CN103418392A - Reverse water gas shift catalyst and preparation method thereof - Google Patents
Reverse water gas shift catalyst and preparation method thereof Download PDFInfo
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- CN103418392A CN103418392A CN2012101474222A CN201210147422A CN103418392A CN 103418392 A CN103418392 A CN 103418392A CN 2012101474222 A CN2012101474222 A CN 2012101474222A CN 201210147422 A CN201210147422 A CN 201210147422A CN 103418392 A CN103418392 A CN 103418392A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 56
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000008367 deionised water Substances 0.000 claims abstract description 9
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 9
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 150000001768 cations Chemical class 0.000 claims abstract description 3
- 238000001035 drying Methods 0.000 claims abstract description 3
- 229910052751 metal Inorganic materials 0.000 claims abstract description 3
- 239000002184 metal Substances 0.000 claims abstract description 3
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 3
- 239000000203 mixture Substances 0.000 claims description 9
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 4
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims description 2
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 2
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 2
- 238000000034 method Methods 0.000 claims description 2
- 239000004323 potassium nitrate Substances 0.000 claims description 2
- 235000010333 potassium nitrate Nutrition 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 23
- 230000000694 effects Effects 0.000 abstract description 11
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 abstract description 3
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 abstract 1
- 229910017052 cobalt Inorganic materials 0.000 abstract 1
- 239000010941 cobalt Substances 0.000 abstract 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 abstract 1
- XMHIUKTWLZUKEX-UHFFFAOYSA-N hexacosanoic acid Chemical compound CCCCCCCCCCCCCCCCCCCCCCCCCC(O)=O XMHIUKTWLZUKEX-UHFFFAOYSA-N 0.000 abstract 1
- 239000007788 liquid Substances 0.000 description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- 239000010949 copper Substances 0.000 description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010453 quartz Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 229910002091 carbon monoxide Inorganic materials 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000013112 stability test Methods 0.000 description 2
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 239000003708 ampul Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000007809 chemical reaction catalyst Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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Abstract
本发明公开了一种逆水煤气变换反应的催化剂及其制备方法，该催化剂以CeO2为载体，负载钴作为活性组分，活性组分Co的含量为催化剂质量的1～30%，K为助剂。制备方法包括：用去离子水配置含金属阳离子K、Co、Ce及含柠檬酸溶液，溶液在70-90℃搅拌得到溶胶；溶胶经干燥、焙烧后得到催化剂。本发明的优点在于，制备方法简便，制得的催化剂用于逆水煤气变换反应具有活性高、选择性好和稳定性良好的特点。
The invention discloses a catalyst for a reverse water gas shift reaction and a preparation method thereof. The catalyst uses CeO2 as a carrier, cobalt as an active component, the content of the active component Co is 1 to 30% of the mass of the catalyst, and K is the auxiliary agent. The preparation method comprises: preparing a solution containing metal cations K, Co, Ce and citric acid with deionized water, stirring the solution at 70-90 DEG C to obtain a sol; drying and roasting the sol to obtain a catalyst. The invention has the advantages of simple and convenient preparation method, and the prepared catalyst has the characteristics of high activity, good selectivity and good stability when used in reverse water gas shift reaction.
Description
Technical field
The present invention relates to for the Co of Reversed Water-gas Shift reaction catalyst basedly and preparation method thereof, belong to the catalyst technology of carbon dioxide conversion application.
Background technology
In recent years, along with a large amount of CO
2The greenhouse effects that discharge causes are day by day serious, CO
2Conversion and application study day by day active, wherein the Reversed Water-gas Shift reaction is considered to that one of reaction of application prospect is arranged most.Reversed Water-gas Shift reaction (RWGS:CO
2+ H
2=CO+H
2O Δ H=40.6kJ/mol) can utilize CO
2Generate more valuable CO.At present, for the Reversed Water-gas Shift repercussion study, be mainly copper-based catalysts.Copper-based catalysts is selectively good, but activity and high high-temp stability are poor, and the emphasis for the Reversed Water-gas Shift repercussion study is to improve its activity and high high-temp stability at present.In copper-based catalysts, add the auxiliary agents such as alkali metal can further improve activity and the stability of catalyst.Except Cu is catalyst based, mainly also has ZnO/Al for the Reversed Water-gas Shift catalyst
2O
3, MoS
2, WS
2Deng catalyst.MoS
2, WS
2The activity of catalyst and Ni/Al
2O
3, Co/Al
2O
3, Fe/Al
2O
3Compare low, but the reaction of its Reversed Water-gas Shift selectively approach 100%.Ni/Al
2O
3, Co/Al
2O
3And Fe/Al
2O
3Catalyst has certain activity, wherein Ni/Al to methanation reaction
2O
3The methanation reaction activity of catalyst is the highest.
The subject matter that the Reversed Water-gas Shift catalysts exists at present is heat endurance and poor selectivity.Cu is catalyst based due to poor heat stability, is difficult to be applied to the reaction of high temperature Reversed Water-gas Shift, even add auxiliary agent can improve its heat endurance and activity, but its activity and heat endurance still remain to be improved.Ni/Al
2O
3Although the catalyst activity is very high, the methanation side reaction easily occurs on catalyst, be not suitable for the Reversed Water-gas Shift reaction yet.
For above-mentioned situation, we had carried out the catalyst based research and development of Co for the Reversed Water-gas Shift reaction in recent years, and had obtained some achievements, proposed the application.
Summary of the invention
Primary technical problem to be solved by this invention is to provide a kind of Reversed Water-gas Shift catalyst, and this catalyst has active characteristics high, that selectively get well and have good stability for the Reversed Water-gas Shift reaction.
Another technical problem to be solved by this invention is to provide a kind of preparation method of Reversed Water-gas Shift catalyst, and this catalyst has active characteristics high, that selectively get well and have good stability for the Reversed Water-gas Shift reaction.
The present invention solves the technical scheme that above-mentioned primary technical problem adopts: a kind of Reversed Water-gas Shift catalyst is characterized in that: comprise support C eO
2, active component Co and auxiliary agent K, wherein the quality percentage composition of active component Co is 1～30%, auxiliary agent K quality percentage composition is 1～10%.
The present invention solves the technical scheme that above-mentioned another technical problem adopts: a kind of preparation method of above-mentioned Reversed Water-gas Shift catalyst is characterized in that step process is:
1) according to the quality percentage composition of K in catalyst be 1～10%, the quality percentage composition of Co is 1～30%, take potassium nitrate, cobalt nitrate, cerous nitrate, reach the ratio in the summation of metal cation K, Co, Ce and the mol ratio 1:1 of citric acid～2, take citric acid, they are joined in deionized water, in the water-bath of 10～40 ℃ of temperature, stir and within 1～4 hour, make solution, solution continues stirring and obtains colloidal sol under the water-bath of 70～90 ℃ of temperature.
2) above-mentioned colloidal sol is placed in to baking oven dry 12～24h under 80～120 ℃, the sample after drying is placed in to Muffle furnace at 400～800 ℃ of lower roasting 2～6h, obtain K-Co-CeO
2Catalyst.
Compared with prior art, the invention has the advantages that, preparation process is simple, the catalyst based K-Co-CeO of the Co made
2There are active characteristics high, that selectively get well and have good stability for the Reversed Water-gas Shift reaction.
The accompanying drawing explanation
Fig. 1 is the prepared x%K-10%Co-CeO of embodiment of the present invention 1-6
2(x=1,2,5,7,10) catalyst and Co-CeO
2The CO of catalyst
2Conversion ratio varies with temperature curve map.
Fig. 2 is the prepared x%K-10%Co-CeO of embodiment of the present invention 1-6
2(x=1,2,5,7,10) catalyst and Co-CeO
2The CH of catalyst
4Selectively vary with temperature curve map.
Fig. 3 is the prepared 10%K-10%Co-CeO of the embodiment of the present invention 6
2Catalyst for CO
2Conversion ratio and CH
4Selectively with the reaction time change curve.
The specific embodiment
Embodiment 1:
Take respectively the KNO of 0.104g with electronic balance
3, the Co (NO of 1.975g
3)
26H
2O, the Ce (NO of 8.990g
3)
36H
2O, the citric acid of 4.993g, join wiring solution-forming in the deionized water of 200ml, and the stirred in water bath 1h 40 ℃ of temperature, obtain uniform liquid, till continuing to be stirred under 70 ℃ of water-baths and obtaining colloidal sol.Then dry 24h under 80 ℃ in baking oven, the solid obtained is 600 ℃ of roasting 4h in Muffle furnace, obtain the 1%K-10%Co-CeO2 catalyst.
Take respectively the KNO of 0.208g with electronic balance
3, the Co (NO of 1.975g
3)
26H
2O, the Ce (NO of 8.900g
3)
36H
2O, the citric acid of 5.138g, join wiring solution-forming in the deionized water of 200ml, and the stirred in water bath 1h 40 ℃ of temperature, obtain uniform liquid, till continuing to be stirred under 70 ℃ of water-baths and obtaining colloidal sol.Then dry 24h under 80 ℃ in baking oven, the solid obtained is 600 ℃ of roasting 4h in Muffle furnace, obtain 2%K-10%Co-CeO
2Catalyst.
Take respectively the KNO of 0.52g with electronic balance
3, the Co (NO of 1.975g
3) .6H
2O, the Ce (NO of 8.580g
3)
36H
2O, the citric acid of 5.545g, join wiring solution-forming in the deionized water of 200ml, and the stirred in water bath 1h 40 ℃ of temperature, obtain uniform liquid, till continuing to be stirred under 70 ℃ of water-baths and obtaining colloidal sol.Then dry 24h under 80 ℃ in baking oven, the solid obtained is 600 ℃ of roasting 4h in Muffle furnace, obtain the 5%K-10%Co-CeO2 catalyst
The KNO that divides the 0.728g that has another name called with electronic balance
3, the Co (NO of 1.975g
3)
26H
2O, the Ce (NO of 8.380g
3)
36H
2O, the citric acid of 5.825g, join wiring solution-forming in the deionized water of 200ml, and the stirred in water bath 1h 40 ℃ of temperature, obtain uniform liquid, till continuing to be stirred under 70 ℃ of water-baths and obtaining colloidal sol.Then dry 24h under 80 ℃ in baking oven, the solid obtained is 600 ℃ of roasting 4h in Muffle furnace, obtain 7%K-10%Co-CeO
2Catalyst.
The KNO that divides the 0.728g that has another name called with electronic balance
3, the Co (NO of 1.975g
3)
26H
2O, the Ce (NO of 8.380g
3)
36H
2O, the citric acid of 5.825g, join wiring solution-forming in the deionized water of 200ml, and the stirred in water bath 3h 30 ℃ of temperature, obtain uniform liquid, till continuing to be stirred under 80 ℃ of water-baths and obtaining colloidal sol.Then dry 18h under 100 ℃ in baking oven, the solid obtained is 700 ℃ of roasting 4h in Muffle furnace, obtain 7%K-10%Co-CeO
2-700 catalyst.
Take respectively the KNO of 1.04g with electronic balance
3, the Co (NO of 1.975g
3)
26H
2O, the Ce (NO of 8.070g
3)
36H
2O, the citric acid of 6.240g, join wiring solution-forming in the deionized water of 200ml, and the stirred in water bath 1h 40 ℃ of temperature, obtain uniform liquid, till continuing to be stirred under 70 ℃ of water-baths and obtaining colloidal sol.Then dry 24h under 80 ℃ in baking oven, the solid obtained is 600 ℃ of roasting 4h in Muffle furnace, obtain 10%K-10%Co-CeO
2Catalyst.
The catalyst screening made above-mentioned, getting granularity is 60～100 purpose catalyst 50mg, carries out performance test on the fixed bed quartz tube reactor, the quartz ampoule specification is Φ 12 * 2, the unstripped gas air speed is 120,000mL/hg
cat.Unstripped gas consists of: 50vol.%CO
2, 50vol.%H
2.Sample is at the N of 50ml/min
2Rise to 400 ℃ from room temperature under atmosphere, start to be reacted after passing into unstripped gas.Reaction temperature is from 400 ℃ to 600 ℃, and 50 ℃ of every intensifications are a temperature spot, each temperature spot reaction 0.5h.Adopt the beautiful GC-7900 type gas-chromatography on-line analysis of sky, Shanghai, TDX-01 chromatographic column, fid detector (band methane reborner).CO when catalyst test the results are shown in 2,600 ℃, accompanying drawing 1, accompanying drawing
2Conversion ratio all reaches more than 35%.With 10%Co-CeO
2Catalyst is compared, and in catalyst, adds the K composition can obviously reduce the generation of byproduct methane.
10%K-10%Co-CeO
2The catalyst stability test is carried out on the identical experiment device.Getting granularity is 60～100 purpose 10%K-10%Co-CeO
2Catalyst 50mg carries out performance test on the fixed bed quartz tube reactor, and the unstripped gas air speed is 120,000mL/hg
cat.Unstripped gas consists of: 50vol.%CO
2, 50vol.%H
2.Sample is at the N of 50ml/min
2Rise to 600 ℃ from room temperature under atmosphere, pass into unstripped gas and start reaction.The catalyst stability test result is shown in accompanying drawing 3, CO in 17h
2Conversion ratio reaches 38%, and byproduct methane selectively is less than 0.06%, and catalyst has good stability.
Claims (2)
1. a Reversed Water-gas Shift catalyst, is characterized in that: comprise support C eO
2, active component Co and auxiliary agent K, wherein the quality percentage composition of active component Co is 1～30%, auxiliary agent K quality percentage composition is 1～10%.
2. the preparation method of a Reversed Water-gas Shift catalyst claimed in claim 1 is characterized in that step process is:
According to the quality percentage composition of K in catalyst be 1～10%, the quality percentage composition of Co is 1～30%, take potassium nitrate, cobalt nitrate, cerous nitrate, reach the ratio in the summation of metal cation K, Co, Ce and the mol ratio 1:1 of citric acid～2, take citric acid, they are joined in deionized water, in the water-bath of 10～40 ℃ of temperature, stir and within 1～4 hour, make solution, solution continues stirring and obtains colloidal sol under the water-bath of 70～90 ℃ of temperature;
Above-mentioned colloidal sol is placed in to baking oven dry 12～24h under 80～120 ℃, the sample after drying is placed in to Muffle furnace at 400～800 ℃ of lower roasting 2～6h, obtain K-Co-CeO
2Catalyst.
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| CN103418392B CN103418392B (en) | 2015-10-28 |
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| CN104876205A (en) * | 2015-04-03 | 2015-09-02 | 浙江海洋学院 | Method for preparing carbon nano-fibers through dioxide hydrogenation process |
| CN105854914A (en) * | 2016-03-30 | 2016-08-17 | 浙江海洋学院 | Reverse water-gas shift catalyst prepared from crab shells |
| CN106881084A (en) * | 2015-12-10 | 2017-06-23 | 中国科学院大连化学物理研究所 | One kind is used for reverse water-gas-shift reaction noble metal catalyst and its preparation and application |
| CN108144637A (en) * | 2016-12-05 | 2018-06-12 | 中国科学院大连化学物理研究所 | It is a kind of for the catalyst of reverse water-gas-shift reaction and its preparation and application |
| WO2018122439A1 (en) | 2016-12-29 | 2018-07-05 | Consejo Superior De Investigaciones Científicas (Csic) | Method for producing catalysts of formula my(ce1-xlxo2-x/2)1-y for the use thereof in the reverse water-gas shift reaction and partial oxidation of methane into synthesis gas by means of the method of combustion in solution |
| CN108529625A (en) * | 2018-06-13 | 2018-09-14 | 昆明理工大学 | A method of preparing carbon monoxide using coal |
| CN110479323A (en) * | 2019-07-22 | 2019-11-22 | 中国科学院福建物质结构研究所 | Gas converter technique produces CO catalyst and preparation method thereof to one kind against the current |
| CN114146710A (en) * | 2021-12-02 | 2022-03-08 | 中国科学院上海高等研究院 | Reverse water gas reaction catalyst and preparation method and application thereof |
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| CN108529625A (en) * | 2018-06-13 | 2018-09-14 | 昆明理工大学 | A method of preparing carbon monoxide using coal |
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| CN114682273A (en) * | 2022-03-18 | 2022-07-01 | 昆明理工大学 | Alkali metal synergistic molybdenum disulfide activated carbon dioxide hydrogenation resource utilization method |
| CN115178276A (en) * | 2022-07-12 | 2022-10-14 | 东莞理工学院 | Preparation and application of nickel-based catalyst for reverse water gas shift reaction |
| CN115178276B (en) * | 2022-07-12 | 2023-09-22 | 东莞理工学院 | Preparation and application of a nickel-based catalyst for reverse water gas shift reaction |
| CN116081674A (en) * | 2023-02-08 | 2023-05-09 | 湖州学院 | Synergistic preparation of oxygen vacancy-rich ceria by cathode ray and cobalt doping |
| CN116351428A (en) * | 2023-02-27 | 2023-06-30 | 东莞市振亮精密科技有限公司 | Preparation and application of a reverse water gas shift catalyst with sodium and potassium as additives |
| CN116351428B (en) * | 2023-02-27 | 2024-10-25 | 东莞市振亮精密科技有限公司 | Preparation and application of reverse water gas shift catalyst with sodium and potassium as auxiliary agents |
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