CN101733129A - Aurum-copper bimetallic catalyst for oxidating CO at low temperature under rich hydrogen condition and preparation method thereof - Google Patents
Aurum-copper bimetallic catalyst for oxidating CO at low temperature under rich hydrogen condition and preparation method thereof Download PDFInfo
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- CN101733129A CN101733129A CN200910175309A CN200910175309A CN101733129A CN 101733129 A CN101733129 A CN 101733129A CN 200910175309 A CN200910175309 A CN 200910175309A CN 200910175309 A CN200910175309 A CN 200910175309A CN 101733129 A CN101733129 A CN 101733129A
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- rich hydrogen
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- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
Abstract
The invention relates to an aurum-copper bimetallic catalyst for oxidating CO at low temperature under a rich hydrogen condition. The aurum-copper bimetallic catalyst is characterized in that: the catalyst consists of a CeO2 oxide carrier and an active component Au-Cu; the loading capacity of Au in the active component is 0.1 to 0.5 weight percent; the loading capacity of Cu is 1 to 4 weight percent; and the balance is the carrier. A preparation method for the aurum-copper bimetallic catalyst comprises the following steps: preparing a ceria carrier by a sol-gel method; and loading the active component on the carrier by a deposition-precipitation method. The prepared catalyst has the advantages that: the catalyst has high-efficient catalytic activity and can realize full removal of the CO in the rich hydrogen atmosphere within a temperature range of between 60 and 130 DEG C, the preparation condition is simple, the loading capacity of the Au is effectively reduced and the cost is reduced.
Description
Technical field
The invention belongs to a kind of aurum-copper bimetallic catalyst and preparation method who is used for oxidating CO at low temperature under rich hydrogen condition.
Background technology
Proton Exchange Membrane Fuel Cells PEMFC (proton exchange membrane fuelcell) has following advantage: its power generation process does not relate to oxyhydrogen combustion, thereby is not subjected to the restriction of Carnot cycle, the energy conversion rate height; Do not produce pollution during generating, power generating modulesization, the reliability height, assembling and maintenance are all very convenient, also do not have noise during work.So PEMFC is a kind of cleaning, environmental protection power supply efficiently, be suitable as very much the electrical source of power of automobile of future generation.
The problem that present PEMFC needs solution badly is the elimination problem of the CO of 0.5-1% in the methanol reformed gas, because the maximum patience of fuel cell Pt electrode pair CO is no more than 100ppm.So CO concentration will be eliminated less than 100ppm in advance.Up to the present, the CO selective oxidation is proved to be the easiest the most effective method.
The CO selective oxidation has had the history in more than 40 year under the rich hydrogen condition.Up to the present mainly be divided into two big classes: a class is to be the noble metal catalyst of representative with Pt, Pd, Ru, Rh, Au, though noble metal catalyst has advantages such as reaction temperature is low, but because its reserves are few, price is high, selection of catalysts is low etc. shortcoming, this has limited its further application.One-component oxide or composite oxides, particularly CuO-CeO such as base metal such as Cu, Mn, Co, Ni, Fe
2Catalyst is all showing α-Fe than Au/ aspect active and the selectivity
2O
3And Pt/Al
2O
3Catalytic performance and economy that two class catalyst are more superior.But base metal also have its reaction temperature higher, to water and the unsettled shortcoming of carbon dioxide.
Summary of the invention
It is low to the purpose of this invention is to provide a kind of reaction temperature, the catalytic activity height, good stability be used for aurum-copper bimetallic catalyst of oxidating CO at low temperature under rich hydrogen condition and preparation method thereof.
Catalyst of the present invention is by CeO
2Oxide carrier and active component A u-Cu form, and the load capacity of Au is 0.1-0.5wt% in the active component, and the load capacity of Cu is 1-4wt%, and surplus is a carrier.
Preparation method of the present invention is with Prepared by Sol Gel Method nano-oxide support C eO
2, then active component is impregnated into it on carrier with the deposition-precipitation method.
Preparation of catalysts method of the present invention is as follows:
1) cerous nitrate is dissolved in deionized water, stirs, dropwise add in the aqueous solution of precipitating reagent, after dropwising, the pH value scope of precipitation supernatant must maintain in the 9-14 scope, leaves standstill 20-24h under the room temperature condition;
2) will precipitate suction filtration, washing 4-6 time with deionized water, and wash 3-4 time with absolute ethyl alcohol exchange, 110-120 ℃ of dry 12-20h is that 2-10 ℃/min is warmed up to 400-600 ℃ of roasting 4-6h with the heating rate in the air atmosphere, obtains CeO
2Carrier;
3) ceria supports is dissolved in the water, stirs, its pH is controlled in the 12-14 scope, stir 0.5-1h to wherein adding precipitating reagent.
4) copper nitrate is dissolved in the water, in it, presses catalyst ratio and add chlorauric acid solution, stir.
5) with 4) in the solution for preparing under constantly stirring, dropwise joining 3) in, after dropwising, pH value scope must maintain and continue stirring 1-2h in the 9-12 scope, will precipitate filtering and washing, 110 ℃ of dry 12-20h, 200-400 ℃ of roasting 3-5h in the air atmosphere.
Aforesaid precipitating reagent is NaOH or Na
2CO
3.
The carbon monoxide that catalyst of the present invention is specially adapted in the fuel-cell vehicle hydrogen source system is eliminated, and also is applicable to removing of CO pernicious gas under the low temperature aerobic conditions.
Compared with the prior art the present invention has following substantive distinguishing features:
1) is that the CO that the catalyst system and catalyzing of active component is applied in the hydrogen rich gas atmosphere removes with the Au-Cu bimetallic, still belongs to the first time.
2) Zhi Bei catalyst has very high activity and selectivity, and it is 60 ℃ that the CO under the realization rich hydrogen condition eliminates minimum temperature fully, and corresponding selectivity is 62.8%.
3) Zhi Bei catalyst has the reaction temperature window of broad, and catalyst can be 60-140 ℃ of elimination fully that realizes CO.
4) catalyst is than CuO/CeO
2Catalyst has lower reaction temperature, high catalytic activity.
The specific embodiment
The catalyst of this method preparation carries out CO catalytic oxidation performance evaluation on the microreactor on the microreactor of normal pressure continuous-flow.With the 0.20-0.50g catalyst reactor of packing into, catalyst 250-350 ℃ through air preliminary treatment 1 hour, estimate then.Mix CO, CO in the gas before and after adopting GC-8A gas chromatograph (FID) analytical reactions
2Concentration, wherein the chromatographic column adopting carbon molecular sieve separates, and the methanator of dress Ni catalyst in one of the series connection behind the post makes CO and CO after the separation
2Successively all be converted into methane, and then enter flame ionization ditector.Analyzing the concentration of oxygen change detector with the GC-8A gas chromatograph is thermal conductivity cell detector (TCD), and the analytical column inserts is the 13X molecular sieve.The reaction raw materials overall flow rate is 100mlmin
-1, gas composition is CO: O
2: H
2: N
2=1: 1: 50: 48.
Embodiment 1
1) gets Ce (NO
3)
36H
2O 6.7g is dissolved in the 400ml deionized water, stirs, and note is made a.The 20ml ammonia solvent in the 200ml deionized water, is stirred, and note is made b.Solution among a is dropwise joined (rate of addition is 15ml/min) among the b, stir, pH is that 2h is stirred in 10 continuation after dropwising.Leave standstill 20h under the room temperature condition, use deionized water filtration washing 4 times, each consumption 100ml uses 200ml absolute ethanol washing 4 times, 110 ℃ of dry 12h.In air atmosphere, with 500 ℃ of roasting 4h of Muffle furnace, heating rate is 10 ℃/min.Make CeO
2
2) get that to contain the CuO mass percent be 7.7% copper nitrate solution 0.260g and to contain the Au mass percent be that 0.48% 1g gold chloride is added drop-wise in the 20ml deionized water, stir, obtain golden copper mixed liquor.
3) weighing 2gCeO
2, join in the 150ml deionized water, add 10ml0.5mol/L Na then
2CO
3, make that pH value of solution is 13, stir 1h.Under constantly stirring, golden copper mixed liquor is dropwise added, final solution pH value is 10.Dropwise the back and continue to stir 2h, filtration washing then, 110 ℃ of dry 10h are that 2 ℃/min is warmed up to 300 ℃ of roasting 5h with heating rate in air atmosphere.
The Au that makes
0.25Cu
1.0/ CeO
2Catalyst is CO: O in gas composition
2: H
2: N
2=1: carry out the temperature programming active testing in 1: 50: 48, just can realize the complete oxidation under the CO rich hydrogen condition for 80-140 ℃, the highest selectivity is 49.8%.
Embodiment 2
1) gets Ce (NO
3)
36H
2O 6.7g g is dissolved in the 400ml deionized water, stirs, and note is made a.The 25ml ammonia solvent in the 200ml deionized water, is stirred, and note is made b.Solution among a is dropwise joined (rate of addition is 15ml/min) among the b, stir, pH is that 3h is stirred in 12 continuation after dropwising.Leave standstill 20h under the room temperature condition, use deionized water filtration washing 5 times, each consumption 100ml uses 150ml absolute ethanol washing 3 times, 120 ℃ of dry 20h.In air atmosphere, with 500 ℃ of roasting 4h of Muffle furnace, heating rate is 2 ℃/min.Make CeO
2
2) get that to contain the CuO mass percent be that 7.7% copper nitrate solution 0.650g and the 0.5g gold chloride that contains Au mass percent 0.48% are added drop-wise in the 25ml deionized water, stir, obtain golden copper mixed liquor.
3) weighing 2gCeO
2Grind to form fine powder, be dissolved in the 100ml deionized water, add 0.5mol/L Na then
2CO
310ml makes that pH value of solution is 13, stirs 0.5h.Under constantly stirring, with 2) dropwise add, final solution pH value is 9.Dropwise the back and continue to stir 1.5h, filtration washing then, 110 ℃ of dry 10h are that 2 ℃/min is warmed up to 400 ℃ of roasting 3h with heating rate in air atmosphere.
The Au that makes
0.12Cu
2.5/ CeO
2Catalyst is CO: O in gas composition
2: H
2: N
2=1: carry out the temperature programming active testing in 1: 50: 48, just can realize the complete oxidation under the CO rich hydrogen condition for 85-140 ℃, the highest selectivity is 52.8%.
Embodiment 3
1) gets Ce (NO
3)
36H
2O 6.7g is dissolved in the 400ml deionized water, stirs, and note is made a.The 20ml ammonia solvent in the 200ml deionized water, is stirred, and note is made b.Solution among a is dropwise joined (rate of addition is 15ml/min) among the b, stir, pH is that 1h is stirred in 13 continuation after dropwising.Leave standstill 20h under the room temperature condition, use deionized water filtration washing 5 times, each consumption 100ml uses 200ml absolute ethanol washing 4 times, 120 ℃ of dry 12h.In air atmosphere, with roasting 4h in 400 ℃ of air atmospheres of Muffle furnace, heating rate is 8 ℃/min.Make CeO
2
2) get that to contain the CuO mass percent be that 7.7% copper nitrate solution 0.650g and the 2g gold chloride that contains Au mass percent 0.48% are added drop-wise in the 25ml deionized water, stir, obtain golden copper mixed liquor.
3) weighing 2gCeO
2Grind to form fine powder, be dissolved in the 150ml deionized water, add 0.1mol/L NaOH 10ml then and make that pH value of solution is 14, stir 1h.Under constantly stirring, golden copper mixed liquor is dropwise added, final solution pH value is 11.Dropwise the back and continue to stir 1.5h, filtration washing then, 110 ℃ of dry 15h are that 2 ℃/min is warmed up to 300 ℃ of roasting 3h with heating rate in air atmosphere.
The Au that makes
0.5Cu
5.0/ CeO
2Catalyst is CO: O in gas composition
2: H
2: N
2=1: carry out the temperature programming active testing in 1: 50: 48, just can realize the complete oxidation under the CO rich hydrogen condition for 60-130 ℃, the highest selectivity is 62.8%.
Embodiment 4
1) gets Ce (NO
3)
36H
2O 6.7g is dissolved in the 300ml deionized water, stirs, and note is made a.The 20ml ammonia solvent in the 200ml deionized water, is stirred, and note is made b.Solution among a is dropwise joined (rate of addition is 15ml/min) among the b, stir, pH is that 1.5h is stirred in 13 continuation after dropwising.Leave standstill 20h, filtration washing 4 times is used 200ml absolute ethanol washing 4 times, 110 ℃ of dry 15h.In air atmosphere, with 400 ℃ of roasting 4h of Muffle furnace, heating rate is 6 ℃/min.Make CeO
2
2) get that to contain the CuO mass percent be that 7.7% copper nitrate solution 0.650g and the 1g gold chloride that contains Au mass percent 0.48% are added drop-wise in the 25ml deionized water, stir, obtain golden copper mixed liquor.
3) weighing 2gCeO
2Grind to form fine powder, be dissolved in the 150ml deionized water, add 0.1mol/L NaOH 10ml then and make that pH value of solution is 14, stir 1h.Under constantly stirring, golden copper mixed liquor is dropwise added, final solution pH value is 12.Dropwise the back and continue to stir 1.5h, filtration washing then, 110 ℃ of dry 15h are that 2 ℃/min is warmed up to 300 ℃ of roasting 5h with heating rate in air atmosphere.
The Au that makes
0.25Cu
2.5/ CeO
2Catalyst is CO: O in gas composition
2: H
2: N
2=1: carry out the temperature programming active testing in 1: 50: 48, just can realize the complete oxidation under the CO rich hydrogen condition for 70-135 ℃, the highest selectivity is 60.5%.
Embodiment 5
1) gets Ce (NO
3)
36H
2O 6.7g is dissolved in the 300ml deionized water, stirs, and note is made a.The 30ml ammonia solvent in the 200ml deionized water, is stirred, and note is made b.Solution among a is dropwise joined (rate of addition is 15ml/min) among the b, stir, pH is 14 after dropwising, and continues to stir 3h.Leave standstill 20h under the room temperature condition, use deionized water filtration washing 5 times, each consumption 1000ml uses 2000ml absolute ethanol washing 4 times, 110 ℃ of dry 12h.In air atmosphere, with 400 ℃ of roasting 4h of Muffle furnace, heating rate is 3 ℃/min.Make CeO
2
2) get that to contain the CuO mass percent be that 7.7% copper nitrate solution 0.260g and the 1g gold chloride that contains Au mass percent 0.48% are added drop-wise in the 20ml deionized water, stir, obtain golden copper mixed liquor.
3) weighing 2gCeO
2Grind to form fine powder, be dissolved in the 150ml deionized water, add 0.1mol/L NaOH 5ml then and make that pH value of solution is 13, stir 1h.Under constantly stirring, golden copper mixed liquor is dropwise added, final solution pH value is 10.Dropwise the back and continue to stir 1.5h, filtration washing then, 110 ℃ of dry 15h are that 2 ℃/min is warmed up to 300 ℃ of roasting 3h with heating rate in air atmosphere.
The Au that makes
0.1Cu
1.0/ CeO
2Catalyst is CO: O in gas composition
2: H
2: N
2=1: carry out the temperature programming active testing in 1: 50: 48, just can realize the complete oxidation under the CO rich hydrogen condition for 90-130 ℃, the highest selectivity is 66.5%.
Embodiment 6
1) gets Ce (NO
3)
36H
2O 6.7g is dissolved in the 450ml deionized water, stirs, and note is made a.The 40ml ammonia solvent in the 200ml deionized water, is stirred, and note is made b.Solution among a is dropwise joined (rate of addition is 15ml/min) among the b, stir, pH is 14 after dropwising, and continues to stir 1h.Leave standstill 22h under the room temperature condition, use deionized water filtration washing 5 times, each consumption 1000ml uses 1500ml absolute ethanol washing 3 times, 110 ℃ of dry 12h.In air atmosphere, with 400 ℃ of roasting 4h of Muffle furnace, heating rate is 4 ℃/min.Make CeO
2
2) get that to contain the CuO mass percent be that 7.7% copper nitrate solution 1.30g and the 2g gold chloride that contains Au mass percent 0.48% are added drop-wise in the 25ml deionized water, stir, obtain golden copper mixed liquor.
3) weighing 2gCeO
2Grind to form fine powder, be dissolved in the 150ml deionized water, add 0.1mol/L NaOH 7.5ml then and make that pH value of solution is 14, stir 1h.Under constantly stirring, golden copper mixed liquor is dropwise added, final solution pH value is 10.Dropwise the back and continue to stir 1.5h, filtration washing then, 110 ℃ of dry 15h are that 2 ℃/min is warmed up to 200 ℃ of roasting 4h with heating rate in air atmosphere.
The Au that makes
0.5Cu
5.0/ CeO
2Catalyst is CO: O in gas composition
2: H
2: N
2=1: carry out the temperature programming active testing in 1: 50: 48, just can realize the complete oxidation under the CO rich hydrogen condition for 65-140 ℃, the highest selectivity is 57.8%.
Claims (3)
1. an aurum-copper bimetallic catalyst that is used for oxidating CO at low temperature under rich hydrogen condition is characterized in that catalyst is by CeO
2Oxide carrier and active component A u-Cu form, and the load capacity of Au is 0.1-0.5wt% in the active component, and the load capacity of Cu is 1-4wt%, and surplus is a carrier.
2. a kind of aurum-copper bimetallic catalyst preparation method who is used for oxidating CO at low temperature under rich hydrogen condition as claimed in claim 1 is characterized in that comprising the steps:
1) cerous nitrate is dissolved in deionized water, stirs, dropwise add in the aqueous solution of precipitating reagent, after dropwising, the pH value scope of precipitation supernatant must maintain in the 9-14 scope, leaves standstill 20-24h under the room temperature condition;
2) will precipitate suction filtration, washing 4-6 time with deionized water, and wash 3-4 time with absolute ethyl alcohol exchange, 110-120 ℃ of dry 12-20h is that 2-10 ℃/min is warmed up to 400-600 ℃ of roasting 4-6h with the heating rate in the air atmosphere, obtains CeO
2Carrier;
3) ceria supports is dissolved in the water, stirs, its pH is controlled in the 12-14 scope, stir 0.5-1h to wherein adding precipitating reagent.
4) copper nitrate is dissolved in the water, in it, presses catalyst ratio and add chlorauric acid solution, stir.
5) with 4) in the solution for preparing under constantly stirring, dropwise joining 3) in, after dropwising, pH value scope must maintain and continue stirring 1-2h in the 9-12 scope, will precipitate filtering and washing, 110 ℃ of dry 12-20h, 200-400 ℃ of roasting 3-5h in the air atmosphere.
3. a kind of preparation method who is used for the aurum-copper bimetallic catalyst of oxidating CO at low temperature under rich hydrogen condition as claimed in claim 1 is characterized in that described precipitating reagent is NaOH or Na
2CO
3
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102728847A (en) * | 2011-04-02 | 2012-10-17 | 中国科学院大连化学物理研究所 | Preparation method for gold-copper bimetal nanospheres |
| CN102989483A (en) * | 2012-12-13 | 2013-03-27 | 北京化工大学常州先进材料研究院 | Preparation method of high-stability Au-Cu/LaMnO3 catalyst |
| CN103007961A (en) * | 2012-12-13 | 2013-04-03 | 北京化工大学常州先进材料研究院 | Catalyst for eliminating CO in hydrogen source of fuel cell and preparation method of catalyst |
| CN107774269A (en) * | 2017-09-14 | 2018-03-09 | 天津大学 | Co deposited synthesis copper ceria catalyst, preparation method and application |
| CN110678630A (en) * | 2017-04-04 | 2020-01-10 | 巴斯夫公司 | On-board ammonia and hydrogen generation |
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| CN115646510A (en) * | 2022-10-25 | 2023-01-31 | 中国石油大学(华东) | Catalyst for CO selective oxidation reaction and preparation method thereof |
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| CN1045549C (en) * | 1993-11-26 | 1999-10-13 | 中国科学技术大学 | Three-effect catalyst and preparing method containing copper and lanthanum-oxides, platinum and rhodium |
| BG62723B1 (en) * | 1997-09-29 | 2000-06-30 | "Ламан-Консулт"Оод | Gold catalyst and its application in fuel components |
| CN101549296B (en) * | 2009-05-06 | 2011-01-12 | 中国科学院山西煤炭化学研究所 | Method for preparing water-resistant carbon-dioxide-resistant CO low-temperature oxidation catalyst |
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| CN102728847A (en) * | 2011-04-02 | 2012-10-17 | 中国科学院大连化学物理研究所 | Preparation method for gold-copper bimetal nanospheres |
| CN102989483A (en) * | 2012-12-13 | 2013-03-27 | 北京化工大学常州先进材料研究院 | Preparation method of high-stability Au-Cu/LaMnO3 catalyst |
| CN103007961A (en) * | 2012-12-13 | 2013-04-03 | 北京化工大学常州先进材料研究院 | Catalyst for eliminating CO in hydrogen source of fuel cell and preparation method of catalyst |
| CN110678630A (en) * | 2017-04-04 | 2020-01-10 | 巴斯夫公司 | On-board ammonia and hydrogen generation |
| CN110678630B (en) * | 2017-04-04 | 2023-10-31 | 巴斯夫公司 | On-board ammonia and hydrogen generation |
| CN107774269A (en) * | 2017-09-14 | 2018-03-09 | 天津大学 | Co deposited synthesis copper ceria catalyst, preparation method and application |
| CN114011406A (en) * | 2021-11-28 | 2022-02-08 | 辽宁石油化工大学 | Ruthenium-based oxide catalyst, preparation method and application |
| CN114011406B (en) * | 2021-11-28 | 2023-10-17 | 辽宁石油化工大学 | Ruthenium-based oxide catalyst, preparation method and application |
| CN115646510A (en) * | 2022-10-25 | 2023-01-31 | 中国石油大学(华东) | Catalyst for CO selective oxidation reaction and preparation method thereof |
| CN115646510B (en) * | 2022-10-25 | 2024-04-16 | 中国石油大学(华东) | Catalyst for CO selective oxidation reaction and preparation method thereof |
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