Zirconium-molybdenum oxide catalyst for methane oxidation to synthesize formaldehyde and its preparation method
A methane oxidation and catalyst technology, applied in the chemical industry, can solve the problems of insufficient activity of lattice oxygen and high reaction temperature, and achieve the effects of good mechanical strength, simple preparation method, high selectivity and yield of formaldehyde
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Embodiment 1
[0017] Calculate the required raw material ammonium molybdate ((NH 4 ) 6 Mo 7 o 24 4H 2 O, Tianjin Chemical Reagent Factory, the amount of analytically pure), be made into the ammonium molybdate aqueous solution that concentration is 0.13g / mL. Add 10.0mL of ammonium molybdate aqueous solution with a concentration of 0.13g / mL to 2.7g of zirconia powder with a particle size of 18nm, dry at 110°C for 8 hours, and bake at 600°C for 10 hours to make a catalyst (ZrO 2 ) 0.63 (Zr(MoO 4 ) 2 ) 0.36 (MoO 3 ) 0 . Zr(MoO 4 ) 2 The particle size is 35nm. Then, the catalyst was ground for 4 hours, pressed under 1.5MPa pressure, and sieved into 40-mesh particles for future use. The prepared catalyst is used in the selective oxidation of methane to formaldehyde. The reaction is carried out in a reaction gas ratio of CH 4 / O 2 / N 2 =10 / 1 / 3, space velocity 12000ml / (g.cat).h -1 , under the conditions of 5.0MPa pressure and 400°C reaction temperature. The catalyst consumption ...
Embodiment 2
[0019] Ammonium molybdate ((NH 4 ) 6 Mo 7 o 24 4H 2 O, Tianjin Chemical Reagent Factory, analytically pure) aqueous solution was added to 3.0 g of zirconia powders with a particle size of 16 nm, dried at 120° C. for 6 hours, and calcined at 550° C. for 11 hours to make a catalyst (ZrO 2 ) 0.74 (Zr(MoO 4 ) 2 ) 0.25 (MoO 3 ) 0.01 . Zr(MoO 4 ) 2 The particle size is 30nm. Then, the catalyst was ground for 4 hours, 180Kg / cm 2 Press to form and screen 30-mesh granules for future use. The prepared catalyst is used in the selective oxidation of methane to formaldehyde. The reaction is carried out in a reaction gas ratio of CH 4 / O 2 / N 2 =10 / 1 / 3, space velocity 12000ml / (g.cat).h -1 , a pressure of 5.0MPa, and a reaction temperature of 380°C. The catalyst consumption is 0.5g. Analysis of the reaction tail gas showed that the methane conversion rate was 3.3%, the formaldehyde selectivity was 53.8%, and the formaldehyde yield was 1.8%.
Embodiment 3
[0021] Ammonium molybdate ((NH 4 ) 6 Mo 7 o 24 4H 2 O, Tianjin Chemical Reagent Factory, analytically pure) aqueous solution joins 1.3g superfine zirconium dioxide (ZrO 2 ) powder, dried at 100°C for 9 hours, and calcined at 650°C for 9 hours to make a catalyst (ZrO 2 ) 0.38 (Zr(MoO 4 ) 2 ) 0.20 (MoO 3 ) 0.42 . Zr(MoO 4 ) 2 The particle size is 44nm. Then, the catalyst was ground for 5 hours, 190Kg / cm 2 Press to form and screen 20-mesh granules for future use. The prepared catalyst is used in the selective oxidation of methane to formaldehyde. The reaction is carried out in a reaction gas ratio of CH 4 / O 2 / N 2=10 / 1 / 3, space velocity 12000ml / (g.cat).h -1 , under the conditions of 5.0MPa pressure and 400°C reaction temperature. Catalyst consumption 0.5g. Analysis of the reaction tail gas showed that the methane conversion rate was 7.0%, the formaldehyde selectivity was 36.0%, and the formaldehyde yield was 2.5%.
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