Sulfur tolerant catalyst suitable for slurry bed methanation, its preparation method and application
A catalyst and slurry bed technology, which is applied in the field of synthetic methane catalyst and preparation, can solve the problems of easy deactivation and low sulfur tolerance of the catalyst, and achieve the effects of increasing low-temperature activity, good reactivity, and improving utilization rate
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[0028] Example 1
[0029] ·Carrier pretreatment: 40~60 mesh, specific surface area is 100m 2 / g of γ-Al 2 O 3 Calcined at 400℃ for 2h; impregnation: at 20℃, stirring speed 60r / min, catalyst composition is as follows: Ni: Mo: γ-Al 2 O 3 The mass percentage of 20%: 15%: 65% preparation. 9.908g Ni(NO 3 ) 2 ·6H 2 O and 5.816g of Mo(NO 3 ) 3 ·5H 2 O is dissolved in 10ml water to make a mixed solution, and 6.5g of the roasted carrier γ-Al 2 O 3 Add the above solution to soak and stir for 12h, continue to stand for 4h, and then solvent to a viscous solution at 50°C.
[0030] ·Drying and roasting: Put the impregnated sample in an oven and dry at 70℃ for 12h. Grind the dried powder and place it in a muffle furnace and roast it at 350℃ for 6h to obtain NiO-Mo 2 O 3 / γ-Al 2 O 3 Forebody
[0031] ·Hydrogen reduction: NiO-Mo 2 O 3 / γ-Al 2 O 3 The front 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 90mL / min, two-stage tempe...
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[0033] Example 2
[0034] ·Carrier pretreatment: 60~80 mesh, specific surface area is 150m 2 / g of SiO 2 Roasting at 450℃ for 3h;
[0035] Impregnation: at 25℃, stirring speed 30r / min, catalyst composition according to Ce: W: SiO 2 The mass percentage of 10%: 15%: 75% preparation. Add 3.099g of Ce(NO 3 ) 3 ·6H 2 O and 3.752g of W (NO 3 ) 3 ·5H 2 O is dissolved in 15ml water to make a mixed solution, and 7.5g of the roasted carrier SiO 2 Add the above solution to soak and stir for 6h, continue to stand for 12h, and then solvent to a viscous solution at 70°C.
[0036] ·Drying and roasting: Put the impregnated sample in an oven and dry at 90℃ for 12h. Grind the dried powder and put it in a muffle furnace and roast it at 400℃ for 6h to obtain Ce-W / SiO 2 Forebody.
[0037] ·Hydrogen reduction: Ce-W / SiO 2 The forebody is ground to 60~80 mesh, the volume composition is 10%H 2 With 90% N 2 , In a mixed atmosphere with a flow rate of 110mL / min, using two-stage temperature program control to in...
Example Embodiment
[0039] Example 3
[0040] ·Carrier pretreatment: 80~100 mesh, specific surface area is 200m 2 / g of MgO is roasted at 450℃ for 6h;
[0041] Impregnation: At 30°C, the stirring speed is 300r / min, and the catalyst composition is prepared according to the mass percentage of Fe:V:MgO 2%:0.5%:97.5%. 1.447g of Fe(NO 3 ) 3 ·9H 2 O and 0.115g of NH 4 VO 3 Dissolve it in 20ml of water to make a mixed solution, add 9.75g of the roasted carrier MgO to the above solution to soak and stir for 36h, continue to stand for 1h, and then solvent to a viscous solution at 80°C.
[0042] ·Drying and roasting: Put the impregnated sample in an oven at 100°C for 20h, ground the dried powder in a muffle furnace and roast at 450°C for 6h to obtain Fe-V / MgO precursor.
[0043] ·Hydrogen reduction: Grind the Fe-V / MgO 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 130mL / min, two-stage temperature program control is used to increase the tempe...
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