A kind of monolithic extruded nickel-based catalyst and its preparation method and application
A nickel-based catalyst, integral extrusion technology, applied in chemical instruments and methods, physical/chemical process catalyst, metal/metal oxide/metal hydroxide catalyst, etc. It can solve the problems of machine power consumption and large pressure drop in the reactor bed, so as to achieve the effects of easy preparation and application, improved high temperature hydrothermal stability, and reduced power consumption.
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Embodiment 1
[0044] (1) Dry ball mill: Weigh γ-Al with particle size less than 10 mesh (0.25 mm) 2 o 3 860g of powder and 125g of ZrO 2 , 25g of SiO 2 Mixing and dry milling with a high-energy ball mill for 16 hours, the particle size of the mixed powder was measured to be 3.5 μm.
[0045] (2) Preparation of precursor solution: Ni(NO 3 ) 2 ·6H 2 O and La(NO 3 ) 3 ·6H 2 O is the precursor, Ni(NO 3 ) 2 solution and La(NO 3 ) 3 solution. Measure 5.00L Ni(NO 3 ) 2 solution and 0.31L La(NO 3 ) 3 The solution is ready for use.
[0046] (3) Preparation of extrusion aids: Measure 2.75L of 1M aluminum sol, 0.6L of 1M zirconium sol, and 0.4L of 1M silica sol as inorganic binder; 60g of methyl cellulose as organic binder; 50g Glycerin is used as a plasticizer; 50g of polyethylene glycol (PEG-4000) is used as a lubricant.
[0047] (4) Kneading process: move the certain ratio of extrusion aids obtained in step (3) together with the mixture obtained in steps (1) and (2) into a kneader...
Embodiment 2
[0052] (1) Dry ball mill: Weigh γ-Al with particle size less than 10 mesh (0.25 mm) 2 o 3 700g of powder and 125g of ZrO 2 Mixing and dry ball milling with a high-energy ball mill for 12 hours, the particle size of the mixed powder was measured to be 5.2 μm.
[0053] (2) Preparation of precursor solution: Ni(NO 3 ) 2 ·6H 2 O and La(NO 3 ) 3 ·6H 2 O is the precursor, Ni(NO 3 ) 2 solution and La(NO 3 ) 3 solution. Measure 9.33L Ni(NO 3 ) 2 solution and 0.31L La(NO 3 ) 3 The solution is ready for use.
[0054] (3) Preparation of extrusion aids: Measure 2.75L of 1M aluminum sol, 0.81L of 1M zirconium sol as inorganic binder; 50g of hydroxypropyl cellulose as organic binder; 30g of glycerol and 20g of Epoxidized linseed oil was used as a plasticizer; 50 g of scallop powder was used as a lubricant.
[0055] (4) The kneading process is the same as the step (4) of Example 1.
[0056] (5) Extrusion process is the same as embodiment 1 step (5).
[0057] (6) Drying an...
Embodiment 3
[0060] Step (1)-step (4) are the same as in Example 1.
[0061] (5) Extrusion process: Extrude the catalyst green body obtained in step (4) with an extruder and cut it into a cross-sectional shape of 40 × 40mm (length × width), a height of 60mm, and an interior of 400 holes per square inch. A catalyst intermediate with holes (400cpsi) and a through-hole wall thickness of 0.4mm.
[0062] (6) Drying and roasting: same as step (6) of Example 1. Obtain embodiment 3 catalyst, composition is 35.7%NiO-4.8%La 2 o 3 -9.5%ZrO 2 -2.3% SiO2 2 -47.7% γ-Al 2 o 3 (400cpsi).
[0063] The above catalyst is loaded into the middle of the methanation reactor, with 10vol.%H 2 -90vol.%N 2 The mixed gas is reduced at 500°C for 5 hours, and then the pressure is 3.0MPa, the temperature is 300°C, and the space velocity is 10000h -1 、H 2 / (3CO+4CO 2 ) was evaluated under the condition that the molar ratio was 1.13. Under the reaction conditions, the CO conversion rate was 99.2%, and the CO ...
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