Sulfur-tolerant catalyst suitable for methanation synthesis of gas slurry reactor and preparation method and application
A catalyst and slurry bed technology, which is applied in the field of synthesis gas slurry bed methanation sulfur-resistant nickel-based catalyst and its preparation, can solve the problems of easy deactivation and low sulfur tolerance of the catalyst, and achieve increased low-temperature activity and good performance. Reactivity, effect of increasing specific surface area
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Embodiment 1
[0027] ·At 15°C, the stirring speed is 60r / min, the catalyst composition is Ni:Mo mass ratio 5:20, 2.478g Ni(NO 3 ) 2 ·6H 2 O and 9.694g of Mo(NO 3 ) 3 ·5H 2 Dissolve O in 10ml of water to make a mixed solution, impregnate and stir for 8 hours, continue to stand for 5 hours, and then solvent to a viscous solution at 50°C;
[0028]Drying and roasting: put the viscous solution in an oven and dry at 80°C for 24h, grind the dried powder and place it in a muffle furnace and roast at 400°C for 5h to obtain NiO-Mo 2 o 3 Prebody;
[0029] Hydrogen reduction: NiO-Mo 2 o 3 The precursor body is ground to 40-60 mesh, and the volume composition is 5%H 2 with 95%N 2 , in a mixed atmosphere with a flow rate of 100mL / min, using two-stage temperature programming control, the temperature was raised from room temperature to 350°C at a rate of 3°C / min, and then raised to 600°C at a rate of 2°C / min for 6 hours. Ni-Mo (Ni:Mo mass ratio 5:20) catalyst was obtained after reduction.
[00...
Embodiment 2
[0032] ·At 25°C, the stirring speed is 150r / min, the catalyst composition is Ce:W mass ratio 30:5, 9.297g Ce(NO 3 ) 3 ·6H 2 O and 1.251g of W(NO 3 ) 3 ·5H 2 O was dissolved in 15ml of water to make a mixed solution, impregnated and stirred for 36h, and then left to stand for 12h, and then dissolved at 90°C to a viscous solution.
[0033] ·Drying and roasting: put the viscous solution in an oven and dry at 70°C for 36h, grind the dried powder and place it in a muffle furnace for 8h at 350°C to get the Ce-W precursor.
[0034] Hydrogen reduction: grind the Ce-W precursor to 60-80 mesh, and the volume composition is 10%H 2 with 90%N 2 , in a mixed atmosphere with a flow rate of 50mL / min, two-stage temperature programming control was used to raise the temperature from room temperature to 450°C at a rate of 5°C / min, and then to 700°C at a rate of 3°C / min for 1 hour. Ce-W (Ce:W mass ratio is 30:5) catalyst was obtained after reduction.
[0035] The catalyst prepared in this ...
Embodiment 3
[0037] ·At 40°C, the stirring speed is 200r / min, the catalyst composition is Fe:V mass ratio 1:40, 0.723g Fe(NO 3 ) 3 9H 2 O and 9.186 g of NH 4 VO 3 Dissolve in 15ml of water to make a mixed solution, impregnate and stir for 2h, continue to stand for 1h, and then solvent to a viscous solution at 80°C.
[0038] ·Drying and roasting: put the viscous solution in an oven and dry at 150°C for 4 hours, grind the dried powder and place it in a muffle furnace and roast at 600°C for 1 hour to obtain the Fe-V precursor.
[0039] Hydrogen reduction: grind the Fe-V precursor to 80-100 mesh, and the volume composition is 15%H 2 with 85%N 2 , in a mixed atmosphere with a flow rate of 140mL / min, using two-stage temperature programming control, the temperature was raised from room temperature to 400°C at a rate of 10°C / min, and then raised to 650°C at a rate of 4°C / min for 10 hours. Fe-V (Fe:V mass ratio of 1:40) catalyst was obtained after reduction.
[0040] The catalyst prepared in...
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