 to catalyze the hydrodeoxygenation reaction of sorbitol. The method includes:
[0099] This embodiment uses Cat1~Cat12 as the activity evaluation of the catalyst: it is carried out in a continuous high-pressure fixed-bed reactor, and the Cat1~Cat12 catalyst loading is 5g, H 2 The flow rate is 30ml / min, the solution injection flow rate is 0.02ml / min, 20wt% sorbitol solution, the reaction pressure is 4MPa, and the reaction temperature is 250°C. The conversion rate of sorbitol was detected by HPLC (Waterse2695), the gas phase product was detected by online gas chromatography flame ionization detector (FID) and thermal conductivity detector (TCD), and the water phase and oil phase collected at 30 ° C were detected by GC ( Shimadzu GC-2030Pro). The test results are shown in Table 1.
[0100] Table 1 Activity evaluation results of different catalysts for sorbitol aqueous phase hy...
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