CN101530809A - Catalyst for preparing synthesis gas, preparation method and application - Google Patents
Catalyst for preparing synthesis gas, preparation method and application Download PDFInfo
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- CN101530809A CN101530809A CN200910074205A CN200910074205A CN101530809A CN 101530809 A CN101530809 A CN 101530809A CN 200910074205 A CN200910074205 A CN 200910074205A CN 200910074205 A CN200910074205 A CN 200910074205A CN 101530809 A CN101530809 A CN 101530809A
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- synthesis gas
- nickel
- silicon nitride
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
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Abstract
A catalyst for preparing synthesis gas takes silicon nitride as a carrier and metallic nickel as an active ingredient. The weight percents of the nickel and the silicon nitride are respectively 1-50wt% and 50-99wt%. The active ingredient nickel is loaded on the surface of the silicon nitride by dipping to prepare the catalyst for preparing synthesis gas. The catalyst has the advantages of high conversion rate, little carbon deposit and long life, etc.
Description
Technical field
The present invention relates to a kind of Catalysts and its preparation method, relate in particular to the Catalysts and its preparation method that a kind of methane portion oxidation or methane carbon dioxide reformation prepare synthesis gas.
Background technology
The China's oil resource is poor relatively, and existing petroleum resources far can not satisfy fuel consume and the chemical industry demand to petroleum resources.Therefore, seek the new energy and chemical industry resource, become and be badly in need of one of key issue that solves.Comparatively speaking, natural gas of China and coal bed gas resource reserves are abundant, as a kind of new energy and chemical industry raw material, are expected to become the substitute of petroleum resources, but their energy densities are low, be difficult for compression, transportation, storage, thereby limited its application in the energy and other association area.Therefore, how natural gas and coal bed gas are converted into and are easy to the high added value fluid product that transports and use, become the important topic that various countries' researcher faces.Because the main component of natural gas and coal bed gas all is a methane, so the key link that natural gas and coal bed gas are converted into chemicals is exactly a methane conversion.Methane portion oxidation and methane carbon dioxide reformation prepare synthesis gas, and synthetic then other chemicals is a kind of effective way of efficiently utilizing natural gas and coal bed gas resource.Because methane portion oxidation carries out under high temperature, high-speed, catalyst activity component easy-sintering, loss, and the easy carbon deposit of catalyst in the course of reaction cause catalyst activity reduction.And synthesizing gas by reforming methane with co 2 is a strong endothermic reaction, and energy consumption is big and catalyst carbon deposition is serious.Therefore, developing the catalyst with active height, good stability is the key of methane preparing synthetic gas research work.
The existing bibliographical information of Catalysts and its preparation method for preparing at present synthesis gas about methane partial oxygen and methane carbon dioxide reformationization, as: Chinese patent (application number: disclose a kind of catalyst that is used for methane portion oxidation synthesis gas 200810071152.5), this catalyst is an active component with transition metal Co and noble metal, alkaline-earth metal is an auxiliary agent, γ-Al
2O
3Be carrier.Chinese patent (application number: the catalyst that discloses a kind of methane portion oxidation synthesis gas 200310109658.8).This catalyst is carrier with the high-ratio surface silicon carbide, and nickel is active component, and rare-earth oxide is an auxiliary agent.Wherein: nickel oxide 6-25%, rare-earth oxide 0-6%, carborundum 69-94%.Chinese patent (application number: disclose a kind of partial oxidation of methane that is used for 200610102307.8) and be equipped with synthetic gas catalyst and preparation method thereof.This catalyst is active component with nickel, is carrier with spherical biological pattern carborundum.It is characterized by: nickel oxide 5-20%, oxides additive 2-25%, carborundum 55-99%.(application number: disclose a kind of catalyst that is used for synthesizing gas by reforming methane with co 2 00106166.6), this catalyst is active component with nickel to Chinese patent, with ultra-fine ZrO
2Be carrier.Chinese patent (application number: disclose a kind of catalyst that is used for the nano-crystal oxide nickel-loaded of synthesizing gas by reforming methane with co 2 00124421.3).The percentage by weight of the constituent of this catalyst is: nickel: 3-30%, nanocrystalline being oxidized to: 70-97%, described nano-crystal oxide are zirconium dioxide or magnesia.Chinese patent (application number: the catalyst that discloses a kind of methane carbon dioxide reformation and methane portion oxidation coupled reaction sulfuration bed preparing synthetic gas 03129073.6).This catalyst is a carrier with the microsphere silica gel of alkaline earth metals calcium, strontium and barium modification, is the bimetallic catalyst of active component with nickel.The catalyst that the methane portion oxidation of present exploitation and methane carbon dioxide reformation prepare synthesis gas is mainly made catalyst carrier with oxide material.Such catalyst causes sintering of catalyst and carbon distribution easily because the heat conductivility of self is relatively poor in course of reaction; And Carboround is having remarkable result aspect anti-sintering that improves catalyst and the carbon distribution, but in course of reaction, still has a spot of carbon distribution to exist, thereby influences the service life of catalyst.Therefore, how improving the heat endurance and the heat-conductive characteristic of catalyst material, is one of key link that solves such catalyst coking and inactivation.
Summary of the invention
The objective of the invention is to solve present methane portion oxidation or methane carbon dioxide reformation and prepare the poor stability that exists in the synthetic gas catalyst and easy problem such as carbon distribution inactivation, develop the catalyst and the preparation method that methane portion oxidation or methane carbon dioxide reformation prepare synthesis gas that can be used for of a kind of catalytic activity height and good stability.
The present invention is by the realization of following method, the soluble metal nickel salt is dissolved in distilled water or the anhydrous ethanol solvent, silicon nitride is immersed in the above-mentioned solution then, under certain condition slaine is deposited on the silicon nitride surface, after the oven dry roasting, can obtain partial oxidation of methane and be equipped with synthetic gas catalyst.The evaluation experimental of catalyst is finished on fixed bed reactors, and the qualitative and quantitative result of gas component finishes by gas-chromatography.
Catalyst of the present invention is carrier with the silicon nitride material, and metallic nickel is an active component, and its percentage by weight consists of:
Nickel 1-50wt% silicon nitride 50-99wt%.
The specific area of aforesaid silicon nitride is 5-100m
2/ g.
Method for preparing catalyst of the present invention is:
(1), compound concentration is the soluble nickel salting liquid of 1-20wt%;
(2), under stirring condition, the silicon nitride carrier is immersed in the above-mentioned nickel salt solution, the part by weight of nickel salt and silicon nitride is 4.7-83:100; Under 20-60 ℃ of temperature, stirred 1-12 hour, the Ph value that abundant mixing makes solvent evaporates or regulator solution is deposited on the carrier surface active component to 6-10;
(3), under 60-150 ℃ of condition, in air, dry, 400 ℃-800 ℃ roasting 1-6 hour, promptly can be used for the catalyst that methane portion oxidation or methane carbon dioxide reformation prepare synthesis gas.
Aforesaid soluble nickel salt comprises nickel nitrate, nickel acetate or nickelous sulfate.
The Application of Catalyst condition
1, partial oxidation of methane is equipped with synthesis gas reaction
The mol ratio of methane and oxygen is 1.9-2.1:1, and reaction temperature is 600-800 ℃, and reaction pressure is for being normal pressure, and air speed is 20000h
-1-30000h
-1, evaluating catalyst carries out in fixed bed miniature quartz pipe reactor.
Catalyst of the present invention is under 600-800 ℃ reaction condition, and methane conversion was greater than 86% when this catalyst was used for methane portion oxidation, and the selectivity of hydrogen and carbon monoxide is greater than 84%.Reaction time was greater than 200 hours.
2, methane carbon dioxide reformation prepares synthesis gas reaction
The mol ratio of methane and carbon dioxide is 0.9-1.1:1, and reaction temperature is 600-800 ℃, and reaction pressure is a normal pressure, and air speed is 1500h
-1-4000h
-1, evaluating catalyst carries out in fixed bed miniature quartz pipe reactor.
Catalyst of the present invention is under 600-800 ℃ reaction condition, and methane conversion was greater than 90% when this catalyst was used for methane carbon dioxide reformation, and carbon dioxide conversion is greater than 85%, and the reaction time was greater than 200 hours.
Advantage of the present invention is as follows:
Have good heat conduction, conductive capability, and the silicon nitride material of very high heat endurance prepares the carrier of synthetic gas catalyst as methane portion oxidation and methane carbon dioxide reformation, by infusion process active component nickel is loaded on the silicon nitride surface, prepare the catalyst of preparation synthesis gas.Advantages such as catalyst of the present invention has the conversion ratio height in the application facet that methane portion oxidation or methane carbon dioxide reformation prepare synthesis gas, and carbon distribution is few, and catalyst life is long.
The specific embodiment
Embodiment 1
Getting 1 gram specific area is 5m
2The alpha-silicon nitride powders of/g is dispersed in alpha-silicon nitride powders in the nickel nitrate aqueous solution of 6.5ml, 2g/ml under 20 ℃ and stirring condition, stirs 12 hours.400 ℃ of roastings 4 hours in Muffle furnace after 60 ℃ of oven dry, can obtain nickel loading is 5wt%, silicon nitride is the catalyst that methane portion oxidation or methane carbon dioxide reformation prepare synthesis gas that can be used for of 95wt%.
It is to carry out in fixed bed reactors that partial oxidation of methane is equipped with synthesis gas reaction, and the mol ratio of methane and oxygen is 2:1, and air speed is 20000h
-1Be used for partial oxidation reaction of methane under 800 ℃ of conditions, methane conversion is 90%, and carbon monoxide selective is 88%, and the selectivity of hydrogen is 86%.Catalyst uses 200h continuously, active not decline.
It is to carry out in the fixed bed quartz tube reactor that methane carbon dioxide reformation prepares synthesis gas reaction, and the mol ratio of methane and carbon dioxide is 1:1, and air speed is 1500h
-1Be used for the methane carbon dioxide reformation reaction under 800 ℃ of conditions, methane conversion is 90%, and carbon dioxide conversion is 88%.Catalyst uses 200h continuously, active not obviously decline.
Embodiment 2
Getting 1 gram specific area is 80m
2The alpha-silicon nitride powders of/g is dispersed in alpha-silicon nitride powders in the nickel nitrate aqueous solution of 53ml, 2g/ml under 20 ℃ and stirring condition, stirs 12 hours.800 ℃ of roastings 6 hours in Muffle furnace again after 100 ℃ of oven dry, can obtain nickel loading is 30wt%, silicon nitride be 70wt% can be used for methane portion oxidation or methane carbon dioxide reformation prepares synthetic gas catalyst.
It is to carry out in fixed bed reactors that partial oxidation of methane is equipped with synthesis gas reaction, and the mol ratio of methane and oxygen is 2:1, and air speed is 23000h
-1Be used for partial oxidation reaction of methane under 700 ℃ of conditions, methane conversion is 89%, and carbon monoxide selective is 87%, and the selectivity of hydrogen is 85%.Catalyst uses 200h continuously, active not decline.
It is to carry out in the fixed bed quartz tube reactor that methane carbon dioxide reformation prepares synthesis gas reaction, and the mol ratio of methane and carbon dioxide is 1:1, and air speed is 2000h
-1Be used for the methane carbon dioxide reformation reaction under 700 ℃ of conditions, methane conversion is 92%, and carbon dioxide conversion is 90%.Catalyst uses 200h continuously, active not obviously decline.
Embodiment 3
Getting 1 gram specific area is 50m
2The alpha-silicon nitride powders of/g is dispersed in alpha-silicon nitride powders in the nickel nitrate alcoholic solution of 5.6ml5g/ml under 50 ℃ and stirring condition, stirs 3 hours.600 ℃ of roastings 4 hours in muffle furnace again after 80 ℃ of oven dry, can obtain nickel loading is 45wt%, silicon nitride is that methane portion oxidation or the methane carbon dioxide reformation of 55wt% prepares synthetic gas catalyst.
It is to carry out in the fixed bed quartz tube reactor that partial oxidation of methane is equipped with synthesis gas reaction, and the mol ratio of methane and oxygen is 1.9:1, and air speed is 25000h
-1Under 600 ℃ of conditions, methane conversion is 87%, and carbon monoxide selective is 86%, and the selectivity of hydrogen is 85%.Catalyst uses 200h continuously, and is active in decline.
It is to carry out in the fixed bed quartz tube reactor that methane carbon dioxide reformation prepares synthesis gas reaction, and the mol ratio of methane and carbon dioxide is 0.9:1, and air speed is 3000h
-1Be used for the methane carbon dioxide reformation reaction under 600 ℃ of conditions, methane conversion is 90%, and carbon dioxide conversion is 88%.Catalyst uses 200h continuously, active not obviously decline.
Embodiment 4
Getting 0.2 gram specific area is 90m
2The alpha-silicon nitride powders of/g is dispersed in alpha-silicon nitride powders under 40 ℃ and stirring condition in 10 milliliters, the nickel acetate aqueous solution of 0.5g/ml, stirs 6 hours.Ph value with the ammoniacal liquor regulator solution is 6-10, makes the nickel in the solution form co-precipitation, is deposited on the silicon nitride surface.Under 100 ℃ of conditions, sample is dried then.Put into 800 ℃ of roastings of Muffle furnace 2 hours again, can obtain nickel loading is 10wt%, and silicon nitride is that methane portion oxidation or the methane carbon dioxide reformation of 90wt% prepares synthetic gas catalyst.
It is to carry out in the fixed bed quartz tube reactor that partial oxidation of methane is equipped with synthesis gas reaction, and the mol ratio of methane and oxygen is 2.1:1, and air speed is 27000h
-1Under 800 ℃ of conditions, methane conversion is 90%, and carbon monoxide selective is 89%, and the selectivity of hydrogen is 87%.Catalyst uses 200h continuously, and is active in decline.
It is to carry out in the fixed bed quartz tube reactor that methane carbon dioxide reformation prepares synthesis gas reaction, and the mol ratio of methane and carbon dioxide is 1:1, and air speed is 4000h
-1Be used for the methane carbon dioxide reformation reaction under 800 ℃ of conditions, methane conversion is 91%, and carbon dioxide conversion is 88%.Catalyst uses 200h continuously, active not obviously decline.
Embodiment 5
Getting 0.1 gram specific area is 50m
2The alpha-silicon nitride powders of/g is dispersed in alpha-silicon nitride powders in the nickel acetate alcoholic solution of 5.6ml, 5g/ml under 20 ℃ and stirring condition, stirs 3 hours.400 ℃ of roastings 5 hours in Muffle furnace again after 80 ℃ of oven dry, can obtain nickel loading is 18wt%, silicon nitride is that methane portion oxidation or the methane carbon dioxide reformation of 82wt% prepares synthetic gas catalyst.
It is to carry out in the fixed bed quartz tube reactor that partial oxidation of methane is equipped with synthesis gas reaction, and the mol ratio of methane and oxygen is 2.1:1, and air speed is 23000h
-1Under 750 ℃ of conditions, methane conversion is 88%, and carbon monoxide selective is 86%, and the selectivity of hydrogen is 85%.Catalyst uses 200h continuously, and is active in decline.
It is to carry out in the fixed bed quartz tube reactor that methane carbon dioxide reformation prepares synthesis gas reaction, and the mol ratio of methane and carbon dioxide is 1:1, and air speed is 1600h
-1Be used for the methane carbon dioxide reformation reaction under 750 ℃ of conditions, methane conversion is 92%, and carbon dioxide conversion is 90%.Catalyst uses 200h continuously, active not obviously decline.
Embodiment 6
Getting 2 gram specific areas is 30m
2The alpha-silicon nitride powders of/g is dispersed in alpha-silicon nitride powders in the nickel sulfate solution of 6.6ml, 5g/ml under 20 ℃ and stirring condition, stirs 5 hours.Ph value with the ammoniacal liquor regulator solution is 6-10 again, makes the nickel in the solution form precipitation, is deposited on the silicon nitride surface.Sample after 100 ℃ of oven dry again in Muffle furnace 600 ℃ burnt 8 hours, can obtain nickel loading is 7wt%, silicon nitride is that methane portion oxidation or the methane carbon dioxide reformation of 93wt% prepares synthetic gas catalyst.
It is to carry out in the fixed bed quartz tube reactor that partial oxidation of methane is equipped with synthesis gas reaction, and the mol ratio of methane and oxygen is 2:1, and air speed is 25000h
-1This catalyst is under 650 ℃ of conditions, and methane conversion is 91%, and carbon monoxide selective is 89%, and the selectivity of hydrogen is 88%.Catalyst uses 200h continuously, and is active in decline.
It is to carry out in the fixed bed quartz tube reactor that methane carbon dioxide reformation prepares synthesis gas reaction, and the mol ratio of methane and carbon dioxide is 1.1:1, and air speed is 3000h
-1Be used for the methane carbon dioxide reformation reaction under 650 ℃ of conditions, methane conversion is 92%, and carbon dioxide conversion is 90%.Catalyst uses 200h continuously, active not obviously decline.
Claims (6)
1, a kind of catalyst for preparing synthesis gas is characterized in that catalyst is carrier with the silicon nitride material, and metallic nickel is an active component, and its percentage by weight consists of:
Nickel 1-50wt% silicon nitride 50-99wt%.
2, a kind of catalyst for preparing synthesis gas as claimed in claim 1, the specific area that it is characterized in that described silicon nitride is 5-100m
2/ g.
3, a kind of Preparation of catalysts method for preparing synthesis gas as claimed in claim 1 or 2 is characterized in that comprising the steps:
(1), compound concentration is the soluble nickel salting liquid of 1-20wt%;
(2), under stirring condition, the silicon nitride carrier is immersed in the above-mentioned nickel salt solution, the part by weight of nickel salt and silicon nitride is 4.7-83:100; Under 20-60 ℃ of temperature, stirred 1-12 hour, the Ph value that abundant mixing makes solvent evaporates or regulator solution is deposited on the carrier surface active component to 6-10;
(3), under 60-150 ℃ of condition, in air, dry, 400 ℃-800 ℃ roasting 1-6 hour, promptly can be used for the catalyst that methane portion oxidation or methane carbon dioxide reformation prepare synthesis gas.
4, as claimed in claim 3 a kind of prepare synthesis gas the preparation method, it is characterized in that described soluble nickel salt is nickel nitrate, nickel acetate or nickelous sulfate.
5, a kind of catalyst for preparing synthesis gas as claimed in claim 1 or 2 is used, and it is characterized in that comprising the steps:
The mol ratio of methane and oxygen is 1.9-2.1:1, and reaction temperature is 600-800 ℃, and reaction pressure is for being normal pressure, and air speed is 20000h
-1-30000h
-1, in fixed bed reactors, carry out.
6, a kind of catalyst for preparing synthesis gas as claimed in claim 1 or 2 is used, and it is characterized in that comprising the steps:
The mol ratio of methane and carbon dioxide is 0.9-1.1:1, and reaction temperature is 600-800 ℃, and reaction pressure is a normal pressure, and air speed is 1500h
-1-4000h
-1, catalyst carries out in fixed bed reactors.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910074205A CN101530809A (en) | 2009-04-18 | 2009-04-18 | Catalyst for preparing synthesis gas, preparation method and application |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910074205A CN101530809A (en) | 2009-04-18 | 2009-04-18 | Catalyst for preparing synthesis gas, preparation method and application |
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| CN101530809A true CN101530809A (en) | 2009-09-16 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107754844A (en) * | 2017-10-31 | 2018-03-06 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation of nickel-base catalyst of carbon distribution and products thereof and application can effectively be reduced by preparing in synthesis gas reaction |
| WO2018205787A1 (en) * | 2017-05-09 | 2018-11-15 | 中科合成油技术有限公司 | Fischer-tropsch synthesis catalyst containing nitride support, preparation method therefor and use thereof |
| CN112403470A (en) * | 2020-11-25 | 2021-02-26 | 榆林学院 | Catalyst for preparing synthesis gas by reforming methane and carbon dioxide and application thereof |
-
2009
- 2009-04-18 CN CN200910074205A patent/CN101530809A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018205787A1 (en) * | 2017-05-09 | 2018-11-15 | 中科合成油技术有限公司 | Fischer-tropsch synthesis catalyst containing nitride support, preparation method therefor and use thereof |
| RU2760904C2 (en) * | 2017-05-09 | 2021-12-01 | Синфюэлс Чайна Текнолоджи Ко., Лтд. | Fischer-tropsch synthesis catalyst containing nitride carrier, and method for its preparation, and its application |
| US11426712B2 (en) | 2017-05-09 | 2022-08-30 | Synfuels China Technology Co., Ltd. | Fischer-Tropsch synthesis catalyst containing nitride support, preparation method therefor and use thereof |
| AU2018264223B2 (en) * | 2017-05-09 | 2022-11-10 | Synfuels China Technology Co., Ltd. | Fischer-tropsch synthesis catalyst containing nitride support, preparation method therefor and use thereof |
| CN107754844A (en) * | 2017-10-31 | 2018-03-06 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation of nickel-base catalyst of carbon distribution and products thereof and application can effectively be reduced by preparing in synthesis gas reaction |
| CN112403470A (en) * | 2020-11-25 | 2021-02-26 | 榆林学院 | Catalyst for preparing synthesis gas by reforming methane and carbon dioxide and application thereof |
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Open date: 20090916 |