CN106311242A - Carbon dioxide methanation catalyst and preparation method thereof - Google Patents
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Abstract
The invention provides a carbon dioxide methanation catalyst. The chemical form of the catalyst is xAOy.zBO, A and B is a compound which comprises two kinds of oxides, wherein A is at least one of oxides of Si, Al and Zr, and B is at least one of oxides of Ca, Ti, and Mg. Predecessors of active components are one or more of oxides of Fe, Co, Ni and Ru. Oxides of Cr, Zn, Cu, Mo, Mn, La and Ce are auxiliary agents. A mechanical mixing method is used for fully mixing, tableting, roasting and moulding the active components and a carrier. Compared with preparation technology of catalysts of the same kind, the carbon dioxide methanation catalyst has the advantages of high mechanical strength, hydro-thermal stability, large water absorption, carbon deposition resistance, and the like; and the process flow is simple and suitable for large scale industrial production.
Description
Technical field
The invention belongs to carbon dioxide methanation catalysis technical field, be specifically related to a kind of for carbon dioxide methanation catalyst and preparation method thereof.
Background technology
Carbon dioxide is organic substance, the primary product of the fossil fuel burnings such as mineral and oil, fossil fuel provides the energy simultaneously in burning, discharge great amount of carbon dioxide gas, carbon dioxide is considered as one of main component causing greenhouse effect and global warming, account for the 67% of greenhouse gases total amount, the living environment of the mankind is constituted a threat to.Along with energy demand is growing, how to control CO2 emissions and become the common problem paid close attention in the whole world, especially in the exploitation of carbon dioxide, how to realize turning waste into wealth, countries in the world scientist all proposes thought and the technology path of many for carbon dioxide at food, biology, agricultural, chemical field.
Carbon dioxide has had good development trend in fields such as preparing soda pop, synthesising biological albumen, production carbamide, synthesizing methanol and various hydroxy acids.In recent years, by French scientist Paul
The carbon dioxide methanation that Sabatier proposes becomes C-1 chemistry study hotspot owing to having clear and definite application prospect, and carbon dioxide methanation is considered as to solve one of energy shortage and the effective way reducing greenhouse effect.Hashimoto etc. propose carbon dioxide recycle strategy and solve CO2 emission problem, and wherein hydrogenation of carbon dioxide methanation reaction is the core articulation realizing recycling.
CO2Being stable material, its standard heat of formation is △ fGm=394.38KJ/mol, CO2As a kind of weak oxidant, can be reduced inputting enough energy, CO simultaneously2It is a kind of complexant, there is less electron donation and bigger accept electronic capability, complex can be generated with many metals.
Carbon dioxide methanation reaction is mainly:
CO2 + 4H2 →
CH4 + 2H2O +165KJ/mol
CO2With H2Mix in 1:4 ratio, under catalysts conditions, hydrogen adsorbs at catalyst surface and dissociates, it is decomposed into H, carbon dioxide is in catalyst surface absorption and reacts with hydrogen and is converted into containing carbon species, being mainly CO containing carbon species, the CO of ADSORPTION STATE is decomposed into carbon and the oxygen of absorption, then reacts generation methane further with hydrogen.
The research of present stage carbon dioxide methanation catalyst is concentrated mainly on transition metal, and especially VIII race's metal, such as Ru, Rh, Ni, Pd, Fe, Co, Cu etc..Research shows the Al of Ru, Rh and Ni even load2O3、SiO2、TiO2With the catalyst of preparation on MgO carrier, there is good catalysis CO2Methanation performance.CO2The preparation method of methanation catalyst mainly has infusion process, coprecipitation, sol-gal process and low-temperature plasma sintering process etc..There is the shortcomings such as process route is complicated, cost is high, synthesis solid solution crystalline substance degree is low, additionally CO in these preparation methoies2Methanation reaction system pressure is high, react the features such as fast air speed is big requires height to stability and the pyrocaloric effect of catalyst.A kind of catalyst for carbon dioxide hydrogenation reaction of Publication No. CN107078, it uses natural sepiolite to be carrier, infusion process carrying active substance, generates methanation catalyst after roasting, and its catalysis activity performance reaches CO2Conversion ratio reaches 99%, CH4Selectivity reaches more than 95%, but natural sepiolite source is narrow, and cost is high, and industrial application value is limited.Publication No. CN101884927 mono-kind is used for catalyst of full methanation of carbon dioxide and preparation method thereof, and it uses Al2O3For carrier, active component is Ni and Fe, loads on carrier by gradation equi-volume impregnating by active substance, and roasting prepares CO step by step2Methanation catalyst.H2/CO2Mol ratio be 4.1 under conditions of, CO2Conversion ratio close to 100%, CH4Selectivity is close to 100%.The one of Publication No. CN103551153 is used for CO2Copper-based catalysts of methanation and preparation method thereof, its preparation method relating to catalyst predominantly carries out substep co-precipitation by the saline solution of the various metallic elements of involved catalyst and alkaline solution, then filter with the desalted water making beating of heat, catalyst cake is carried out drying and dewatering, dried catalyst precursor carries out calcining, beating sheet, by infusion process step load active substance after molding.Guo et al. using plasma strengthening preparation CO2Methanation nickel-base catalyst is catalyzed journal, 2007,28 (5), 429-434.).Catalyst surface is bombarded by high energy electron in plasma and ion etc., promotes catalyst precursor and decomposes, reduces its reduction temperature and refined crystal grain, and the reduction rear catalyst more conventional catalyst activity of activity improves 27.1%.Although plasma technique improves catalyst activity on largely, but scale is limited and energy consumption is higher limits its industrialized production.
In document by patent disclosed above and report, it will be seen that although carbon dioxide methanation catalyst carrier prepared by distinct methods obtains preferable result of the test, no matter but which kind of preparation technology, the drawback such as when all there is complex process or consumption energy consumption, is unfavorable for large-scale industrial production.
Summary of the invention
The purpose of the present invention: the invention provides a kind of carbon dioxide methanation preparing natural gas catalyst and preparation method thereof.The carbon dioxide methanation catalyst obtained by the method is utilized to have process route simple, low power consumption and other advantages；Catalyst has the advantages such as good hydrothermal stability, anti-carbon and high mechanical properties.
Main feature and the method for the present invention be:
. a kind of for carbon dioxide methanation catalyst, catalyst is made up of active component, auxiliary agent and carrier, and the weight/mass percentage composition of each component is, carrier 70-80%, active component 10-20%, auxiliary agent 1-10%.
Described support chemistry form is xAOyZBO, A and B be two type oxides composition complex, during wherein A is Si, Al, Zr oxide at least one, B is at least one in Ca, Ti, Mg oxide.
The predecessor of described active component is one or more in the oxide of Fe, Co, Ni, Ru.
The auxiliary agent that catalyst is used is one or more in the oxide of Cr, Zn, Cu, Mo, Mn, La, Ce.
Catalyst of the present invention utilizes mechanical mixing active component and carrier to be sufficiently mixed, play sheet, roasting, molding.Its preparation process includes: 1) carrier, active component predecessor and auxiliary agent predecessor and binding agent are mixed to get serosity, utilizes high energy ball mill to be milled to median particle diameter D50 in serosity and is less than 0.1 μm；2) good for ball milling serosity fast spraying under the conditions of 120-150 DEG C is dried to obtain material；3) by 2) in material Muffle furnace Program heat up heating, heating rate is 2 DEG C/min, heating final temperature be 420-550 DEG C, be incubated 4h, last molding, prepare carbon dioxide methanation catalyst.
Described binding agent is the one in deionized water and ethanol.
By the carbon dioxide methanation catalyst prepared by mechanical mixing, being filled in fixed-bed tube reactor, reaction condition is: pressure 2.0-5.0MPa, reacting gas air speed 5000 ~ 11000h-1, H2/CO2Mol ratio 4.1, reaction hot(test)-spot temperature controls at about 500-580 DEG C, and after reaction 200h, the activity of catalyst keeps good, CO2Conversion ratio more than 96%, methane selectively more than 98%, post catalyst reaction mechanical strength stills remain in 280-350N/cm, and the surface of catalyst does not has carbon distribution.
Catalyst characteristics of the present invention: use the carbon dioxide methanation catalyst prepared by the present invention, compare the preparation technology of similar catalyst, having that mechanical strength height, hydrothermal stability, water absorption rate be big and the advantage such as anti-carbon, technological process is simply suitable for large-scale industrial production.
Detailed description of the invention
Describe the present invention below in conjunction with being embodied as example, describe the preparation method and applications of carbon dioxide catalyst in detail, but be not limited to the scope of the present invention.
Embodiment 1:
1) Al is weighed respectively2O3MgO powder 113.4g, NiO powder 35.26g, CuO powder 10.25g mixes, and adds deionized water 300ml, utilizes electromagnetic agitation to be sufficiently stirred for 1h.Feed the mixture into 500ml deionized water, utilize bar type ball milling by mixture ball milling 4h, after utilize high energy ball mill ball milling 6h, ball milling rear slurry median particle diameter D50It it is 0.092 μm.Ball milling rear slurry is spray-dried rapidly, the mixed material being uniformly mixed；2) graphite of mass percent 3% is added in mixed material, mix homogeneously, break into φ 5 × 5mm cylindrical tablet；3) column type tablet is at Muffle kiln roasting, and heating rate is 2 DEG C/min, and temperature is incubated 6h under the conditions of being 500 DEG C, with stove natural cooling, obtains catalyst.Through analyzing, in this catalyst, each constituent mass percent composition is: carrier 76.3%, active substance oxide 15.8%, auxiliary agent oxide 8.9%.Catalyst bulk density is 1.43g/cm3, mechanical strength is 326N/cm.
To implementing 1 catalyst, at reaction hot(test)-spot temperature 560 DEG C, system pressure 4.0MPa, unstripped gas gas volume percentage ratio H2: 36.24, CH4: 49.08, CO2: 9.30, N2: 4.38, reaction velocity is 8000h-1Under the conditions of, made catalyst carbon dioxide methanation activity is evaluated.Product gas is through gas chromatographic analysis, CO2Conversion ratio 98.7%, CH4Selectivity 99%.
To implementing 1 catalyst, at reaction hot(test)-spot temperature 500 DEG C, system pressure 3.0MPa, unstripped gas gas volume percentage ratio H2: 36.28, CH4: 50.18, CO2: 9.26, N2: 4.28, reaction velocity is 6000h-1Under the conditions of, made catalyst carbon dioxide methanation activity is evaluated.Product gas is through gas chromatographic analysis, CO2Conversion ratio 99.4%, CH4Selectivity 100%.
Embodiment 2:
1) ZrO is weighed respectively2MgO complex carrier powder 123.25g, NiO powder 32.26g, Cr2O3Powder 11.6g mixes, and adds deionized water 300ml, utilizes electromagnetic agitation to be sufficiently stirred for 1h.Feed the mixture into 500ml deionized water, utilize bar type ball milling by mixture ball milling 4h, after utilize high energy ball mill ball milling 6h, ball milling rear slurry median particle diameter D50It it is 0.095 μm.Ball milling rear slurry is spray-dried rapidly, the mixed material being uniformly mixed；2) graphite of mass percent 3% is added in mixed material, mix homogeneously, break into φ 5 × 5mm cylindrical tablet；3) column type tablet is at Muffle kiln roasting, and heating rate is 2 DEG C/min, and temperature is incubated 6h under the conditions of being 530 DEG C, with stove natural cooling, obtains catalyst.Through analyzing, in this catalyst, each constituent mass percent composition is: carrier 72.3%, active substance oxide 19.1%, auxiliary agent oxide 8.6%.Catalyst bulk density is 1.62g/cm3, mechanical strength is 407N/cm.
To implementing 2 catalyst, at reaction hot(test)-spot temperature 550 DEG C, system pressure 5.0MPa, unstripped gas gas volume percentage ratio H2: 35.39, CH4: 48.24, CO2: 8.72, N2: 8.38, reaction velocity is 11000h-1Under the conditions of, made catalyst carbon dioxide methanation activity is evaluated.Product gas is through gas chromatographic analysis, CO2Conversion ratio 96.4%, CH4Selectivity 98.5%.
To implementing 2 catalyst, at reaction hot(test)-spot temperature 500 DEG C, system pressure 4.0MPa, unstripped gas gas volume percentage ratio H2: 35.33, CH4: 48.27, CO2: 8.74, N2: 8.32, reaction velocity is 6000h-1Under the conditions of, made catalyst carbon dioxide methanation activity is evaluated.Product gas is through gas chromatographic analysis, CO2Conversion ratio 98.4%, CH4Selectivity 100%.
Embodiment 3:
1) Al is weighed respectively2O3CaO complex carrier powder 105.4g, NiO powder 16.5g, Ce2O3Powder 10.3g mixes, and adds deionized water 300ml, utilizes electromagnetic agitation to be sufficiently stirred for 1h.Feed the mixture into 500ml deionized water, utilize bar type ball milling by mixture ball milling 4h, after utilize high energy ball mill ball milling 6h, ball milling rear slurry median particle diameter D50It it is 0.089 μm.Ball milling rear slurry is spray-dried rapidly, the mixed material being uniformly mixed；2) graphite of mass percent 3% is added in mixed material, mix homogeneously, break into φ 5 × 5mm cylindrical tablet；3) column type tablet is at Muffle kiln roasting, and heating rate is 2 DEG C/min, and temperature is incubated 6h under the conditions of being 560 DEG C, with stove natural cooling, obtains catalyst.Through analyzing, in this catalyst, each constituent mass percent composition is: carrier 79.2%, active substance oxide 12.7%, auxiliary agent oxide 7.91%.Catalyst bulk density is 1.58g/cm3, mechanical strength is 424N/cm.
To implementing 3 catalyst, at reaction hot(test)-spot temperature 580 DEG C, system pressure 5.0MPa, unstripped gas gas volume percentage ratio H2: 35.39, CH4: 48.24, CO2: 8.72, N2: 8.38, reaction velocity is 7000h-1Under the conditions of, made catalyst carbon dioxide methanation activity is evaluated.Product gas is through gas chromatographic analysis, CO2Conversion ratio 96.4%, CH4Selectivity 98.5%.
To implementing 3 catalyst, at reaction hot(test)-spot temperature 520 DEG C, system pressure 4.0MPa, unstripped gas gas volume percentage ratio H2: 35.33, CH4: 48.27, CO2: 8.74, N2: 8.32, reaction velocity is 6000h-1Under the conditions of, made catalyst carbon dioxide methanation activity is evaluated.Product gas is through gas chromatographic analysis, CO2Conversion ratio 98.4%, CH4Selectivity 100%.
Embodiment 4:
1) Al is weighed respectively2O3CaO complex carrier powder 105.4g, NiO powder 22.3g, Ce2O3Powder 10.3g mixes, and adds deionized water 300ml, utilizes electromagnetic agitation to be sufficiently stirred for 1h.Feed the mixture into 500ml deionized water, utilize bar type ball milling by mixture ball milling 4h, after utilize high energy ball mill ball milling 6h, ball milling rear slurry median particle diameter D50It it is 0.089 μm.Ball milling rear slurry is spray-dried rapidly, the mixed material being uniformly mixed；2) graphite of mass percent 3% is added in mixed material, mix homogeneously, break into φ 5 × 5mm cylindrical tablet；3) column type tablet is at Muffle kiln roasting, and heating rate is 2 DEG C/min, and temperature is incubated 6h under the conditions of being 560 DEG C, with stove natural cooling, obtains catalyst.Through analyzing, in this catalyst, each constituent mass percent composition is: carrier 75.2%, active substance oxide 15.9%, auxiliary agent oxide 8.9%.Catalyst bulk density is 1.62g/cm3, mechanical strength is 421N/cm.
To implementing 3 catalyst, at reaction hot(test)-spot temperature 560 DEG C, system pressure 5.0MPa, unstripped gas gas volume percentage ratio H2: 41.34, CH4: 42.24, CO2: 10.52, N2: 5.38, reaction velocity is 8000h-1Under the conditions of, made catalyst carbon dioxide methanation activity is evaluated.Product gas is through gas chromatographic analysis, CO2Conversion ratio 98.1%, CH4Selectivity 99.2%.
To implementing 3 catalyst, at reaction hot(test)-spot temperature 520 DEG C, system pressure 4.0MPa, unstripped gas gas volume percentage ratio H2: 42.33, CH4: 40.58, CO2: 11.74, N2: 6.57, reaction velocity is 6000h-1Under the conditions of, made catalyst carbon dioxide methanation activity is evaluated.Product gas is through gas chromatographic analysis, CO2Conversion ratio 99.6%, CH4Selectivity 100%.
Embodiment 5:
1) TiO is weighed respectively2MgO support powder 122.5g, Co2O3Powder 27.2g, Cr2O3Powder 11.6g mixes, and adds deionized water 300ml, utilizes electromagnetic agitation to be sufficiently stirred for 1h.Feed the mixture into 500ml deionized water, utilize bar type ball milling by mixture ball milling 4h, after utilize high energy ball mill ball milling 6h, ball milling rear slurry median particle diameter D50It it is 0.096 μm.Ball milling rear slurry is spray-dried rapidly, the mixed material being uniformly mixed；2) graphite of mass percent 3% is added in mixed material, mix homogeneously, break into φ 5 × 5mm cylindrical tablet；3) column type tablet is at Muffle kiln roasting, and heating rate is 2 DEG C/min, and temperature is incubated 6h under the conditions of being 530 DEG C, with stove natural cooling, obtains catalyst.Through analyzing, in this catalyst, each constituent mass percent composition is: carrier 76.5%, active substance oxide 17.1%, auxiliary agent oxide 6.4%.Catalyst bulk density is 1.58g/cm3, mechanical strength is 387N/cm.
To implementing 2 catalyst, at reaction hot(test)-spot temperature 580 DEG C, system pressure 3.0MPa, unstripped gas gas volume percentage ratio H2: 35.39, CH4: 48.24, CO2: 8.72, N2: 8.38, reaction velocity is 10000h-1Under the conditions of, made catalyst carbon dioxide methanation activity is evaluated.Product gas is through gas chromatographic analysis, CO2Conversion ratio 97.3%, CH4Selectivity 99.2%.
To implementing 2 catalyst, at reaction hot(test)-spot temperature 500 DEG C, system pressure 2.0MPa, unstripped gas gas volume percentage ratio H2: 35.33, CH4: 48.27, CO2: 8.74, N2: 8.32, reaction velocity is 7000h-1Under the conditions of, made catalyst carbon dioxide methanation activity is evaluated.Product gas is through gas chromatographic analysis, CO2Conversion ratio 100%, CH4Selectivity 100%.
Embodiment 6:
1) TiO is weighed respectively2CaO support powder 126.5g, Co2O3Powder 36.2g, Cr2O3Powder 12.3g mixes, and adds deionized water 300ml, utilizes electromagnetic agitation to be sufficiently stirred for 1h.Feed the mixture into 500ml deionized water, utilize bar type ball milling by mixture ball milling 4h, after utilize high energy ball mill ball milling 6h, ball milling rear slurry median particle diameter D50It it is 0.096 μm.Ball milling rear slurry is spray-dried rapidly, the mixed material being uniformly mixed；2) graphite of mass percent 3% is added in mixed material, mix homogeneously, break into φ 5 × 5mm cylindrical tablet；3) column type tablet is at Muffle kiln roasting, and heating rate is 2 DEG C/min, and temperature is incubated 6h under the conditions of being 530 DEG C, with stove natural cooling, obtains catalyst.Through analyzing, in this catalyst, each constituent mass percent composition is: carrier 76.5%, active substance oxide 17.1%, auxiliary agent oxide 6.4%.Catalyst bulk density is 1.58g/cm3, mechanical strength is 387N/cm.
To implementing 2 catalyst, at reaction hot(test)-spot temperature 580 DEG C, system pressure 3.0MPa, unstripped gas gas volume percentage ratio H2: 36.29, CH4: 46.24, CO2: 9.72, N2: 8.68, reaction velocity is 10000h-1Under the conditions of, made catalyst carbon dioxide methanation activity is evaluated.Product gas is through gas chromatographic analysis, CO2Conversion ratio 98.2%, CH4Selectivity 98.9%.
To implementing 2 catalyst, at reaction hot(test)-spot temperature 500 DEG C, system pressure 2.5MPa, unstripped gas gas volume percentage ratio H2: 37.33, CH4: 45.27, CO2: 9.84, N2: 7.52, reaction velocity is 8000h-1Under the conditions of, made catalyst carbon dioxide methanation activity is evaluated.Product gas is through gas chromatographic analysis, CO2Conversion ratio 100%, CH4Selectivity 100%.
Claims (6)
1. one kind is used for carbon dioxide methanation catalyst, it is characterised in that catalyst is made up of active component, auxiliary agent and carrier, and the weight/mass percentage composition of each component is, carrier 70-80%, active component 10-20%, auxiliary agent 1-10%.
2. catalyst as claimed in claim 1, it is characterised in that described carrier is A and the complex of B two type oxide composition, during wherein A is Si, Al, Zr oxide at least one, B is at least one in Ca, Ti, Mg oxide.
3. catalyst as claimed in claim 1, it is characterised in that the predecessor of described active component is one or more in the oxide of Fe, Co, Ni, Ru.
4. catalyst as claimed in claim 1, it is characterised in that described auxiliary agent is one or more in the oxide of Cr, Zn, Cu, Mo, Mn, La, Ce.
5. the preparation method of methanation catalyst as claimed in claim 1, it is characterized in that, preparation process includes: 1) carrier, active component predecessor and auxiliary agent predecessor and binding agent are mixed to get serosity, utilizes high energy ball mill to be milled to median particle diameter D50 in serosity and is less than 0.1 μm；2) good for ball milling serosity fast spraying under the conditions of 120-150 DEG C is dried to obtain material；3) by 2) in material Muffle furnace Program heat up heating, heating rate is 2 DEG C/min, heating final temperature be 420-550 DEG C, be incubated 4h, last molding, prepare carbon dioxide methanation catalyst.
6. preparation method as claimed in claim 5, it is characterised in that binding agent used is the one in deionized water and ethanol.
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| CN112138654B (en) * | 2020-09-11 | 2023-06-27 | 杨郅栋 | Catalyst for hydromethanation of carbon dioxide and application thereof |
| CN114735646A (en) * | 2021-01-07 | 2022-07-12 | 中国石油化工股份有限公司 | Oxygen carrier for chemical ring hydrogen production and preparation method and application thereof |
| CN113634257A (en) * | 2021-08-05 | 2021-11-12 | 华东师范大学 | Application of bifunctional catalyst to CO in flue gas2Integration of capture and methanation |
| CN114377679A (en) * | 2022-01-26 | 2022-04-22 | 中国科学院上海高等研究院 | Carbon dioxide capturing and converting integrated bifunctional catalyst, preparation method and application |
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