CN111097441A - Catalyst for reforming methane and carbon dioxide to prepare synthesis gas and preparation method thereof - Google Patents
Catalyst for reforming methane and carbon dioxide to prepare synthesis gas and preparation method thereof Download PDFInfo
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- CN111097441A CN111097441A CN202010032805.XA CN202010032805A CN111097441A CN 111097441 A CN111097441 A CN 111097441A CN 202010032805 A CN202010032805 A CN 202010032805A CN 111097441 A CN111097441 A CN 111097441A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/85—Chromium, molybdenum or tungsten
- B01J23/88—Molybdenum
- B01J23/887—Molybdenum containing in addition other metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/8877—Vanadium, tantalum, niobium or polonium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/32—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air
- C01B3/34—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air by reaction of hydrocarbons with gasifying agents
- C01B3/38—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air by reaction of hydrocarbons with gasifying agents using catalysts
- C01B3/40—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air by reaction of hydrocarbons with gasifying agents using catalysts characterised by the catalyst
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- 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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- Inorganic Chemistry (AREA)
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Abstract
The invention discloses a catalyst for reforming methane and carbon dioxide to prepare synthesis gas and a preparation method thereof, wherein the catalyst comprises an active component, an auxiliary agent and a carrier component, the active component is nickel and cobalt, the auxiliary agent is one or more of Zr, La, Ce, Co, Mo or V, Mo mainly exists in the form of MoO3, the carrier component is modified alumina, and the weight ratio of the raw materials is as follows: 4-8% of active component, 80-91% of carrier component and 5-12% of auxiliary agent. According to the catalyst for preparing the synthesis gas by reforming the methane and the carbon dioxide and the preparation method thereof, the alumina carrier is modified by utilizing the ammonium molybdate and the soluble aluminum-containing compound, so that the stability of the alumina carrier in the use process is improved, metal active components in the catalyst can be uniformly and respectively arranged on the surface of the carrier, the catalyst keeps good catalytic effect, and meanwhile, the double functions of sintering resistance and carbon deposition resistance are improved.
Description
Technical Field
The invention belongs to the technical field of catalyst preparation, and particularly relates to a catalyst for preparing synthesis gas by reforming methane and carbon dioxide and a preparation method thereof.
Background
Methane is widely distributed in nature, is the main component of natural gas, is also abundantly present in shale gas and combustible ice, and has abundant reserves. Methane is also one of the important greenhouse gases. Carbon dioxide gas is the most important cause of the greenhouse effect, the emission of carbon dioxide to the atmosphere of human beings is increased year by year, and how to treat the carbon dioxide to relieve the greenhouse effect becomes a common challenge for all human beings. The methane and carbon dioxide reforming reaction consumes two greenhouse gases of methane and carbon dioxide, and the generated synthesis gas has a low H2/CO ratio, is suitable for downstream synthesis such as Fischer-Tropsch synthesis, and has high social benefit and economic benefit.
In the traditional catalyst for preparing synthesis gas by catalytic reforming of methane and carbon dioxide, a carrier of the catalyst mainly exists in a metal oxide or active carbon structure form, and the carrier has poor stability in high-temperature sintering after reaction with active components and auxiliaries, has poor sintering and carbon deposition resistant effects in the high-temperature sintering process, and cannot meet the requirements in the current stage.
Disclosure of Invention
The invention aims to provide a catalyst for reforming methane and carbon dioxide to prepare synthesis gas and a preparation method thereof, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
the catalyst for preparing the synthesis gas by reforming the methane and the carbon dioxide comprises an active component, an auxiliary agent and a carrier component, wherein the active component is nickel and cobalt, the auxiliary agent is one or more of Zr, La, Ce, Co, Mo or V, Mo mainly exists in the form of MoO3, the carrier component is modified alumina, and the weight ratio of the raw materials is as follows: 4-8% of active component, 80-91% of carrier component and 5-12% of auxiliary agent.
Preferably, the preparation steps of the modified alumina of the support component are as follows: and sequentially or simultaneously introducing ammonium molybdate and a soluble aluminum-containing compound into the alumina-based carrier, and carrying out heat treatment to obtain the dried improved alumina-based carrier.
Preferably, the ammonium salt and the soluble aluminum-containing compound are introduced into the alumina-based support sequentially or simultaneously by an impregnation method.
A preparation method of a catalyst for preparing synthesis gas by methane and carbon dioxide reforming comprises the following steps:
s1: weighing nickel nitrate and cobalt nitrate containing nickel and cobalt components, dissolving the nickel nitrate and the cobalt nitrate in a polyalcohol solution, stirring and standing to form a nickel-cobalt transparent solution A;
s2: adding citric acid or oxalic acid into the nickel-cobalt transparent solution A, stirring and standing to obtain a mixed solution B;
s3: adding the dried modified carrier into the mixed solution B in the S2, adding the active component, uniformly stirring, drying in a water bath condition, and transferring to an oven for drying after drying;
s4: and drying and roasting the mixed solution after the completion of the drying in the S-step to obtain the catalyst.
Preferably, in S1, the polyhydric alcohol is one or more of xylitol, sorbitol, mannitol and arabitol, and the mass ratio of the nickel nitrate and the cobalt nitrate to the polyhydric alcohol is 1:3-5 and 1:1-3 respectively.
Preferably, in S1, the nickel nitrate and the cobalt nitrate can also be nickel acetate and cobalt acetate, and the molar ratio of nickel to cobalt in the nickel nitrate and the cobalt nitrate is 1: 1.
Preferably, in S2, citric acid or oxalic acid is added in a molar ratio of 1:1 to the nickel nitrate and cobalt nitrate.
Preferably, in S4, the device used in calcination is a muffle furnace, and the calcination temperature is 300-600 ℃, and the distribution time is 2-5 hours.
The invention has the technical effects and advantages that: according to the catalyst for preparing the synthesis gas by reforming the methane and the carbon dioxide and the preparation method thereof, the alumina carrier is modified by utilizing the ammonium molybdate and the soluble aluminum-containing compound, so that the stability of the alumina carrier in the use process is improved, the metal active components in the catalyst can be uniformly and respectively arranged on the surface of the carrier, the double functions of sintering resistance and carbon deposition resistance of the catalyst are improved while the catalyst keeps a good catalytic effect, and in addition, the catalytic effect is improved by the matching of a plurality of groups of metal active components.
Detailed Description
The technical solutions in the present invention will be described clearly and completely with reference to the contents of the present invention, and it is obvious that the described contents are only a part of the contents of the present invention, and not all of the contents. All other matters which can be obtained by a person skilled in the art without making creative efforts based on the contents of the present invention belong to the protection scope of the present invention.
Example 1
The invention provides a catalyst for reforming methane and carbon dioxide to prepare synthesis gas, which comprises an active component, an auxiliary agent and a carrier component, wherein the active component is nickel and cobalt, the auxiliary agent is one or more of Zr, La, Ce, Co, Mo or V, Mo mainly exists in the form of MoO3, the carrier component is modified alumina, and the weight ratio of the raw materials is as follows: the active component is 4%, the carrier component is 91% and the auxiliary agent is 5%.
Specifically, the preparation steps of the modified alumina of the carrier component are as follows: and sequentially or simultaneously introducing ammonium molybdate and a soluble aluminum-containing compound into the alumina-based carrier, and carrying out heat treatment to obtain the dried improved alumina-based carrier.
Specifically, the introduction of the ammonium salt and the soluble aluminum-containing compound into the alumina-based carrier is carried out sequentially or simultaneously by an impregnation method.
A preparation method of a catalyst for preparing synthesis gas by methane and carbon dioxide reforming comprises the following steps:
s1: weighing nickel nitrate and cobalt nitrate containing nickel and cobalt components, dissolving the nickel nitrate and the cobalt nitrate in a polyalcohol solution, stirring and standing to form a nickel-cobalt transparent solution A;
s2: adding citric acid or oxalic acid into the nickel-cobalt transparent solution A, stirring and standing to obtain a mixed solution B;
s3: adding the dried modified carrier into the mixed solution B in the S2, adding the active component, uniformly stirring, drying in a water bath condition, and transferring to an oven for drying after drying;
s4: and drying and roasting the mixed solution after the completion of the drying in the S-step to obtain the catalyst.
Specifically, in S1, the polyhydric alcohol is one or more of xylitol, sorbitol, mannitol, and arabitol, and the mass ratios of the nickel nitrate and the cobalt nitrate to the polyhydric alcohol are 1:3 and 1:1, respectively.
Specifically, in S1, the nickel nitrate and the cobalt nitrate may be nickel acetate or cobalt acetate, and the molar ratio of nickel to cobalt in the nickel nitrate and cobalt nitrate is 1: 1.
Specifically, in S2, citric acid or oxalic acid is added, and the molar ratio of nickel nitrate to cobalt nitrate is 1: 1.
Specifically, in S4, the equipment used for calcination was a muffle furnace, the calcination temperature was 300 ℃, and the distribution time was 2 hours.
Example 2
The catalyst for preparing the synthesis gas by reforming the methane and the carbon dioxide comprises an active component, an auxiliary agent and a carrier component, wherein the active component is nickel and cobalt, the auxiliary agent is one or more of Zr, La, Ce, Co, Mo or V, Mo mainly exists in the form of MoO3, the carrier component is modified alumina, and the weight ratio of the raw materials is as follows: the active component is 6%, the carrier component is 86% and the auxiliary agent is 8%.
Specifically, the preparation steps of the modified alumina of the carrier component are as follows: and sequentially or simultaneously introducing ammonium molybdate and a soluble aluminum-containing compound into the alumina-based carrier, and carrying out heat treatment to obtain the dried improved alumina-based carrier.
Specifically, the introduction of the ammonium salt and the soluble aluminum-containing compound into the alumina-based carrier is carried out sequentially or simultaneously by an impregnation method.
A preparation method of a catalyst for preparing synthesis gas by methane and carbon dioxide reforming comprises the following steps:
s1: weighing nickel nitrate and cobalt nitrate containing nickel and cobalt components, dissolving the nickel nitrate and the cobalt nitrate in a polyalcohol solution, stirring and standing to form a nickel-cobalt transparent solution A;
s2: adding citric acid or oxalic acid into the nickel-cobalt transparent solution A, stirring and standing to obtain a mixed solution B;
s3: adding the dried modified carrier into the mixed solution B in the S2, adding the active component, uniformly stirring, drying in a water bath condition, and transferring to an oven for drying after drying;
s4: and drying and roasting the mixed solution after the completion of the drying in the S-step to obtain the catalyst.
Specifically, in S1, the polyhydric alcohol is one or more of xylitol, sorbitol, mannitol, and arabitol, and the mass ratios of the nickel nitrate and the cobalt nitrate to the polyhydric alcohol are 1:4 and 1:2, respectively.
Specifically, in S1, the nickel nitrate and the cobalt nitrate may be nickel acetate or cobalt acetate, and the molar ratio of nickel to cobalt in the nickel nitrate and cobalt nitrate is 1: 1.
Specifically, in S2, citric acid or oxalic acid is added, and the molar ratio of nickel nitrate to cobalt nitrate is 1: 1.
Specifically, in S4, the equipment used in the calcination was a muffle furnace, the calcination temperature was 450 ℃, and the distribution time was 3.5 hours.
Example 3
The catalyst for preparing the synthesis gas by reforming the methane and the carbon dioxide comprises an active component, an auxiliary agent and a carrier component, wherein the active component is nickel and cobalt, the auxiliary agent is one or more of Zr, La, Ce, Co, Mo or V, Mo mainly exists in the form of MoO3, the carrier component is modified alumina, and the weight ratio of the raw materials is as follows: 8 percent of active component, 80 percent of carrier component and 12 percent of auxiliary agent.
Specifically, the preparation steps of the modified alumina of the carrier component are as follows: and sequentially or simultaneously introducing ammonium molybdate and a soluble aluminum-containing compound into the alumina-based carrier, and carrying out heat treatment to obtain the dried improved alumina-based carrier.
Specifically, the introduction of the ammonium salt and the soluble aluminum-containing compound into the alumina-based carrier is carried out sequentially or simultaneously by an impregnation method.
A preparation method of a catalyst for preparing synthesis gas by methane and carbon dioxide reforming comprises the following steps:
s1: weighing nickel nitrate and cobalt nitrate containing nickel and cobalt components, dissolving the nickel nitrate and the cobalt nitrate in a polyalcohol solution, stirring and standing to form a nickel-cobalt transparent solution A;
s2: adding citric acid or oxalic acid into the nickel-cobalt transparent solution A, stirring and standing to obtain a mixed solution B;
s3: adding the dried modified carrier into the mixed solution B in the S2, adding the active component, uniformly stirring, drying in a water bath condition, and transferring to an oven for drying after drying;
s4: and drying and roasting the mixed solution after the completion of the drying in the S-step to obtain the catalyst.
Specifically, in S1, the polyhydric alcohol is one or more of xylitol, sorbitol, mannitol, and arabitol, and the mass ratios of the nickel nitrate and the cobalt nitrate to the polyhydric alcohol are 1:5 and 1:3, respectively.
Specifically, in S1, the nickel nitrate and the cobalt nitrate may be nickel acetate or cobalt acetate, and the molar ratio of nickel to cobalt in the nickel nitrate and cobalt nitrate is 1: 1.
Specifically, in S2, citric acid or oxalic acid is added, and the molar ratio of nickel nitrate to cobalt nitrate is 1: 1.
Specifically, in S4, the equipment used for calcination was a muffle furnace, the calcination temperature was 600 ℃, and the distribution time was 5 hours.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments or portions thereof without departing from the spirit and scope of the invention.
Claims (8)
1. A catalyst for preparing synthesis gas by reforming methane and carbon dioxide is characterized in that: the catalyst comprises an active component, an auxiliary agent and a carrier component, wherein the active component is nickel and cobalt, the auxiliary agent is one or more of Zr, La, Ce, Co, Mo or V, Mo mainly exists in the form of MoO3, the carrier component is modified alumina, and the weight ratio of the raw materials is as follows: 4-8% of active component, 80-91% of carrier component and 5-12% of auxiliary agent.
2. The catalyst for reforming methane and carbon dioxide to synthesis gas according to claim 1, wherein: the preparation steps of the modified alumina of the carrier component are as follows: and sequentially or simultaneously introducing ammonium molybdate and a soluble aluminum-containing compound into the alumina-based carrier, and carrying out heat treatment to obtain the dried improved alumina-based carrier.
3. The catalyst for reforming methane and carbon dioxide to synthesis gas according to claim 2, wherein: the introduction of the ammonium salt and the soluble aluminum-containing compound into the alumina-based support is carried out sequentially or simultaneously by an impregnation method.
4. The method according to claim 1, wherein the catalyst is prepared by reforming methane with carbon dioxide to produce synthesis gas, and the method comprises the following steps: the method comprises the following steps:
s1: weighing nickel nitrate and cobalt nitrate containing nickel and cobalt components, dissolving the nickel nitrate and the cobalt nitrate in a polyalcohol solution, stirring and standing to form a nickel-cobalt transparent solution A;
s2: adding citric acid or oxalic acid into the nickel-cobalt transparent solution A, stirring and standing to obtain a mixed solution B;
s3: adding the dried modified carrier into the mixed solution B in the S2, adding the active component, uniformly stirring, drying in a water bath condition, and transferring to an oven for drying after drying;
s4: and drying and roasting the mixed solution after the completion of the drying in the S-step to obtain the catalyst.
5. The method for preparing a catalyst for methane carbon dioxide reforming to synthesis gas according to claim 3, wherein: in S1, the polyalcohol is one or more of xylitol, sorbitol, mannitol and arabitol, and the mass ratio of the nickel nitrate to the polyalcohol is 1:3-5 and the mass ratio of the cobalt nitrate to the polyalcohol is 1: 1-3.
6. The method for preparing a catalyst for methane carbon dioxide reforming to synthesis gas according to claim 3, wherein: in S1, the nickel nitrate and the cobalt nitrate can also be nickel acetate and cobalt acetate, and the molar ratio of nickel to cobalt in the nickel nitrate and the cobalt nitrate is 1: 1.
7. The method for preparing a catalyst for methane carbon dioxide reforming to synthesis gas according to claim 3, wherein: in S2, citric acid or oxalic acid is added, and the molar ratio of nickel nitrate to cobalt nitrate is 1: 1.
8. The method for preparing a catalyst for methane carbon dioxide reforming to synthesis gas according to claim 3, wherein: in S4, the device used in roasting is a muffle furnace, the roasting temperature is 300-600 ℃, and the distribution time is 2-5 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010032805.XA CN111097441A (en) | 2020-01-13 | 2020-01-13 | Catalyst for reforming methane and carbon dioxide to prepare synthesis gas and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010032805.XA CN111097441A (en) | 2020-01-13 | 2020-01-13 | Catalyst for reforming methane and carbon dioxide to prepare synthesis gas and preparation method thereof |
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| CN111097441A true CN111097441A (en) | 2020-05-05 |
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| CN202010032805.XA Withdrawn CN111097441A (en) | 2020-01-13 | 2020-01-13 | Catalyst for reforming methane and carbon dioxide to prepare synthesis gas and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11286160B2 (en) | 2020-01-28 | 2022-03-29 | Saudi Arabian Oil Company | Nickel-containing catalyst composition having enhanced acidity for autothermal reforming processes |
| US11338270B2 (en) | 2020-01-28 | 2022-05-24 | Saudi Arabian Oil Company | Catalyst compositions having enhanced acidity for autothermal reforming processes |
| US11365120B2 (en) | 2020-01-28 | 2022-06-21 | Saudi Arabian Oil Company | Nickel-containing catalyst composition having enhanced acidity for steam reforming processes |
| US11396006B2 (en) | 2020-01-28 | 2022-07-26 | Saudi Arabian Oil Company | Nickel-containing catalyst composition having enhanced acidity for bi-reforming processes |
| US11478777B2 (en) * | 2020-01-28 | 2022-10-25 | Saudi Arabian Oil Company | Catalyst compositions having enhanced acidity for dry reforming processes |
| US11498053B2 (en) | 2020-01-28 | 2022-11-15 | Saudi Arabian Oil Company | Nickel-containing catalyst composition having enhanced acidity for dry reforming processes |
-
2020
- 2020-01-13 CN CN202010032805.XA patent/CN111097441A/en not_active Withdrawn
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11286160B2 (en) | 2020-01-28 | 2022-03-29 | Saudi Arabian Oil Company | Nickel-containing catalyst composition having enhanced acidity for autothermal reforming processes |
| US11338270B2 (en) | 2020-01-28 | 2022-05-24 | Saudi Arabian Oil Company | Catalyst compositions having enhanced acidity for autothermal reforming processes |
| US11365120B2 (en) | 2020-01-28 | 2022-06-21 | Saudi Arabian Oil Company | Nickel-containing catalyst composition having enhanced acidity for steam reforming processes |
| US11396006B2 (en) | 2020-01-28 | 2022-07-26 | Saudi Arabian Oil Company | Nickel-containing catalyst composition having enhanced acidity for bi-reforming processes |
| US11478777B2 (en) * | 2020-01-28 | 2022-10-25 | Saudi Arabian Oil Company | Catalyst compositions having enhanced acidity for dry reforming processes |
| US11498053B2 (en) | 2020-01-28 | 2022-11-15 | Saudi Arabian Oil Company | Nickel-containing catalyst composition having enhanced acidity for dry reforming processes |
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