CN102389801A - Nickel-based catalyst for obtaining synthetic gas through carbon dioxide reforming of methane and preparation method for nickel-based catalyst - Google Patents
Nickel-based catalyst for obtaining synthetic gas through carbon dioxide reforming of methane and preparation method for nickel-based catalyst Download PDFInfo
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Abstract
The invention relates to the technical field of catalysts for obtaining synthetic gas through carbon dioxide reforming of methane, and discloses a nickel-based catalyst for obtaining the synthetic gas through the carbon dioxide reforming of the methane and a preparation method for the nickel-based catalyst. The nickel-based catalyst for obtaining the synthetic gas through the carbon dioxide reforming of the methane consists of NiO, MgO and gamma-Al2O3. The preparation method comprises the following steps of: 1, preparing a mixed solution; and 2, preparing the nickel-based catalyst. Compared with the prior art, the method has the advantages that: the methane conversion rate of the nickel-based catalyst is greatly improved, the service life is also greatly prolonged, and the carbon deposition rate is greatly reduced; and the nickel-based catalyst is low in cost and has better economy.
Description
Technical field
the present invention relates to the catalyst technical field that methane carbon dioxide reformation obtains synthesis gas, are nickel-base catalysts of a kind of methane carbon dioxide reformation acquisition synthesis gas and preparation method thereof.
Background technology
carbon dioxide is one of main gas that produces greenhouse effects.Face the poverty-stricken situation of global warming, how to make its recycling, more and more become one of human hot issue of paying close attention to the most.Utilize the methane carbon dioxide reformation technology; Preparation synthesis gas (mixture of carbon monoxide and hydrogen), synthetic through F-T then, preparation oxygenatedchemicals or liquid fuel; For alleviating energy crisis; Low carbon emission reduction, utilization of waste as resource is significant to progressively realizing human society entering sustainable development pattern.
are having under the catalyst condition, and carbon dioxide conversion can reach more than 90%; Under the catalyst-free condition, carbon dioxide and methane reaction, its conversion ratio is almost nil.
common infusion process is to prepare one of the most frequently used method of methane carbon dioxide reformation catalyst at present.
One of document " synthetic chemistry " 2008.Vo1.16. № 5.495～498 by Guo Fang, Chu Wei, Huang Liqiong, Xie Zaiku deliver " the carrier Acidity of Aikalinity is to CO
2
/ CH
4
Reforming reaction is with the influence of nickel-base catalyst " literary composition, it adopts common immersion process for preparing methane carbon dioxide reformation catalyst.Discover Ni/MgO-Al
2
O
3
Catalyst shows better catalytic activity and higher reaction yield.
" the CeO that two " catalysis journal " 2003.Vol.28. № 2.19～22 of document is delivered by Jin Mingshan, rope palm bosom, Xu Xiufeng, strange generation
2
To supporting the CH of Ni catalyst
4
With CO
2
The influence that reforming reaction is active " literary composition, it has investigated the catalytic activity of support type Ni catalyst in the methane carbon dioxide reformation reaction of common immersion process for preparing.Life experiment result behind the reaction 40h shows Ni/CeO
2
/ Al
2
O
3
Catalyst not only has very high methane and carbon dioxide activity of conversion, and demonstrates good anti-carbon deposit performance.
So far though infusion process still is a kind of method of using always, proving effective of Preparation of Catalyst, there are some drawbacks in
, like low, the poor activity of catalyst life of preparation etc.
Summary of the invention
the invention provides a kind of methane carbon dioxide reformation and obtain nickel-base catalyst of synthesis gas and preparation method thereof; Overcome the problem that above-mentioned prior art exists, its catalyst has advantages such as methane conversion height, selectivity is good, the life-span is long.
One of technical scheme of the present invention realizes through following measure: a kind of methane carbon dioxide reformation obtains the nickel-base catalyst of synthesis gas, and it consists of nickel oxide 5% to 15%, magnesia 2% to 10% and gama-alumina 75% to 93% by mass percent; This nickel-base catalyst obtains by following step:
First step preparation mixed solution: with Ni (NO
3
)
2
6H
2
O, Mg (NO
3
)
2
6H
2
O and deionized water are the preparation of raw material mixed solution; In this mixed solution, Ni (NO
3
)
2
Concentration be 0.2 mol/L to 0.5mol/L, Mg (NO
3
)
2
Concentration is 0.3 mol/L to 0.6mol/L;
Second step preparation: earlier with γ-Al
2
O
3
Add in the Rotary Evaporators, heating vacuumizes, and is heated to 40 ℃ to 60 ℃, and vacuum reaches under the 0.065MPa to 0.085MPa, keeps 5 minutes to 10 minutes; Under above-mentioned vacuum, above-mentioned first step gained mixed solution is added in the above-mentioned Rotary Evaporators, and make the solid in the Rotary Evaporators be immersed in the mixed solution fully; Under above-mentioned vacuum, keep 30 ℃ to 50 ℃ of liquidus temperatures, under the rotation condition, kept 20 hours to 30 hours; Then, in above-mentioned vacuum and rotation down, be warmed up to 60 ℃ to 80 ℃, drying or be evaporated to no liquid phase obtains solid content; At last, 650 ℃ under 750 ℃, with this solid content roasting 4 hours to 6 hours, promptly prepare nickel-base catalyst.
Can further carry out following selection or/and optimize to one of technical scheme of the invention described above:
Rotary speed in
above-mentioned second step is controlled at 160 rev/mins to 200 rev/mins.
The reduction activation process of
above-mentioned nickel-base catalyst is undertaken by following step: this nickel-base catalyst is filled in the reaction tube, with the heating rate of 5 ℃/min to 15 ℃/min this nickel-base catalyst is carried out heating reduction; When temperature reached 200 ℃, the flow velocity feeding hydrogen with 0.25 m/min to 0.45m/min was raised to 750 ℃ to 800 ℃ until temperature, picks up counting, and continues to obtain in 3 hours to 5 hours the nickel-base catalyst of reduction activation.
Two of technical scheme of the present invention realizes through following measure: a kind ofly obtain the preparation method of the nickel-base catalyst of synthesis gas according to above-mentioned methane carbon dioxide reformation, it is undertaken by following step:
First step preparation mixed solution: with Ni (NO
3
)
2
6H
2
O, Mg (NO
3
)
2
6H
2
O and deionized water are the preparation of raw material mixed solution; In this mixed solution, Ni (NO
3
)
2
Concentration be 0.2 mol/L to 0.5mol/L, Mg (NO
3
)
2
Concentration is 0.3 mol/L to 0.6mol/L;
Second step preparation: earlier with γ-Al
2
O
3
Add in the Rotary Evaporators, heating vacuumizes, and is heated to 40 ℃ to 60 ℃, and vacuum reaches under the 0.065MPa to 0.085MPa, keeps 5 minutes to 10 minutes; Under above-mentioned vacuum, above-mentioned first step gained mixed solution is added in the above-mentioned Rotary Evaporators, and make the solid in the Rotary Evaporators be immersed in the mixed solution fully; Under above-mentioned vacuum, keep 30 ℃ to 50 ℃ of liquidus temperatures, under the rotation condition, kept 20 hours to 30 hours; Then, in above-mentioned vacuum and rotation down, be warmed up to 60 ℃ to 80 ℃, drying or be evaporated to no liquid phase obtains solid content; At last, 650 ℃ under 750 ℃, with this solid content roasting 4 hours to 6 hours, promptly prepare nickel-base catalyst.
Two of technical scheme of the present invention realizes through following measure:
Rotary speed in
above-mentioned second step is controlled at 160 rev/mins to 200 rev/mins.
The reduction activation process of
above-mentioned nickel-base catalyst is undertaken by following step: this nickel-base catalyst is filled in the reaction tube, with the heating rate of 5 ℃/min to 15 ℃/min this nickel-base catalyst is carried out heating reduction; When temperature reached 200 ℃, the flow velocity feeding hydrogen with 0.25 m/min to 0.45m/min was raised to 750 ℃ to 800 ℃ until temperature, picks up counting, and continues to obtain in 3 hours to 5 hours the nickel-base catalyst of reduction activation.
good effect of the present invention is: relative with prior art; The methane conversion of gained nickel-base catalyst of the present invention has increased significantly, the life-span also is greatly improved, coke deposit rate has had significantly reduction, and cost of the present invention is low, economy is better.
The specific embodiment
the present invention does not receive the restriction of following embodiment, can confirm concrete embodiment according to technical scheme of the present invention and actual conditions.
further describe the present invention below in conjunction with embodiment.
Embodiment 1, and the nickel-base catalyst that this methane carbon dioxide reformation obtains synthesis gas consists of nickel oxide 5% to 15%, magnesia 2% to 10% and gama-alumina 75% to 93% by mass percent; The preparation method that this methane carbon dioxide reformation obtains the nickel-base catalyst of synthesis gas is undertaken by following step:
First step preparation mixed solution: with Ni (NO
3
)
2
6H
2
O, Mg (NO
3
)
2
6H
2
O and deionized water are the preparation of raw material mixed solution; In this mixed solution, Ni (NO
3
)
2
Concentration be 0.2 mol/L to 0.5mol/L, Mg (NO
3
)
2
Concentration is 0.3 mol/L to 0.6mol/L;
Second step preparation: earlier with γ-Al
2
O
3
Add in the Rotary Evaporators, heating vacuumizes, and is heated to 40 ℃ to 60 ℃, and vacuum reaches under the 0.065MPa to 0.085MPa, keeps 5 minutes to 10 minutes; Under above-mentioned vacuum, above-mentioned first step gained mixed solution is added in the above-mentioned Rotary Evaporators, and make the solid in the Rotary Evaporators be immersed in the mixed solution fully; Under above-mentioned vacuum, keep 30 ℃ to 50 ℃ of liquidus temperatures, under the rotation condition, kept 20 hours to 30 hours; Then, in above-mentioned vacuum and rotation down, be warmed up to 60 ℃ to 80 ℃, drying or be evaporated to no liquid phase obtains solid content; At last, 650 ℃ under 750 ℃, with this solid content roasting 4 hours to 6 hours, promptly prepare nickel-base catalyst.
embodiment 2 is with the difference of embodiment 1: the rotary speed in above-mentioned second step is controlled at 160 rev/mins to 200 rev/mins.
embodiment 3 is with the difference of embodiment 1 to 2: the rotary speed in above-mentioned second step is controlled at 160 rev/mins or 200 rev/mins.
embodiment 4; The reduction activation process of embodiment 1 to 3 gained nickel-base catalyst is undertaken by following step: this nickel-base catalyst is filled in the reaction tube, with the heating rate of 5 ℃/min to 15 ℃/min this nickel-base catalyst is carried out heating reduction; When temperature reached 200 ℃, the flow velocity feeding hydrogen with 0.25 m/min to 0.45m/min was raised to 750 ℃ to 800 ℃ until temperature, picks up counting, and continues to obtain in 3 hours to 5 hours the nickel-base catalyst of reduction activation.
embodiment 5; The reduction activation process of embodiment 1 to 3 gained nickel-base catalyst is undertaken by following step: this nickel-base catalyst is filled in the reaction tube, with the heating rate of 5 ℃/min or 15 ℃/min this nickel-base catalyst is carried out heating reduction; When temperature reached 200 ℃, the flow velocity feeding hydrogen with 0.25 m/min or 0.45m/min was raised to 750 ℃ or 800 ℃ until temperature, picks up counting, and continues 3 hours or obtained in 5 hours the nickel-base catalyst of reduction activation.
in the present invention: except as otherwise herein provided, the unit of percentage % all is a mass percent.
The foregoing description gained nickel-base catalyst is tested: after above-mentioned nickel-base catalyst reduction process finishes, switch to reaction gas, react down at 750 ℃ to 850 ℃, wherein reaction gas CO
2
/ CH
4
=1～1.5 (volume ratios), GHSV=1500～6000ml/hgCat.; After reaction finished, the question response pipe was cooled to room temperature, took out catalyst.
The average result that
are tested is following: methane conversion reaches 95% to 100%, and carbon dioxide conversion reaches 80% to 90%, and selectivity is 90% to 97%, and coke deposit rate≤1.9mg/gCath reacts 240 hours not inactivations.
The evaluation experimental that catalyst in one of document is done under 700 ℃ is: at reaction gas CO
2
/ CH
4
Under=1 (volume ratio) condition, methane conversion is 67.50%; React after 6 hours, methane conversion is 64.36%.
Document two in the evaluation experimental under 750 ℃, done of catalyst be: at reaction gas CO
2
/ CH
4
=1 (volume ratio), GHSV=6000h
-1
Under the condition, in reaction time 40h, keep methane conversion 96%, carbon dioxide conversion 86%, coke deposit rate are 2.4mg/gCath.
the present invention with the comparative analysis of prior art is: compare with one of document, though evaluation experimental reaction temperature of the present invention is higher than 700 ℃, methane conversion has increased significantly, and the life-span also is greatly improved.Compare with two of document, though methane of the present invention and carbon dioxide conversion are very nearly the same, the life-span also has increased significantly, and coke deposit rate has had significantly reduction.In addition, auxiliary agent of the present invention is a magnesium (Mg) (more cheap), and two auxiliary agent of document is cerium (Ce) (expensive).This shows that also cost of the present invention is low, economy is better.
Claims (6)
1. the nickel-base catalyst of a methane carbon dioxide reformation acquisition synthesis gas is characterized in that consisting of nickel oxide 5% to 15%, magnesia 2% to 10% and gama-alumina 75% to 93% by mass percent; This nickel-base catalyst obtains by following step:
First step preparation mixed solution: with Ni (NO
3)
26H
2O, Mg (NO
3)
26H
2O and deionized water are the preparation of raw material mixed solution; In this mixed solution, Ni (NO
3)
2Concentration be 0.2 mol/L to 0.5mol/L, Mg (NO
3)
2Concentration is 0.3 mol/L to 0.6mol/L;
Second step preparation: earlier with γ-Al
2O
3Add in the Rotary Evaporators, heating vacuumizes, and is heated to 40 ℃ to 60 ℃, and vacuum reaches under the 0.065MPa to 0.085MPa, keeps 5 minutes to 10 minutes; Under above-mentioned vacuum, above-mentioned first step gained mixed solution is added in the above-mentioned Rotary Evaporators, and make the solid in the Rotary Evaporators be immersed in the mixed solution fully; Under above-mentioned vacuum, keep 30 ℃ to 50 ℃ of liquidus temperatures, under the rotation condition, kept 20 hours to 30 hours; Then, in above-mentioned vacuum and rotation down, be warmed up to 60 ℃ to 80 ℃, drying or be evaporated to no liquid phase obtains solid content; At last, 650 ℃ under 750 ℃, with this solid content roasting 4 hours to 6 hours, promptly prepare nickel-base catalyst.
2. methane carbon dioxide reformation according to claim 1 obtains the nickel-base catalyst of synthesis gas, it is characterized in that the rotary speed in second step is controlled at 160 rev/mins to 200 rev/mins.
3. methane carbon dioxide reformation according to claim 1 and 2 obtains the nickel-base catalyst of synthesis gas; The reduction activation process that it is characterized in that this nickel-base catalyst is undertaken by following step: this nickel-base catalyst is filled in the reaction tube, with the heating rate of 5 ℃/min to 15 ℃/min this nickel-base catalyst is carried out heating reduction; When temperature reached 200 ℃, the flow velocity feeding hydrogen with 0.25 m/min to 0.45m/min was raised to 750 ℃ to 800 ℃ until temperature, picks up counting, and continues 3 hours to 5 hours, obtains the nickel-base catalyst of reduction activation.
4. a methane carbon dioxide reformation obtains the preparation method of the nickel-base catalyst of synthesis gas, it is characterized in that being undertaken by following step:
First step preparation mixed solution: with Ni (NO
3)
26H
2O, Mg (NO
3)
26H
2O and deionized water are the preparation of raw material mixed solution; In this mixed solution, Ni (NO
3)
2Concentration be 0.2 mol/L to 0.5mol/L, Mg (NO
3)
2Concentration is 0.3 mol/L to 0.6mol/L;
Second step preparation: earlier with γ-Al
2O
3Add in the Rotary Evaporators, heating vacuumizes, and is heated to 40 ℃ to 60 ℃, and vacuum reaches under the 0.065MPa to 0.085MPa, keeps 5 minutes to 10 minutes; Under above-mentioned vacuum, above-mentioned first step gained mixed solution is added in the above-mentioned Rotary Evaporators, and make the solid in the Rotary Evaporators be immersed in the mixed solution fully; Under above-mentioned vacuum, keep 30 ℃ to 50 ℃ of liquidus temperatures, under the rotation condition, kept 20 hours to 30 hours; Then, in above-mentioned vacuum and rotation down, be warmed up to 60 ℃ to 80 ℃, drying or be evaporated to no liquid phase obtains solid content; At last, 650 ℃ under 750 ℃, with this solid content roasting 4 hours to 6 hours, promptly prepare nickel-base catalyst.
5. methane carbon dioxide reformation according to claim 4 obtains the preparation method of the nickel-base catalyst of synthesis gas, it is characterized in that the rotary speed in second step is controlled at 160 rev/mins to 200 rev/mins.
6. obtain the preparation method of the nickel-base catalyst of synthesis gas according to claim 4 or 5 described methane carbon dioxide reformations; The reduction activation process that it is characterized in that this nickel-base catalyst is undertaken by following step: this nickel-base catalyst is filled in the reaction tube, with the heating rate of 5 ℃/min to 15 ℃/min this nickel-base catalyst is carried out heating reduction; When temperature reached 200 ℃, the flow velocity feeding hydrogen with 0.25 m/min to 0.45m/min was raised to 750 ℃ to 800 ℃ until temperature, picks up counting, and continues to obtain in 3 hours to 5 hours the nickel-base catalyst of reduction activation.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102974353A (en) * | 2012-12-07 | 2013-03-20 | 新疆大学 | NiO/gamma-Al2O3 catalyst of methane and carbon dioxide reforming synthesis gas and method for preparing NiO/gamma-Al2O3 catalyst of methane and carbon dioxide reforming synthesis gas |
| CN104383927A (en) * | 2014-11-17 | 2015-03-04 | 太原理工大学 | Catalyst for methane and carbon dioxide reforming synthesis gas and preparation method of catalyst |
| CN104549558A (en) * | 2013-10-24 | 2015-04-29 | 中国石油化工股份有限公司 | Reducing method of semi-regenerative reforming catalyst |
| CN105413734A (en) * | 2015-12-07 | 2016-03-23 | 西南化工研究设计院有限公司 | Nickel-based catalyst for preparing reducing gas by reforming methane-carbon dioxide and preparation method of nickel-based catalyst |
| CN105498852A (en) * | 2014-09-26 | 2016-04-20 | 中国石油化工股份有限公司 | Nickel-based catalyst carrier and preparation method and application thereof, and nickel-based catalyst and preparation method and application thereof |
| CN106423172A (en) * | 2016-08-26 | 2017-02-22 | 内江师范学院 | Embedded type hollow structural nickel-based catalyst for carbon dioxide thermal reforming and preparation method thereof |
| CN106607032A (en) * | 2015-10-21 | 2017-05-03 | 中国石油化工股份有限公司 | Methane dry reforming catalyst, preparation method and application thereof and method for preparing synthesis gas through methane dry reforming |
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|---|---|---|---|---|
| CN102974353A (en) * | 2012-12-07 | 2013-03-20 | 新疆大学 | NiO/gamma-Al2O3 catalyst of methane and carbon dioxide reforming synthesis gas and method for preparing NiO/gamma-Al2O3 catalyst of methane and carbon dioxide reforming synthesis gas |
| CN102974353B (en) * | 2012-12-07 | 2014-11-26 | 新疆大学 | NiO/gamma-Al2O3 catalyst of methane and carbon dioxide reforming synthesis gas and method for preparing NiO/gamma-Al2O3 catalyst of methane and carbon dioxide reforming synthesis gas |
| CN104549558A (en) * | 2013-10-24 | 2015-04-29 | 中国石油化工股份有限公司 | Reducing method of semi-regenerative reforming catalyst |
| CN104549558B (en) * | 2013-10-24 | 2016-08-24 | 中国石油化工股份有限公司 | A kind of method of reducing of semi regeneration reforming catalyst |
| CN105498852B (en) * | 2014-09-26 | 2018-06-15 | 中国石油化工股份有限公司 | Nickel catalyst agent carrier and its preparation method and application and nickel-base catalyst and its preparation method and application |
| CN105498852A (en) * | 2014-09-26 | 2016-04-20 | 中国石油化工股份有限公司 | Nickel-based catalyst carrier and preparation method and application thereof, and nickel-based catalyst and preparation method and application thereof |
| CN104383927B (en) * | 2014-11-17 | 2016-06-01 | 太原理工大学 | The Catalysts and its preparation method of a kind of methane and CO 2 reformation preparing synthetic gas |
| CN104383927A (en) * | 2014-11-17 | 2015-03-04 | 太原理工大学 | Catalyst for methane and carbon dioxide reforming synthesis gas and preparation method of catalyst |
| CN106607032A (en) * | 2015-10-21 | 2017-05-03 | 中国石油化工股份有限公司 | Methane dry reforming catalyst, preparation method and application thereof and method for preparing synthesis gas through methane dry reforming |
| CN105413734A (en) * | 2015-12-07 | 2016-03-23 | 西南化工研究设计院有限公司 | Nickel-based catalyst for preparing reducing gas by reforming methane-carbon dioxide and preparation method of nickel-based catalyst |
| CN105413734B (en) * | 2015-12-07 | 2020-05-26 | 西南化工研究设计院有限公司 | Nickel-based catalyst for preparing reducing gas by reforming methane-carbon dioxide and preparation method thereof |
| CN106423172A (en) * | 2016-08-26 | 2017-02-22 | 内江师范学院 | Embedded type hollow structural nickel-based catalyst for carbon dioxide thermal reforming and preparation method thereof |
| CN106423172B (en) * | 2016-08-26 | 2018-11-20 | 内江师范学院 | The inlaid hollow structure nickel-base catalyst and preparation method of carbon dioxide thermal reforming |
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