CN102299345A - Application of methane reforming catalyst to molten carbonate fuel cell - Google Patents
Application of methane reforming catalyst to molten carbonate fuel cell Download PDFInfo
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Abstract
The invention discloses application of a methane reforming catalyst to a molten carbonate fuel cell. The catalyst comprises the following components in percentage by weight: 4 to 25 percent of active ingredient nickel, 0 to 10 percent of rare-earth element catalyst aid and 65 to 96 percent of alumina carrier. The preparation method of the catalyst is simple and can be operated at an intermediate temperature under the condition of a low water-carbon ratio, and the catalyst has high reaction activity, carbon deposition resistance and stability.
Description
Technical field
The present invention relates to be used for the reforming catalyst of molten carbonate fuel cell (MCFC), the application of particularly a kind of methane reforming catalyst in molten carbonate fuel cell.
Background technology
Fuel cell is a kind of Blast Furnace Top Gas Recovery Turbine Unit (TRT) that chemical energy in fuel and the oxidant is converted into electric energy.It is without the overheated machine process, so be not subjected to the restriction of Carnot cycle, the energy conversion efficiency height.Simultaneously, it is again a kind of Blast Furnace Top Gas Recovery Turbine Unit (TRT) of cleanliness without any pollution.Wherein, molten carbonate fuel cell (MCFC) is the Blast Furnace Top Gas Recovery Turbine Unit (TRT) at 600-700 ℃ of hot operation, except These characteristics, also has the unrivaled advantage of many other fuel cells, as need not to adopt noble metal electrode, can reduce the battery cost greatly; The bigger fuel scope of application is arranged, except hydrogen, carbon monoxide, also can directly act as a fuel with natural gas, coal gas gasification and other hydrocarbon.
With natural gas during as MCFC fuel, methane and vapor reforming hydrogen production gas, carbon monoxide, hydrogen and carbon monoxide participate in occurring in the electrochemical reaction of galvanic anode:
CH
4+H
2O→CO+3H
2 (1)
H
2+CO
3 2-→H
2O+CO
3+2e
- (2)
CO+CO
3 2-→2CO
2+2e
- (3)
Methane vapor reforming can be divided into outer reformation, indirect internal reforming (IIR) and directly interior reform (DIR) among the MCFC.Reformation molten carbonate fuel cell (DIR-MCFC) has following major advantage directly:
(1) owing to do not need external reformer, reduced system cost;
(2) the energy coupling of realization electrochemistry, reforming reaction: the electrochemical reaction heat release, the reforming reaction strong endothermic, the two can realize complementation, the cell row heat load reduces;
(3) the material coupling of realization electrochemistry, reforming reaction: the anode electro-oxidation reaction generates the CO of water vapour, reforming reaction generation
2Can be recycled; Electrode reaction anode consumption hydrogen can be broken the reforming reaction thermodynamical equilibrium, improves methane conversion and cell power generation efficient;
(4) hydrogen is more evenly distributed in the DIR-MCFC anode, and Temperature Distribution is also more even in the battery.
Usually under the state, the methane vapor reforming reaction temperature generally more than 850 ℃, water and methane mol ratio (also be called steam/hydrocarbons ratio, S/C) elect as more than 3: 1, but in view of 600-700 ℃ of MCFC working temperature, so require the DIR-MCFC reforming catalyst in 600-700 ℃, to operate, and have sufficiently high activity.
The water generation reforming reaction that methane and electrochemical reaction generate in the DIR-MCFC anode gas chamber, need not extraneous water supply in theory, but battery is under open-circuit condition or under low current density, water content is low in the anode gas chamber, steam/hydrocarbons ratio is low, the easy carbon distribution of catalyst, thus catalysqt deactivation caused, influence catalyst life.So require the DIR-MCFC reforming catalyst under the low steam carbon ratio condition, to work, guaranteeing to possess high carbon accumulation resisting ability under the sufficiently high active prerequisite.
Based on above-mentioned 2 points, the present invention develops a kind of can the operation under middle temperature, low steam carbon ratio condition, can be used for the methane reforming catalyst of MCFC.Though the relevant report of methane vapor reforming catalyst is arranged, but still needleless is to the report of particular surroundings use among the MCFC both at home and abroad.
(Catalysis Today.2004 is 98:575-581) to catalyst Rh/MgO-Al for Y.Wang etc.
2O
3Study, find at low steam carbon ratio H
2O/C=1: under 2 the situation, after reaction had been carried out 14 hours, catalyst was without any the vestige of carbon distribution, and still keeps higher activity, but because the noble metal cost is higher, can't large-scale application.
(Applied Catalysis A:General.2007 is 330:12-22) at Ni/AL for N.V.Parizott etc.
2O
3In added metal A g, at low steam carbon ratio H
2O/C=1: 2 o'clock, 600 ℃ were carried out the water vapour methane reforming reaction, found that the adding of Ag has good anti-carbon.But the adding of Ag has significantly suppressed catalyst activity.
The La/Ni/Al of WO 097319 preparation
2O
3Catalyst forms at 800-960 ℃ of following sintering by coprecipitation.This catalyst is adapted to methane vapor reforming and methane self-heating recapitalization, but this catalyst not under 650 ℃, low steam carbon ratio environment (S/C≤1) carry out catalytically active assessment.
Chinese patent CN1130256C discloses a kind of Mo-W catalyst, and this method for preparing catalyst comprises molybdenum tungsten solution impregnation in porous carrier, subsequently its carbonization is got the molybdenum tungsten carbide, passivation and getting under nitrogen environment again.This catalyst is at low steam carbon ratio (S/C=0.5), and (＞800 ℃) have higher methane conversion under the high temperature.This patent does not provide the performance of catalyst under the middle temperature (650 ℃).
Chinese patent CN100398203C discloses the methane vapor reforming catalyst that a kind of carbon dioxide is strengthened, and this Preparation of catalysts method comprises CaO and NiO and alumina support are composited.This catalyst can effectively adsorb the CO that produces in the reforming process
2, improve methane conversion.But this catalyst use amount is bigger, and (S/C≤1) carries out the test of reforming reaction catalyst activity and anti-carbon not under the low steam carbon ratio environment.
Chinese patent CN101327440A discloses a kind of methane steam reforming composite catalyst, and this catalyst is to be being composited of carrier with the alundum (Al with nickel metallic atom catalyst and heteropoly phosphorus molybdenum tungstic acid catalyst.The steam/hydrocarbons ratio (S/C=4) that this catalyst is higher is operated under (440 ℃) condition under the lower temperature, and methane conversion can reach 100%, but patent is not given in the catalyst performance under the low steam carbon ratio condition.
It is the nickel-base catalyst of carrier with Ce, Zr that Chinese patent CN101224427A discloses a kind of, and this catalyst is to make the Ce/Zr carrier with the precipitation method earlier, adopts infusion process to make again.This catalyst more than 96%, carry out the catalyst activity evaluation but this method is also undeclared under which kind of steam/hydrocarbons ratio condition, and operating temperature is also higher at 750 ℃ of following methane conversions.
Summary of the invention
The object of the invention is to provide the application of a kind of methane reforming catalyst in molten carbonate fuel cell, and its molten carbonate fuel cell that can operate under middle temperature low steam carbon ratio condition is used; Method for preparing catalyst is simple, and it can be operated under middle temperature, low steam carbon ratio condition, reactivity height, anti-carbon strong, good stability.
For achieving the above object, the invention provides the application of a kind of methane reforming catalyst in molten carbonate fuel cell, this catalyst comprises that content is that the active component nickel of 5-25wt%, rare earth element catalyst aid, the content that content is 0-10wt% are the alumina support of 65-95wt%.
In the above-mentioned catalyst, the content of active component nickel is preferably 10-25wt%.
Described rare earth element is one or more among Ce, La, Pr, Nd, Pm, Sm, Eu, the Gd, is preferably Ce and/or La; The content of described rare earth element is preferably 0-7wt%.
The present invention also provides a kind of molten carbonate fuel cell methane vapor reforming Preparation of catalysts method, and preparation process is as follows:
1). with alumina support under 600-800 ℃ of high temperature roasting 1-10 hour;
2). be dissolved in the deionized water by the soluble-salt of catalyst proportion of composing, the alumina support after the roasting is immersed in the described solution nickel, rare earth element, after dipping is complete, drying;
3). at 450 ℃ of roasting 2-10 hours, obtained described catalyst at 650 ℃ of following roasting 2-10 hours.
Described rare earth element is cerium and/or lanthanum.
The soluble-salt of described nickel, rare earth element is the nitrate of nitrate, cerium and/or the lanthanum of nickel.
Institute's controlling catalyst packed into carry out catalyst performance evaluation in the fixed bed reactors.Wherein reactor is a quartz reactor, internal diameter 10mm, high 800mm.Catalyst is used hydrogen reducing earlier at a certain temperature, carries out catalytic performance test then under 650 ℃.
Catalyst provided by the invention has following advantage:
1. the present invention adopts direct dipping process, and the preparation method is simple, and condition is controlled easily, and is with low cost.
2. catalyst catalytic performance height provided by the invention, under 650 ℃ of high temperature, steam/hydrocarbons ratio is that 2 o'clock methane conversions can reach 75%, H in the product
2/ CO (mol ratio) reaches 6-7.
3. catalyst provided by the invention has good carbon accumulation resisting ability and alkali resistant poisoning capability.Under 650 ℃ of high temperature, steam/hydrocarbons ratio is 1 o'clock, and the continuity of carrying out in molten carbonate fuel cell 55 hours is investigated, and catalyst activity there is no decline.
4. under 650 ℃ of high temperature, be 0.5 o'clock at ultralow steam/hydrocarbons ratio, methane conversion reaches 37%.
Description of drawings:
Fig. 1 carries out 55 hours stability experiments for 13.8%Ni catalyst in the embodiment of the invention 7 in molten carbonate fuel cell.Reaction temperature is 650 ℃, steam/hydrocarbons ratio S/C=1.
Embodiment
Embodiment 1:
The 19.7%Ni catalyst, the preparation method is as follows:
Take by weighing the Ni (NO of 6.0g
3)
26H
2O is dissolved in it in 2ml deionized water, treat that nitrate dissolves fully after, with 5.0g Al
2O
3Carrier impregnation is in Ni (NO
3)
2In the solution, treat that solution is adsorbed in carrier fully after, will put into 80 ℃ of insulating box inner drying 5h with the carrier of nitrate.With dried Al
2O
3Put into the Muffle furnace roasting, at 450 ℃ of following roasting 3h, roasting 3h under 650 ℃ of high temperature.
Taking by weighing the 1.0g catalyst packs into and carries out activity rating in the fixed bed quartz tube reactor.The quartz ampoule internal diameter is 10mm, high 800mm.Reactor feeds hydrogen and nitrogen mixture (mol ratio is 3: 7) with 3 ℃/min programming rate to 650 ℃, continue reduction 5h at 650 ℃, then hydrogen and nitrogen mixture are switched to methane and water, when S/C=2, estimate, methane conversion reaches 74.3%, and hydrogen yield is 71.8%.
Embodiment 2:
The 25%Ni catalyst, the preparation method is as follows:
Take by weighing 8.2g Ni (NO
3)
26H
2O is dissolved in it in 2.5ml deionized water, and subsequent step is with embodiment 1.
Catalyst carries out activity rating in quartz ampoule.Under 650 ℃, during S/C=2, methane conversion reaches 73.8%.
Embodiment 3:
Divide infusion process 3%Ce+17.7%Ni catalyst, the preparation method is as follows:
Take by weighing 0.56g Ce (NO
3)
36H
2O prepares the 3%Ce catalyst by embodiment 1 method.Take by weighing 5.3g Ni (NO again
3)
26H
2O is dissolved in it in appropriate amount of deionized water, and in nickel nitrate solution, subsequent step is with embodiment 1 with the 3%Ce catalyst soakage prepared.Obtain the catalyst of dipping Ce, back dipping Ni earlier.
Catalyst carries out activity rating in quartz ampoule.Under 650 ℃, during S/C=2, methane conversion reaches 73.9%, and hydrogen yield is 74.8%.
Embodiment 4:
Divide infusion process 19.7%Ni+3%Ce catalyst, the preparation method is as follows:
Take by weighing 6.0g Ni (NO
3)
26H
2O prepares the 19.7%Ni catalyst by embodiment 1 method.Take by weighing 0.57g Ce (NO again
3)
36H
2O is dissolved in it in appropriate amount of deionized water, and in cerous nitrate solution, subsequent step is with embodiment 1 with the 19.7%Ni catalyst soakage prepared.Obtain the catalyst of dipping Ni, back dipping Ce earlier.
Catalyst carries out activity rating in quartz ampoule.Under 650 ℃, methane conversion reaches 74.3% during S/C=2, and hydrogen yield is 76%.
Embodiment 5:
Flood the 15%Ni+5%Ce catalyst altogether, the preparation method is as follows:
Take by weighing 4.34g Ni (NO
3)
26H
2O and 0.54g Ce (NO
3)
36H
2O is dissolved in it in appropriate amount of deionized water together, and subsequent step is with embodiment 1.Obtain the catalyst of common dipping Ni and Ce.
Catalyst carries out activity rating in quartz ampoule.Under 650 ℃, during S/C=0.5, methane conversion reaches 37%, and hydrogen yield is 56.6%.
Embodiment 6:
Flood the 15%Ni+1.5%Ce+1.5%La catalyst altogether, the preparation method is as follows:
Take by weighing 4.34g Ni (NO
3)
26H
2O, 0.27g Ce (NO
3)
36H
2O and 0.27gNi (NO
3)
26H
2O is dissolved in it in appropriate amount of deionized water together, and subsequent step is with embodiment 1.Obtain the catalyst of common dipping Ni, Ce and La.
Catalyst is estimated in molten carbonate fuel cell.At S/C=1,650 ℃ of battery open circuit voltages that place an order can reach 1.151V, and three battery pack open circuit voltages reach 4.38V.
Embodiment 7:
The 13.8%Ni catalyst, the preparation method is as follows:
Take by weighing 4.0g Ni (NO
3)
26H
2O prepares the 13.8%Ni catalyst by embodiment 1 method.
This catalyst at S/C=1, is carried out 55 hours stability experiments under 650 ℃ in molten carbonate fuel cell, catalyst activity is undamped in 55 hours.See Fig. 1.
Comparative example 1:
The La/Ni/Al of WO 097319 preparation
2O
3Catalyst forms at 800-960 ℃ of following sintering by coprecipitation.This catalyst is adapted to methane vapor reforming and methane self-heating recapitalization, but this catalyst not under 650 ℃, low steam carbon ratio environment (S/C≤1) carry out catalytically active assessment, in MCFC, do not carry out activity and estimation of stability.
Comparative example 2:
Chinese patent CN1130256C discloses a kind of Mo-W catalyst, and this method for preparing catalyst comprises molybdenum tungsten solution impregnation in porous carrier, subsequently its carbonization is got the molybdenum tungsten carbide, passivation and getting under nitrogen environment again.This catalyst is at low steam carbon ratio (S/C=0.5), and (＞800 ℃) have higher methane conversion under the high temperature.But this catalyst does not carry out activity and estimation of stability yet in MCFC.
Comparative example 3:
Pressing the prepared catalyst of document (Catalysis Today 146 (2009) 148-153) report, is 700 ℃ in temperature, during S/C=1, and CH
4The conversion ratio maximum is about 35%.And press the common dipping 15%Ni+5%Ce catalyst of this patent method preparation, and under 650 ℃, CH during S/C=0.5
4Conversion ratio is about 37%.
Claims (8)
1. the application of methane reforming catalyst in molten carbonate fuel cell, it is characterized in that: this catalyst comprises that content is that the active component nickel of 5-25wt%, rare earth element catalyst aid, the content that content is 0-10wt% are the alumina support of 65-95wt%, and it can be used in the directly interior reformation molten carbonate fuel cell.
2. application according to claim 1 is characterized in that: the content of active component nickel is 10-25wt%.
3. application according to claim 1 is characterized in that: rare earth element is one or more among Ce, La, Pr, Nd, Pm, Sm, Eu, the Gd.
4. application according to claim 3 is characterized in that: rare earth element is Ce and/or La.
5. application according to claim 1 is characterized in that: the content of rare earth element is 0-7wt%.
6. application according to claim 1 is characterized in that: described Preparation of catalysts step is as follows:
1). with alumina support under 600-800 ℃ of high temperature roasting 1-10 hour;
2). be dissolved in the deionized water by the soluble-salt of catalyst proportion of composing, the alumina support after the roasting is immersed in the described solution nickel, rare earth element, after dipping is complete, drying;
3). at 450 ℃ of roasting 2-10 hours, obtained described catalyst at 650 ℃ of following roasting 2-10 hours.
7. application according to claim 6 is characterized in that: described rare earth element is cerium and/or lanthanum.
8. application according to claim 6 is characterized in that: the soluble-salt of nickel, rare earth element is the nitrate of nickel, cerium and/or lanthanum.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105642305A (en) * | 2014-12-06 | 2016-06-08 | 中国石油化工股份有限公司 | Preparation method of catalyst for methane steam reforming to produce hydrogen |
| CN105688916A (en) * | 2016-02-23 | 2016-06-22 | 中国科学院上海高等研究院 | High-dispersion high-load high-activity nickel-based catalyst for low-temperature methane reforming and application of high-dispersion high-load high-activity nickel-based catalyst for low-temperature methane reforming |
| CN105727955A (en) * | 2014-12-06 | 2016-07-06 | 中国石油化工股份有限公司 | Preparation method of catalyst for methane reforming with vapor to natural gas |
| CN108134102A (en) * | 2018-01-04 | 2018-06-08 | 四川天科技股份有限公司 | A kind of catalyst for methane steam reforming in fuel cell |
| CN112449615A (en) * | 2018-08-03 | 2021-03-05 | 株式会社新生能源研究 | Steam reforming catalyst |
| CN114011424A (en) * | 2021-11-26 | 2022-02-08 | 北京理工大学 | Composite carrier catalyst, preparation method and application |
| CN114471526A (en) * | 2020-10-27 | 2022-05-13 | 中国石油化工股份有限公司 | Reforming catalyst and preparation method and application thereof |
| CN115254130A (en) * | 2022-08-23 | 2022-11-01 | 辽宁大学 | Rare earth element Sm modified Ni-based water-resistant catalyst and preparation method and application thereof |
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| CN105642305A (en) * | 2014-12-06 | 2016-06-08 | 中国石油化工股份有限公司 | Preparation method of catalyst for methane steam reforming to produce hydrogen |
| CN105727955A (en) * | 2014-12-06 | 2016-07-06 | 中国石油化工股份有限公司 | Preparation method of catalyst for methane reforming with vapor to natural gas |
| CN105642305B (en) * | 2014-12-06 | 2017-10-27 | 中国石油化工股份有限公司 | A kind of method for preparing catalyst for hydrogen production from methane vapor reforming |
| CN105727955B (en) * | 2014-12-06 | 2018-01-16 | 中国石油化工股份有限公司 | A kind of preparation method of catalyst for hydrogen production from methane vapor reforming |
| CN105688916A (en) * | 2016-02-23 | 2016-06-22 | 中国科学院上海高等研究院 | High-dispersion high-load high-activity nickel-based catalyst for low-temperature methane reforming and application of high-dispersion high-load high-activity nickel-based catalyst for low-temperature methane reforming |
| CN105688916B (en) * | 2016-02-23 | 2018-10-26 | 中国科学院上海高等研究院 | A kind of high dispersive high load high activity low temperature methane reforming nickel-base catalyst and its application |
| CN108134102A (en) * | 2018-01-04 | 2018-06-08 | 四川天科技股份有限公司 | A kind of catalyst for methane steam reforming in fuel cell |
| CN112449615A (en) * | 2018-08-03 | 2021-03-05 | 株式会社新生能源研究 | Steam reforming catalyst |
| CN114471526A (en) * | 2020-10-27 | 2022-05-13 | 中国石油化工股份有限公司 | Reforming catalyst and preparation method and application thereof |
| CN114011424A (en) * | 2021-11-26 | 2022-02-08 | 北京理工大学 | Composite carrier catalyst, preparation method and application |
| CN114011424B (en) * | 2021-11-26 | 2024-04-16 | 北京理工大学 | Composite carrier catalyst, preparation method and application |
| CN115254130A (en) * | 2022-08-23 | 2022-11-01 | 辽宁大学 | Rare earth element Sm modified Ni-based water-resistant catalyst and preparation method and application thereof |
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Application publication date: 20111228 |