CN105289616A - Carbon dioxide methanation catalyst (Ni/CexZr(1-x)O2) and preparation method thereof - Google Patents

Carbon dioxide methanation catalyst (Ni/CexZr(1-x)O2) and preparation method thereof Download PDF

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CN105289616A
CN105289616A CN201510739501.6A CN201510739501A CN105289616A CN 105289616 A CN105289616 A CN 105289616A CN 201510739501 A CN201510739501 A CN 201510739501A CN 105289616 A CN105289616 A CN 105289616A
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catalyst
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尚兴付
汪学广
聂望欣
邓蒂固
丁伟中
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上海大学
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Abstract

The invention discloses a carbon dioxide methanation catalyst (Ni/CexZr(1-x)O2) and a preparation method thereof. The preparation method comprises the following steps: (a) adding a certain amount of nickel nitrate, a certain amount of cerium nitrate and a certain amount of zirconium nitrate into 50ml of deionized water to prepare a mixed solution with the content of Ni being 10-40wt.% in the catalyst (Ni/CexZr(1-x)O2); (b) transferring the prepared mixed solution into a thermostat water bath pan at 80 DEG C, uniformly stirring, quickly pouring a 100ml of2 mol/Lsal volatile solution into the mixed solution, stirring, heating, drying at a constant temperature, and then acquiring the powder; (c) roasting the powder after being dried for 5h in a muffle furnace by increasing the room temperature to 500 DEG C at a heating rate of 2 DEG C/min, and then putting the powder after being roasted into a steel moldfor extruding and forming, breaking and sieving, thereby acquiring the grains with the grain sizes being 40-60 meshes; and(d) reducing for 2h at the temperature being 400 DEG C in a hydrogen atmosphere, thereby acquiring the Ni/CexZr(1-x)O2 catalyst. The catalyst prepared by adopting the preparation method has relatively high catalytic activity, selectivity and stability at 250-400 DEG C. The preparation method is simple, easy to operate and low in cost.

Description

A kind of carbon dioxide methanation Ni/Ce xzr 1-xo 2catalysts and its preparation method

Technical field

The invention discloses a kind of for carbon dioxide methanation catalyst (Ni/Ce xzr 1-xo 2) and preparation method thereof, belong to catalyst preparation technical field.

Background technology

1902, french chemist PaulSabatier reported first catalytic hydrogenating reduction technology (the i.e. CO of carbon dioxide 2methanation reaction): CO 2(g)+4H 2(g)=CH 4(g)+2H 2o (g) △ H 0298K=-252.9KJ.mol -1, CO 2methanation reaction is CO 2an important chemical reaction of recycling, the day by day exhausted and CO to solution gas reserves 2the problem important in inhibitings such as caused ecology and environment.CO is reached by catalysis 2methanation fast, becomes one of rather noticeable problem in C-1 chemistry research.

At current carried out CO 2in the research of hydrogenation methanation reaction, the exploitation of catalyst is a focus.Chinese scholars expands large quantity research, RSCAdvances, and report in 5 (2015): 22759-76, active component Ni, Fe, Co, Ru, Rh, Pd, Pt, Ir etc. are dispersed in Al 2o 3, SiO 2, TiO 2, ZrO 2, CeO 2deng the CO on oxide carrier 2methanation catalyst, because have relatively high catalytic activity and stability is extensively studied.By improving activity and the stability of method for preparing catalyst and optimization of catalysts component raising catalyst.Find by literature search, existing carbon dioxide methanation catalyst component and preparation method thereof, the cost of material of catalyst is high, and preparation method is loaded down with trivial details, and catalyst catalytic activity below 350 DEG C prepared by the method is low, poor stability, poor selectivity.

Summary of the invention

The object of the present invention is to provide and a kind of there is the carbon dioxide methanation catalyst (Ni/Ce that catalytic activity is high, catalytic stability good, production cost is low xzr 1-xo 2), this method for preparing catalyst is simple, easy to operate, cost is lower, has certain application prospect.

A kind of carbon dioxide methanation catalyst (Ni/Ce of the present invention xzr 1-xo 2), it is made up of carrier and active component, it is characterized in that, described carrier adopts cerium zirconium sosoloid, and it is with chemical general formula Ce xzr 1-xo 2represent, described active component is W metal, and wherein, the atomic molar of cerium, zirconium is than being x:(1-x), and 0<x<1, the content of W metal accounts for 10 ~ 40wt.% of carrier quality.

A kind of carbon dioxide methanation catalyst (Ni/Ce of the present invention xzr 1-xo 2) preparation method, mainly comprise following steps:

A. by a certain amount of nickel nitrate (Ni (NO 3) 26H 2o), cerous nitrate (Ce (NO 3) 36H 2o), zirconium nitrate (Zr (NO 3) 45H 2o) join respectively in 50ml deionized water, Ni is active component, with elemental metal, is mixed with at catalyst (Ni/Ce xzr 1-xo 2) in the content of W metal be the mixed solution of 10 ~ 40wt.%;

B. the mixed solution that step a prepares is moved into 80 DEG C of thermostat water baths, with 180 ~ 200 revs/min of speed uniform stirrings, when temperature reaches 80 DEG C, be that the sal volatile 100ml of 2mol/L pours in mixed solution by 100ml concentration, continue agitating heating, temperature remains on 80 DEG C; After constant temperature drying, obtain powder;

C. the powder after being dried by step b, in Muffle furnace, with the programming rate of 2 DEG C/min, rises to 500 DEG C of roasting 5h from room temperature; Then by the powder after above-mentioned roasting at 25 ~ 35kN/Cm 2pressure under to be placed in punching block extruded; With after through broken, sieve, obtaining particle diameter is 40 ~ 60 object particles;

D. the particle obtained by step c is in the hydrogen atmosphere of 30ml/min at reducing gas flow ,temperature is reductase 12 h at 400 DEG C, obtained Ni/Ce xzr 1-xo 2catalyst.

The features and advantages of the invention are as described below:

(1). the present invention is raw material with metal nitrate, take ammonium carbonate as precipitating reagent, has prepared CO by step precipitation method 2methanation catalyst Ni/Ce xzr 1-xo 2(0≤x≤1), 250 oC~ 400 oc has higher catalytic activity and selective, and has high stability, can effective catalysis carbon dioxide hydrogenation reaction at ambient pressure, impels it to become methane.

(2). Catalyst for CO of the present invention 2maximum conversion rate more than 90%, CH 4maximum selectivity is 100%.

(3). method for preparing catalyst of the present invention is simple, easy to operate, cost is lower, has certain application prospect.

Accompanying drawing explanation

Fig. 1 is the X-ray diffractogram of carrier in embodiments of the invention 1-5.

Fig. 2 is 40%Ni/Ce in embodiments of the invention 4 0.9zr 0.1o 2catalyst is carrying out CO 2x-ray diffractogram before hydrogenation methanation reaction.

Fig. 3 is that in embodiments of the invention 1,2,4, carrier loaded 40wt.%Ni catalyst is 7000ml/g.h in air speed, and temperature is 250 DEG C ~ 400 DEG C reactions, CO 2hydrogenation methanation reaction catalytic evaluation result figure.

Fig. 4 is 40%Ni/Ce in embodiments of the invention 1 0.9zr 0.1o 2catalyst is at 300 DEG C, and air speed is 28000ml/gh and 52000ml/gh, 500 hours long-time reaction stability resolution charts.

Fig. 5 is that in embodiments of the invention 3, cerium zirconium mol ratio is the Ce of 9:1 0.9zr 0.1o 2the catalyst of carrier loaded different content Ni is 7000ml/g.h in air speed, 250 DEG C ~ 400 DEG C, CO 2hydrogenation methanation reaction catalytic evaluation result figure.

Detailed description of the invention

By following examples, the present invention is further described, but the present invention is not limited in the present embodiment.

Embodiment 1

A. Ce (NO is taken 3) 36H 2o3.91g, Zr (NO 3) 45H 2o0.43g, Ni (NO 3) 26H 2o5.63g, adds deionized water 50ml, is stirred to dissolving and is mixed with mixed solution.

B. solution moves to 80 DEG C of water-baths, constantly stirs, and pours rapidly above-mentioned mixed solution into, continues to be stirred to evaporate to dryness, forward roasting in Muffle furnace to the sal volatile 100ml of the 2mol/L prepared, and is raised to 500 DEG C of roasting 5h from room temperature with the heating rate of 2 DEG C/min., support C e 0.9zr 0.1o 2x-ray diffractogram as shown in Figure 1, in figure, the oxide of cerium zirconium defines solid solution Ce 0.9zr 0.1o 2..

C. by the powder after roasting at 25 ~ 35kN/Cm 2pressure under extruded in punching block; With after through broken, sieve, obtaining particle diameter is 40 ~ 60 object particles.

D. the particle flow obtained is the H of 30ml/min 2,from room temperature 10 othe heating rate of C/min is warmed up to 400 DEG C, after reductase 12 h, namely obtains 40%Ni/Ce 0.9zr 0.1o 2catalyst, as shown in Figure 2, in figure, is 40%Ni/Ce 0.9zr 0.1o 2catalyst is carrying out CO 2x-ray diffractogram before hydrogenation methanation reaction, as can be seen from Figure 2, through H 2after reduction, the main component of catalyst is Ce 0.9zr 0.1o 2nickel-loaded.

For verifying that catalyst of the present invention uses result, to carbon dioxide methanation (Ni/Ce of the present invention xzr 1-xo 2) catalyst evaluates, its catalyst activity evaluation method is as follows: carry out on a fixed bed, and catalyst is placed in the middle part of reactor flat-temperature zone, supports with quartz sand; CO 2the experiment condition of methanation: normal pressure, temperature 250 DEG C ~ 400 DEG C, feed gas volume air speed is 7000ml/gh ~ 52000ml/gh, and feeding gas constitutive molar ratio is H 2/ CO 2=4:1, product mist is first through water condenser, preliminary hydro-extraction, again through loading the drying tube of calcium sulfate, remove further and generate remaining steam in gas, after stable reaction, start timing sample analysis, after purge drying process, gas detects product gas component by GC-9800 type chromatograph

CO 2(g)+4H 2(g)=CH 4(g)+2H 2O(g)

While there is carbon dioxide methanation reaction, can occur

CO 2(g)+4H 2(g)=CO(g)+2H 2O(g)

CO 2conversion ratio and CH 4, the selective of CO passes through formulae discovery below:

In formula, X cO2for CO 2conversion ratio, S iselective for product, N represents molar flow, and i is CH 4, CO.

The 40%Ni/Ce obtained in embodiment 1 0.9zr 0.1o 2catalyst, at normal pressure, when feed gas volume air speed is 7000ml/gh, 250 DEG C ~ 400 DEG C reactions, calculates according to above-mentioned formula (1), formula (2), CO 2conversion ratio at different temperatures, as shown in Figure 3, during 300 DEG C of reactions, CO 2conversion ratio is up to 92.23%, CH 4selective be 100%, when air speed is 28000ml/gh, CO 2conversion ratio is 86.75%, CH 4selective be 99.91%; Fig. 4 is 40%Ni/Ce 0.9zr 0.1o 2catalyst is at 300 DEG C, and air speed is 28000ml/gh and 52000ml/gh, 500h hour long-time reaction stability resolution chart, and as can be seen from Figure 4, air speed is 28000ml/gh and 52000ml/gh, starts the stage of reaction, CO 2conversion ratio is stabilized in 88.5% and 86.6% respectively, along with the prolongation in reaction time, and CO 2conversion ratio does not change substantially, and at the end of 500h reaction, air speed is the corresponding CO of 28000ml/gh and 52000ml/gh. 2conversion ratio reduces to 86.9% and 83.87% respectively, and the catalytic activity of catalyst remains unchanged, and has higher stability.

Embodiment 2

A. Ce (NO is taken 3) 36H 2o2.17g, Zr (NO 3) 45H 2o2.15g, Ni (NO 3) 26H 2o4.98g adds deionized water 50ml, is stirred to dissolving, is mixed with mixed solution.

B. the solution prepared is moved to 80 DEG C of water-baths, constantly stir, pour rapidly above-mentioned mixed solution into the sal volatile 100ml of 2mol/L, continue to be stirred to evaporate to dryness, forward roasting in Muffle furnace to, be raised to 500 DEG C of roasting 5h from room temperature with the heating rate of 2 DEG C/min and obtain powder, support C e 0.5zr 0.5o 2x-ray diffractogram as shown in Figure 1, in figure, the oxide of cerium zirconium defines solid solution Ce 0.5zr 0.5o 2..

C. by the powder after roasting at 25 ~ 35kN/Cm 2pressure under extruded in punching block; With after through broken, sieve, obtaining particle diameter is 40 ~ 60 object particles.

D. the particle flow obtained is the H of 30ml/min 2, from room temperature with 10 othe heating rate of C/min is warmed up to 400 DEG C, after reductase 12 h, namely obtains 40%Ni/Ce 0.5zr 0.5o 2catalyst.

The 40%Ni/Ce obtained in embodiment 2 0.5zr 0.5o 2catalyst, at normal pressure, feed gas volume air speed is under 7000ml/gh air speed, 250 DEG C ~ 400 DEG C reactions, calculates, CO according to above-mentioned formula (1), formula (2) 2conversion ratio at different temperatures, as shown in Figure 3, during 300 DEG C of reactions, CO 2conversion ratio is up to 90.43%, CH 4selective be 100%.

Embodiment 3

A. Ce (NO is taken 3) 36H 2o3.91g, Zr (NO 3) 45H 2o0.43g, 3.51gNi (NO 3) 26H 2o adds deionized water 50ml, is stirred to dissolving and is mixed with mixed solution.

B. solution is moved to 80 DEG C of water-baths, constantly stir, pour rapidly above-mentioned mixed solution into the sal volatile 100ml of 2mol/L, continue to be stirred to evaporate to dryness, forward roasting in Muffle furnace to, be warmed up to 500 DEG C of roasting 5h from room temperature with the heating rate of 2 DEG C/min, support C e 0.9zr 0.1o 2x-ray diffractogram as shown in Figure 1, in figure, the oxide of cerium zirconium defines solid solution Ce 0.9zr 0.1o 2.

C. by the powder after roasting at 25 ~ 35kN/Cm 2pressure under extruded in punching block; With after through broken, sieve, obtaining particle diameter is 40 ~ 60 object particles.

D. the particle flow obtained is the H of 30ml/min 2, from room temperature 10 othe heating rate of C/min is warmed up to 400 DEG C, after reductase 12 h, namely obtains 30%Ni/Ce 0.9zr 0.1o 2catalyst.

The 30%Ni/Ce obtained in embodiment 3 0.9zr 0.1o 2catalyst is at normal pressure, and feed gas volume air speed is under 7000ml/gh air speed, 250 DEG C ~ 400 DEG C reactions, calculates, CO according to above-mentioned formula (1), formula (2) 2conversion ratio at different temperatures as shown in Figure 4,300 DEG C of reactions, CO 2conversion ratio is up to 90.46%, CH 4selective be 100%.Fig. 4 is that cerium zirconium is than being 9:1 support C e 0.9zr 0.1o 2load different content Raney nickel is 7000ml/g.h in air speed, 250 DEG C ~ 400 DEG C catalytic reaction evaluation result figure, as can be seen from Figure 4, and CO at the same reaction temperature 2conversion ratio raises with the increase of nickel content; When 250 DEG C, 40%Ni/Ce 0.9zr 0.1o 2in catalysis, CO 2conversion ratio is up to 82.36%. temperature when being elevated to 300 DEG C, 40%Ni/Ce 0.9zr 0.1o 2catalyst for CO 2conversion ratio is up to 92.23%., due to carbon dioxide methanation reaction be exothermic reaction, temperature raise to 400 DEG C, CO on each catalyst 2conversion ratio reduces a little.

Embodiment 4

A. nitric acid nickel (NO is taken 3) 26H 2o5.29g, cerous nitrate Ce (NO 3) 36H 2o3.04g, zirconium nitrate Zr (NO 3) 45H 2o1.29g joins in 50ml deionized water respectively, is stirred to dissolving and is mixed with mixed solution.

B. the solution configured is moved to 80 DEG C of thermostat water baths, continuous stirring, when temperature reaches 80 DEG C, pour rapidly the sal volatile 100ml of concentration 2mol/L into above-mentioned mixed solution, continue agitating heating evaporate to dryness, obtaining powder forwards in Muffle furnace by powder, rises to 500 DEG C of roastings 5 hours, support C e with the programming rate of 2 DEG C/min from room temperature 0.7zr 0.3o 2x-ray diffractogram as shown in Figure 1, in figure, the oxide of cerium zirconium defines solid solution Ce 0.7zr 0.3o 2.

C. by the powder after roasting at 25 ~ 35kN/Cm 2pressure under extruded in punching block, with after through broken, sieve, obtaining particle diameter is 40 ~ 60 object particles.

D. the particle flow obtained is the H of 30ml/min 2, from room temperature with 10 oc/min is warmed up to 400 DEG C, after reductase 12 h, i.e. and obtained 40%Ni/Ce 0.7zr 0.3o 2catalyst.

The 40%Ni/Ce obtained in embodiment 4 0.7zr 0.3o 2catalyst is at normal pressure, and feed gas volume air speed is 7000ml/gh, 250 DEG C ~ 400 DEG C reactions, calculates, CO according to above-mentioned formula (1), formula (2) 2conversion ratio at different temperatures as shown in Figure 3,300 DEG C reaction time, CO 2conversion ratio is up to 91.22%, CH 4selective be 100%.

Embodiment 5

A. Ce (NO is taken 3) 36H 2o3.91g, Zr (NO 3) 45H 2o0.43g, Ni (NO 3) 26H 2o2.05g deionized water 50ml, is stirred to dissolving and is mixed with mixed solution.

B. solution moves to 80 DEG C of water-baths, constantly stirs, and pours rapidly above-mentioned mixed solution into, continues to be stirred to evaporate to dryness, forward roasting in Muffle furnace to the sal volatile 100ml of 2mol/L, is raised to 500 DEG C of roasting 5h, support C e from room temperature with the heating rate of 2 DEG C/min 0.9zr 0.1o 2x-ray diffractogram as shown in Figure 1, in figure, the oxide of cerium zirconium defines solid solution Ce 0.9zr 0.1o 2..

C. by the powder after roasting at 25 ~ 35kN/Cm 2pressure under extruded in punching block; With after through broken, sieve, obtaining particle diameter is 40 ~ 60 object particles.

D. the particle flow obtained is the H of 30ml/min 2, from room temperature with 10 othe heating rate of C/min is warmed up to 400 DEG C, after reductase 12 h, namely obtains 20%Ni/Ce 0.9zr 0.1o 2catalyst.

The 20%Ni/Ce obtained in embodiment 5 0.9zr 0.1o 2catalyst is at normal pressure, and feed gas volume air speed is under 7000ml/gh air speed, 250 DEG C ~ 400 DEG C reactions, calculates, CO according to above-mentioned formula (1), formula (2) 2conversion ratio at different temperatures as shown in Figure 5., during 350 DEG C of reactions, CO 2conversion ratio is up to 87.27%, CH 4selective be 100%.

the project detected and the instrument of use thereof

XRD collection of illustrative plates mensuration is carried out, with the target product obtained by determination experiment and purity at RigakuD/max-2550X x ray diffractometer x to gained sample.Condition determination is CuKa(l=1.5406), 40KV, 100mA, Scanspeed:0.02 °/s.Analytical gas uses GC-9800 chromatogram, and service condition is: post case temperature is 80 ~ 130 oC, the temperature of vaporizer is 120 oc, the flow of high-purity argon carrier gas is 30mLmin -1, thermal conductivity detector (TCD) (TCD) temperature is 150 oc, its bridge stream is 70mA, and chromatographic column is 5A molecular sieve packed column (2m × Φ 3mm).

Claims (2)

1. a carbon dioxide methanation catalyst (Ni/Ce xzr 1-xo 2), it is made up of carrier and active component, it is characterized in that, described carrier adopts cerium zirconium sosoloid, and it is with chemical general formula Ce xzr 1-xo 2represent, described active component is W metal, and wherein, the atomic molar of cerium, zirconium is than being x:(1-x), and 0<x<1, the content of W metal accounts for 10 ~ 40wt.% of catalyst gross mass.
2. a carbon dioxide methanation catalyst (Ni/Ce xzr 1-xo 2) preparation method, mainly comprise following steps:
A. by a certain amount of nickel nitrate (Ni (NO 3) 26H 2o), cerous nitrate (Ce (NO 3) 36H 2o), zirconium nitrate (Zr (NO 3) 45H 2o) join respectively in 50ml deionized water, Ni is active component, with elemental metal, is mixed with at catalyst (Ni/Ce xzr 1-xo 2) in the content of W metal be the mixed solution of 10 ~ 40wt.%;
B. the mixed solution that step a prepares is moved into 80 DEG C of thermostat water baths, with 180 ~ 200 revs/min of speed uniform stirrings, when temperature reaches 80 DEG C, be that the sal volatile 100ml of 2mol/L pours in mixed solution by 100ml concentration, continue agitating heating, temperature remains on 80 DEG C; After constant temperature drying, obtain powder;
C. the powder after being dried by step b, in Muffle furnace, with the programming rate of 2 DEG C/min, rises to 500 DEG C of roasting 5h from room temperature; Then by the powder after above-mentioned roasting at 25 ~ 35kN/Cm 2pressure under to be placed in punching block extruded; With after through broken, sieve, obtaining particle diameter is 40 ~ 60 object particles;
D. the particle obtained by step c is in the hydrogen atmosphere of 30ml/min at reducing gas flow ,temperature is reductase 12 h at 400 DEG C, obtained Ni/Ce xzr 1-xo 2catalyst.
CN201510739501.6A 2015-11-04 2015-11-04 Carbon dioxide methanation catalyst (Ni/CexZr(1-x)O2) and preparation method thereof CN105289616A (en)

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CN107029727A (en) * 2016-02-04 2017-08-11 中国人民大学 A kind of catalyst of catalytically liquefying biomass oil and preparation method and application

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