CN102500385A - NiO/Cel-xPrxO2 catalyst for ethanol steam reforming reaction and preparation method thereof - Google Patents
NiO/Cel-xPrxO2 catalyst for ethanol steam reforming reaction and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an NiO/Cel-xPrxO2 catalyst for ethanol steam reforming reaction and a preparation method thereof, which belong to the technical field of loaded metal catalysts for hydrocarbon reforming. The catalyst takes Cel-xPrxO2 as a carrier and Ni as an active component, the mass ratio of NiO to the carrier is between 0.01 and 0.2. The preparation method of the catalyst comprises the steps that: A solution is prepared from Ce and Pr nitrate in a certain molar ratio and Ni nitrate and the carrier in the mass ratio; B solution is prepared from Na2CO3 and NaOH in the molar ratio; according to the ratio (2:1) of solute materials in the B solution to solute materials in the A solution, the A and B solution is mixed, aged and dried; and an obtained solid material is roasted, and the NiO/Cel-xPrxO2 catalyst is obtained. The catalyst and the preparation method thereof have the advantages that: a preparation process is simple, the prepared catalyst has good reaction activity, higher hydrogen selectivity and better anti-carbon deposition performance.
Description
Technical field
The present invention relates to a kind of ethanol steam reforming reaction NiO/Ce that is used for
1-xPr
xO
2Catalyst and preparation method belong to the load type metal catalyst technology that hydrocarbon is reformed.
Background technology
Ethanol steam reforming (SRE) catalyst mainly comprises: oxide type catalyst, noble metal type catalyst, and base metal type catalyst.Non-precious metal catalyst mainly with Cu, Ni, Co as active component.For nickel-base catalyst, Al
2O
3, MgO, SiO
2And CeO
2-ZrO
2Deng often being used as carrier.With Ni/Al
2O
3Catalyst is an example, and it reaches 91% at ethanol conversion more than 500 ℃, and contains 70% (φ) H in the gas of reaction back
2But, Al
2O
3Acidity cause carbon deposit more serious, less stable.The easy carbon distribution of copper-based catalysts, and the accessory substance that generates is more, copper-based catalysts easy-sintering under higher temperature in addition.
Ni is catalyst based to receive people's favor because of it has selectivity and the cheap relatively price that high reforming activity becomes reconciled.Metal Ni can promote the fracture of ethanol C-C, helps the ethanol gasification, thereby reduces accessory substance (like acetone, acetate, acetaldehyde etc.).But be used for the SRE part that also comes with some shortcomings as the catalyst of active component with Ni.For example metal Ni at high temperature, particularly under the condition that steam exists, sintering causes the catalyst activity specific area to descend the catalyst permanent deactivation easily.Except the particle sintering, the carbon distribution in the reforming process also is to cause another main cause of the catalyst based inactivation of Ni.Through the carrier of selecting for use some to have special nature, or add auxiliary agent or strengthen the interaction between metal-carrier, can so that these shortcomings of Ni series catalysts significantly improved.Wherein, CeO
2Have good storage oxygen performance, redox property and produce preferably and interact, in catalytic reaction, be widely used with carried metal.CeO
2On its surface and body all can generate the oxygen room mutually, the oxygen room can activation the oxygen molecule of absorption, thereby make its with carbon distribution reaction elimination catalyst on the carbon distribution that deposits.In addition, CeO
2And the interaction between the metal active constituent of load can be avoided the sintering of metal nanoparticle, thereby improves the stability of catalyst.
In recent years, Yang Yu etc. have prepared the Ni series catalysts of different carriers load with equi-volume impregnating, and have investigated the influence of carrier for the hydrogen production by ethanol steam reforming reactivity worth.The result shows, under 650 ℃, 101.3kPa, different carriers for ethanol all near transforming fully, but to the hydrogen selective size order is: ZnO ≈ La
2O
3＞CeO
2＞ZrO
2The author thinks that the interaction degree between Ni and carrier can influence catalyst activity and selectivity.A little less than interacting, when active component exists with NiO basically mutually, selection of catalysts property is lower; Too by force, do not have the NiO phase time when interacting, activity of such catalysts and selectivity are all very low; Stronger when interacting, when part Ni and carrier function generated new thing and coexist mutually mutually and with NiO, activity of such catalysts and selectivity were the highest.Wang Jian etc. have prepared NiO/CeO with coprecipitation
2Catalyst, and be used for the ethanol steam reforming reaction.This catalyst is in the time of 550 ℃, and ethanol conversion is 99.3%, the selectivity about 55% of hydrogen.
At present, be mainly about the used catalyst carrier of ethanol steam reforming reaction: CeO
2, ZnO, MgO, perovskite, ZrO etc. did not see use Ce as yet
1-xPr
xO
2Pertinent literature report as catalyst carrier.Therefore, this patent proposes a kind of NEW TYPE OF COMPOSITE oxide type support C e first
1-xPr
xO
2And preparation method thereof, and with its carrier as the ethanol steam reforming reaction.Catalyst through the coprecipitation preparation
NiO/Ce
1-xPr
xO
2Can make Ni and carrier produce stronger interaction, make that the particle diameter of this catalyst active component Ni after reducing is very little and be the surface that high dispersion state is distributed in carrier; In addition, this composite oxide carrier Ce
1-xPr
xO
2Can promote CeO through mixing of Pr
2Redox property, help generating more oxygen room, thereby improve the anti-carbon performance of catalyst.This catalyst series through the coprecipitation preparation has higher activity and hydrogen selective.
The content invention
The object of the invention is to provide a kind of ethanol steam reforming reaction NiO/Ce that is used for
1-xPr
xO
2Catalyst and preparation method, this catalyst shows good reaction activity, higher hydrogen selective in the entire reaction temperature range, possess anti-carbon performance preferably simultaneously.Its preparation method process is simple.
The present invention realizes through following technical proposals, a kind of ethanol steam reforming reaction NiO/Ce that is used for
1-xPr
xO
2Catalyst is characterized in that: this catalyst particle size 0.1mm～10mm, and with Ce
1-xPr
xO
2Be carrier, Ce wherein,, the mol ratio of Pr is (1-x): x, x is between 0～0.5; Ni is an active component, and the mass ratio of NiO and carrier is between 0.01～0.2.
Above-mentioned Preparation of catalysts method is characterized in that comprising following process:
1) press Ce,, the mol ratio of Pr is (1-x): x, x is in 0～0.5 interval; The mass ratio of NiO and carrier is between 0.01～0.2, takes by weighing Ce (NO
3)
36H
2O, Pr (NO
3)
36H
2O, Ni (NO
3)
36H
2O is dissolved in the deionized water, stirs to obtain A solution;
2) press Na
2CO
3With the mol ratio of NaOH be 1: 1, it is added deionized water is made into B solution;
3) ratio according to the material of solute in the amount of solute substance in the solution B and the solution A is 2: 1; The pH value that is added to A, two kinds of solution of B and drip in the container and controls precipitated liquid is 9～11; Stir precipitation reaction 0.5～1h; Continue to stir 4～6h at ambient temperature; Aging 24h; Subsequent filtration spends the deionised water filter cake up to sedimentary pH＜7.5, and gained sediment dry 18～24h in 60～120 ℃ thermostatic drying chamber obtains solids;
4) solids that step 3) is obtained is 3～10 ℃/min at the roasting kiln roasting with heating rate, is warming up to 550～750 ℃ of roasting 3～5h, obtains NiO/Ce
1-xPr
xO
2Catalyst.
Advantage of the present invention has: this catalyst adopts coprecipitation, and a step makes supported complex oxide catalyst and catalyst carrier Ce
1-xPr
xO
2NiO in the course of reaction
xBe reduced, and high dispersive is at Ce
1-xPr
xO
2On the carrier, this catalyst has good reaction activity, higher hydrogen selective, and it possesses anti-carbon performance preferably simultaneously.Active testing shows catalyst 10,000～500,000h
-1In the air speed scope, this catalyst can make ethanol transform fully at a lower temperature and have higher hydrogen selective.
Description of drawings:
Fig. 1 is for using the made catalyst of embodiment 2 and embodiment 4, and ethanol conversion is with temperature variation curve.
Among the figure: curve 1 is for using the catalyst of embodiment 2 systems, and ethanol conversion is with temperature variation curve; Curve 2 is for using the catalyst of embodiment 4 systems, and ethanol conversion is with temperature variation curve.
Fig. 2 is 10% (wt) NiO/Ce before and after the prereduction
0.7Pr
0.3O
2XRD figure spectrum.
Among the figure: curve 1 is reduction back 10% (wt) NiO/Ce
0.7Pr
0.3O
2The XRD figure spectrum of catalyst; Curve 2 is reduction preceding 10% (wt) NiO/Ce
0.7Pr
0.3O
2The XRD figure spectrum of catalyst.
Fig. 3 is for using the made catalyst of embodiment 3, and ethanol conversion and products distribution are with the change curve of reaction temperature.
Among the figure: curve 1 is for using the made catalyst of embodiment 3, and ethanol conversion is with temperature variation curve; Curve 2 is for using the made catalyst of embodiment 3, and hydrogen selective is with temperature variation curve; Curve 3 is for using the made catalyst of embodiment 3, and the acetaldehyde selectivity is with temperature variation curve; Curve 4 is for using the made catalyst of embodiment 3, and CO is with temperature variation curve; Curve 5 is for using the made catalyst of embodiment 3, CO
2With temperature variation curve; Curve 6 is for using the made catalyst of embodiment 3, CH
4With temperature variation curve.
Fig. 4 is embodiment 2 and the DTA-TG spectrogram of the made catalyst sample behind 650 ℃ of reaction 8h of embodiment 4.
Among the figure: curve 1 is the thermogravimetric curve behind the embodiment 2 prepared catalyst reactions; Curve 2 is the thermogravimetric curve behind the embodiment 4 prepared catalyst reactions; Curve 3 is embodiment 2 prepared catalyst differential thermal analysis curves; Curve 4 is embodiment 4 prepared catalyst differential thermal analysis curves.
The specific embodiment
Catalyst preparation process is following: weigh in the balance and get Ce (NO
3)
36H
2O 4.605g, Pr (NO
3)
36H
2O1.967g, Ni (NO
3)
36H
2O 0.101g, (Ce and Pr mol ratio 7: 3, NiO are 0.01 with the ratio of the mass fraction of carrier) is dissolved in the 80ml deionized water, and stirring obtains A solution.Take by weighing Na
2CO
31.593g, NaOH 0.625g (Na
2CO
3With the mol ratio of NaOH be 1: 1), add the 50ml deionized water and be made into B solution, A, two kinds of mixed solutions of B and drip are added, the pH value of control precipitated liquid in 9～11 scopes, constantly stirring.After dripping off, continue to stir 4h at ambient temperature, aging 24h.Subsequent filtration, up to PH＜7.5, the gained sediment is dry 24h in 80 ℃ thermostatic drying chamber with the deionized water cyclic washing.The solid that obtains is at the roasting kiln roasting, and roasting process is: at 750 ℃ of following roasting 4h, heating rate is 5 ℃/min.Obtain catalyst 2.300g, yield is 88%.
Will more than make catalyst and be used for ethanol steam reforming and prepare hydrogen-rich gas:
The performance test of catalyst is carried out on micro fixed-bed reactor, will consist of 25vol.% ethanol, 75vol.% steam, and all the other are N
2, be 100 with air speed, 000h
-1Feed reactor, react at 350～650 ℃.Catalyst amount is 75mg, 40～60 orders.Use N before the reaction earlier
2Purged 60 minutes, and used the H of 5vol.% again
2-Ar gaseous mixture, flow velocity are 50ml/min, 450 ℃ of following reduction 60min of temperature programming.After reduction finishes, change temperature to the reaction temperature that needs, with the mixed solution of micro pump input second alcohol and water, the mol ratio of ethanol and water is 1: 3, gets into reactor 140 ℃ of vaporizer vaporization backs and begins reaction.Adopt SP2100 type gas-chromatography to carry out on-line analysis, separate H with the TDX-01 molecular sieve column
2, N
2, CO, CO
2And CH
4, carrier gas is high-purity He, flow velocity is 30ml/min; Separate H with Porapak-Q
2Products such as O, ethanol, acetaldehyde and acetone, carrier gas is high-purity H
2, flow velocity is 30ml/min.TCD detects.
Test result is following: 1%Ni/Ce
0.7Pr
0.3O
2In the time of 650 ℃ ethanol near conversion ratio, the hydrogen selective average is on 75% in the probe temperature interval.
Catalyst preparation process is following: weigh in the balance and get Ce (NO
3)
36H
2O 4.605g, Pr (NO
3)
36H
2O1.967g, Ni (NO
3)
36H
2O 1.610g, (Ce and Pr mol ratio 7: 3, NiO are 0.16 with the ratio of the mass fraction of carrier) is dissolved in the 80ml deionized water, and stirring obtains A solution.Take by weighing Na
2CO
31.593g, NaOH 0.625g (Na
2CO
3With the mol ratio of NaOH be 1: 1), add the 50ml deionized water and be made into B solution, A, two kinds of mixed solutions of B and drip are added, the pH value of control precipitated liquid in 9～11 scopes, constantly stirring.After dripping off, continue to stir 4h at ambient temperature, aging 24h.Subsequent filtration, up to PH＜7.5, the gained sediment is dry 24h in 80 ℃ thermostatic drying chamber with the deionized water cyclic washing.The solid that obtains is at the roasting kiln roasting, and roasting process is: at 750 ℃ of following roasting 4h, heating rate is 5 ℃/min.Obtain catalyst 2.789g, yield is 93%.
Will more than make catalyst and be used for ethanol steam reforming and prepare hydrogen-rich gas, the condition of reorganization is with embodiment 1.Test result is following: 16% (wt) NiO/Ce
0.7Pr
0.3O
2Ethanol conversion has reached 82.19% in the time of 400 ℃, and ethanol transforms fully in the time of 500 ℃.The hydrogen selective average is near 65% in the probe temperature interval.Behind 650 ℃ of reaction 8h, catalyst performance is tested the same embodiment 2 with this catalyst, and test result shows 16% (wt) NiO/Ce
0.7Pr
0.3O
2Have good anti-carbon performance, it has a small weightlessness near 100 ℃, and weight-loss ratio is 1.57%, does not occur obvious weightless peak in the high temperature range.
Catalyst preparation process is following: weigh in the balance and get Ce (NO
3)
36H
2O 4.605g, Pr (NO
3)
36H
2O1.967g, Ni (NO
3)
36H
2O 2.013g, (Ce and Pr mol ratio 7: 3, NiO are 0.2 with the ratio of the mass fraction of carrier) is dissolved in the 80ml deionized water, and stirring obtains A solution.Take by weighing Na
2CO
31.593g, NaOH 0.625g (Na
2CO
3With the mol ratio of NaOH be 1: 1), add the 50ml deionized water and be made into B solution, A, two kinds of solution of B and drip are added, the pH value of control precipitated liquid in 9～11 scopes, constantly stirring.After dripping off, continue to stir 4h at ambient temperature, aging 24h.Subsequent filtration, up to PH＜7.5, the gained sediment is dry 24h in 80 ℃ thermostatic drying chamber with the deionized water cyclic washing.The solid that obtains is at the roasting kiln roasting, and roasting process is: at 750 ℃ of following roasting 4h, heating rate is 5 ℃/min.Obtain catalyst 2.792g, yield is 90%.
Catalyst preparation process is following: weigh in the balance and get Ce (NO
3)
36H
2O 6.579g, Ni (NO
3)
36H
2O1.005g, (Ce and Pr mol ratio 1: 0, NiO are 0.1 with the ratio of the mass fraction of carrier) is dissolved in the 80ml deionized water, and stirring obtains A solution.Take by weighing Na
2CO
31.593g, NaOH 0.625g (Na
2CO
3With the mol ratio of NaOH be 1: 1), add the 50ml deionized water and be made into B solution, A, two kinds of mixed solutions of B and drip are added, the pH value of control precipitated liquid in 9～11 scopes, constantly stirring.After dripping off, continue to stir 4h at ambient temperature, aging 24h.Subsequent filtration, up to PH＜7.5, the gained sediment is dry 24h in 80 ℃ thermostatic drying chamber with the deionized water cyclic washing.The solid that obtains is at the roasting kiln roasting, and roasting process is: at 750 ℃ of following roasting 4h, heating rate is 5 ℃/min.Obtain catalyst 2.725g, yield is 91%.
Will more than make catalyst and be used for ethanol steam reforming and prepare hydrogen-rich gas, the condition of reorganization is with embodiment 1.Test result is following: 16% (wt) NiO/CeO
2Catalyst ethanol conversion in the time of 400 ℃ is merely 43%, even ethanol is not realized transforming fully yet in the time of 650 ℃.
Embodiment 5
Catalyst preparation process is following: weigh in the balance and get Ce (NO
3)
36H
2O 3.257g, Pr (NO
3)
46H
2O3.263g, Ni (NO
3)
36H
2O 1.007g, (Ce and Pr mol ratio 1: 1, NiO are 0.1 with the ratio of the mass fraction of carrier) is dissolved in the 80ml deionized water, and stirring obtains A solution.Take by weighing Na
2CO
31.593g, NaOH 0.625g (Na
2CO
3With the mol ratio of NaOH be 1: 1), add the 50ml deionized water and be made into B solution, A, two kinds of mixed solutions of B and drip are added, the pH value of control precipitated liquid in 9～11 scopes, constantly stirring.After dripping off, continue to stir 4h at ambient temperature, aging 24h.Subsequent filtration, up to PH＜7.5, the gained sediment is dry 24h in 80 ℃ thermostatic drying chamber with the deionized water cyclic washing.The solid that obtains is at the roasting kiln roasting, and roasting process is: at 750 ℃ of following roasting 4h, heating rate is 5 ℃/min.Obtain catalyst 2.562g, yield is 90%.
Claims (2)
1. one kind is used for ethanol steam reforming reaction NiO/Ce
1-xPr
xO
2Catalyst is characterized in that: this catalyst particle size 0.1mm～10mm, and with Ce
1-xPr
xO
2Be carrier, Ce wherein,, the mol ratio of Pr is (1-x): x, x is between 0～0.5; Ni is an active component, and the mass ratio of NiO and carrier is between 0.01～0.2.
2. one kind prepares the described ethanol steam reforming reaction NiO/Ce that is used for of claim 1
1-xPr
xO
2The method of catalyst is characterized in that comprising following process:
1) press Ce,, the mol ratio of Pr is (1-x): x, x is in 0～0.5 interval; The mass ratio of NiO and carrier is between 0.01～0.2, takes by weighing Ce (NO
3)
36H
2O, Pr (NO
3)
36H
2O, Ni (NO
3)
36H
2O is dissolved in the deionized water, stirs to obtain A solution;
2) press Na
2CO
3With the mol ratio of NaOH be 1: 1, it is added deionized water is made into B solution;
3) ratio according to the material of solute in the amount of solute substance in the solution B and the solution A is 2: 1; The pH value that is added to A, two kinds of solution of B and drip in the container and controls precipitated liquid is 9～11; Stir precipitation reaction 0.5～1h; Continue to stir 4～6h at ambient temperature; Aging 24h; Subsequent filtration spends the deionised water filter cake up to sedimentary pH＜7.5, and gained sediment dry 18～24h in 60～120 ℃ thermostatic drying chamber obtains solids;
4) solids that step 3) is obtained is 3～10 ℃/min at the roasting kiln roasting with heating rate, is warming up to 550～750 ℃ of roasting 3～5h, obtains NiO/Ce
1-xPr
xO
2Catalyst.
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|---|---|---|---|
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103908968A (en) * | 2014-04-01 | 2014-07-09 | 广西科技大学 | Hydrogen preparing catalyst composed of praseodymium-zirconium-nickel-ferrite-copper oxides and preparation method thereof |
| CN108671927A (en) * | 2018-04-28 | 2018-10-19 | 中国科学院工程热物理研究所 | Composite catalyst and preparation method, the hydrogen production process of hydrogen production from methanol-steam reforming |
| CN111389404A (en) * | 2020-01-21 | 2020-07-10 | 天津大学 | Preparation method and application of cerium oxide supported nickel catalyst |
| CN114160149A (en) * | 2021-12-08 | 2022-03-11 | 中国科学院生态环境研究中心 | Cu-based catalyst for hydrogen production by oxidation and reforming of ethanol and preparation method and application thereof |
| CN115069242A (en) * | 2022-05-05 | 2022-09-20 | 有研工程技术研究院有限公司 | Catalyst for hydrogen production by oxidation and reforming of ethanol and preparation and activation methods thereof |
-
2011
- 2011-10-26 CN CN2011103274584A patent/CN102500385A/en active Pending
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| J.L. YE ET AL.: "Steam reforming of ethanol over Ni/CexTi1-xO2 catalysts", 《INTERNATIONAL JOURNAL OF HYDROGEN ENERGY》 * |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103908968A (en) * | 2014-04-01 | 2014-07-09 | 广西科技大学 | Hydrogen preparing catalyst composed of praseodymium-zirconium-nickel-ferrite-copper oxides and preparation method thereof |
| CN103908968B (en) * | 2014-04-01 | 2016-01-06 | 广西科技大学 | Catalyst for preparing hydrogen be made up of praseodymium zirconium ferronickel Cu oxide and preparation method thereof |
| CN108671927A (en) * | 2018-04-28 | 2018-10-19 | 中国科学院工程热物理研究所 | Composite catalyst and preparation method, the hydrogen production process of hydrogen production from methanol-steam reforming |
| CN108671927B (en) * | 2018-04-28 | 2022-08-23 | 中国科学院工程热物理研究所 | Composite catalyst for hydrogen production by methanol steam reforming, preparation method and hydrogen production method |
| CN111389404A (en) * | 2020-01-21 | 2020-07-10 | 天津大学 | Preparation method and application of cerium oxide supported nickel catalyst |
| CN114160149A (en) * | 2021-12-08 | 2022-03-11 | 中国科学院生态环境研究中心 | Cu-based catalyst for hydrogen production by oxidation and reforming of ethanol and preparation method and application thereof |
| CN114160149B (en) * | 2021-12-08 | 2023-06-16 | 中国科学院生态环境研究中心 | Cu-based catalyst for ethanol oxidation reforming hydrogen production and preparation method and application thereof |
| CN115069242A (en) * | 2022-05-05 | 2022-09-20 | 有研工程技术研究院有限公司 | Catalyst for hydrogen production by oxidation and reforming of ethanol and preparation and activation methods thereof |
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Application publication date: 20120620 |