WO2014137293A1 - Procédé de préparation d'un catalyseur métallique supporté à forte dispersion - Google Patents

Procédé de préparation d'un catalyseur métallique supporté à forte dispersion Download PDF

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Publication number
WO2014137293A1
WO2014137293A1 PCT/SG2014/000108 SG2014000108W WO2014137293A1 WO 2014137293 A1 WO2014137293 A1 WO 2014137293A1 SG 2014000108 W SG2014000108 W SG 2014000108W WO 2014137293 A1 WO2014137293 A1 WO 2014137293A1
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WO
WIPO (PCT)
Prior art keywords
salt
metal
oxide
powder
nitrate
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PCT/SG2014/000108
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English (en)
Inventor
Sibudjing Kawi
Liuye MO
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National University Of Singapore
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Publication of WO2014137293A1 publication Critical patent/WO2014137293A1/fr

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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
    • C01B3/22—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of gaseous or liquid organic compounds
    • C01B3/24—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of gaseous or liquid organic compounds of hydrocarbons
    • C01B3/26—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of gaseous or liquid organic compounds of hydrocarbons using catalysts
    • 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
    • B01J23/72—Copper
    • 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
    • B01J23/74—Iron group metals
    • B01J23/75—Cobalt
    • 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
    • B01J23/83—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 rare earths or actinides
    • 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
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/391—Physical properties of the active metal ingredient
    • B01J35/393—Metal or metal oxide crystallite size
    • 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
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/02—Impregnation, coating or precipitation
    • B01J37/0201—Impregnation
    • B01J37/0203—Impregnation the impregnation liquid containing organic compounds
    • 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
    • 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
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J35/61—Surface area
    • B01J35/615—100-500 m2/g
    • 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
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/16—Reducing
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/02—Processes for making hydrogen or synthesis gas
    • C01B2203/0205—Processes for making hydrogen or synthesis gas containing a reforming step
    • C01B2203/0227—Processes for making hydrogen or synthesis gas containing a reforming step containing a catalytic reforming step
    • C01B2203/0238—Processes for making hydrogen or synthesis gas containing a reforming step containing a catalytic reforming step the reforming step being a carbon dioxide reforming step
    • 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

Definitions

  • CH 4 methane
  • C0 2 carbon dioxide
  • synthesis gas which, as a mixture of carbon monoxide (CO) and hydrogen (H 2 ) gases, is used in various industrial applications.
  • This invention is based on an unexpected discovery of a process for preparing a highly dispersed supported metal catalyst that is suitable for the commercial application.
  • the present invention concerns a process of preparing a highly dispersed supported metal catalyst.
  • the process includes the following steps: (i) preparing a solution that contains a metal salt and a monofunctional organic acid, (ii) mixing an inert oxide powder into the solution to form a homogenous mixture; (iii) drying the homogenous mixture at 50 - 200 °C to yield a dried mass; (iv) calcining the dried mass at 250 - 1000 °C to cause formation of a metal oxide on the surface of the powder; and (v) incubating the calcined mass in a hydrogen atmosphere at 250 - 1000 °C to reduce the metal oxide to a particulate metal.
  • the monofunctional organic acid can be a monocarboxylic acid containing 3 to 40 carbon atoms (e.g., oleic acid, stearic acid, hexanoic acid, butyric acid, propanoic acid, or a combination thereof).
  • the inert oxide powder can be a silica powder, an alumina powder, an aluminum silicate powder, a titanium oxide powder, a zirconium oxide powder, a cerium oxide powder, a lanthanum oxide powder, a carbon powder, a zeolite powder, or a combination thereof.
  • Examples of a metal salt include a copper salt, a nickel salt, a cerium salt, a lanthanum salt, a samarium salt, a magnesium salt, a cobalt salt, a ruthenium salt;, a rhodium salt, a palladium salt, a silver salt, an osmium salt, an iridium salt, a platinum salt, a gold salt, and a combination thereof.
  • Specific examples of a metal salt also include a metal oxide, a metal nitrate, a metal chloride, a metal acetate, a metal formate, and a combination thereof.
  • the metal salt can be copper nitrate, nickel nitrate, cerium nitrate, lanthanum nitrate, samarium nitrate, copper oxide, lanthanum oxide, samarium oxide, nickel oxide, or a combination thereof.
  • the metal salt is copper nitrate
  • the monofunctional organic acid is oleic acid
  • the inert oxide powder is silica powder.
  • the metal salt is nickel nitrate
  • the monofunctional organic acid is oleic acid
  • the inert oxide powder is silica powder.
  • Another aspect of this invention concerns a different process of preparing a highly dispersed supported metal catalyst.
  • the process includes the following steps: (i) preparing a first solution that contains a metal salt; (ii) preparing a second solution that contains a monofunctional organic acid; (iii) mixing an inert oxide powder into the second solution to form a first homogenous mixture; (iv) mixing the first homogenous mixture with the first solution to form a second homogenous mixture; (v) drying the homogenous mixture at 50 - 200 °C to yield a dried mass; (vi) calcining the dried mass at 250 - 1000 °C to cause formation of a metal oxide on the surface of the powder; and (vii) incubating the calcined mass in a hydrogen atmosphere at 250 - 1000 °C to reduce the metal oxide to a particulate metal.
  • Examples of the monofunctional organic acid, inert oxide powder, and metal oxide are enumerated above.
  • the metal catalyst prepared by the process of the invention includes a transition metal (e.g., copper and nickel) or a noble metal (e.g., platinum and gold), both of which can be doped with other metals to form a bi-metallic or multi-metallic catalyst.
  • a transition metal e.g., copper and nickel
  • a noble metal e.g., platinum and gold
  • Metal particles are to be prepared by the process of the invention.
  • An inert oxide powder as a catalyst support, plays a key role in achieving high dispersion of the metal particles over its surface.
  • the inert oxide powder has a surface area greater than 200 m 2 /g. Strong interactions between metal particles and their support, i.e., the inert oxide powder, are necessary to achieve small metal particle sizes, as well as high dispersion and high mobility of metal particles on the support surface.
  • a monofunctional organic acid and a melt salt are used in the process of the invention.
  • the monofunctional organic acid acts as a promoter to facilitate high dispersion of metal particles.
  • the molar ratio of the monofunctional organic acid to the metal in the metal salt is 0.01 to 3.
  • the molar ratios are preferably ⁇ 0.05 and ⁇ 0.5, respectively.
  • a solvent is used to prepare a solution that contains the metal salt.
  • the solvent may be any liquid which can dissolve the metal salt and can be removed from an inert oxide powder support by drying or vacuum evaporation.
  • the solvent include, but are not limited to, water, acetic acid, alcohols (e.g., methanol, ethanol, ethylene glycol, and a mixture thereof).
  • Described below is an exemplary procedure of sequential impregnation for preparing a highly dispersed supported metal catalyst.
  • a solution that contains a metal salt (e.g., copper nitrate) and a monocarboxylic acid (e.g., oleic acid) is prepared.
  • An inert oxide powder e.g., silica powder
  • the mixture may then be dried at 80-200 °C (e.g., 100-150°C) in an oven with or without vacuum.
  • the dried mass is calcined at a temperature of 250-1000°C (e.g., 300-900°C) in air or another suitable atmosphere.
  • the preferable temperature for preparing a copper catalyst is 300-500°C and for preparing a nickel catalyst is 600-800 °C.
  • the calcined mass is reduced at a temperature of 250- 1000° C in an atmosphere containing hydrogen at an amount of 1-100 mol% (e.g., 5-10 mol%). A highly dispersed supported metal catalyst is thus obtained.
  • An inert oxide powder e.g., silica powder
  • a solution that contains a monocarboxylic acid e.g., oleic acid
  • a metal salt e.g., copper nitrate
  • the metal particle size or crystallite size of a catalyst thus obtained is determined by transmission electron microscopy (TEM) or powder X-ray diffraction (XRD), as is well known to those skilled in the art.
  • Catalytic activities of a catalyst can be measured as follows in one of the two chemical reactions, i.e., reforming of CH 4 and C0 2 (dry reforming of carbon dioxide and methane, DRM) and water gas shift reaction (WGSR).
  • DRM dry reforming of carbon dioxide and methane
  • WGSR water gas shift reaction
  • the flow rates of methane, carbon dioxide, and nitrogen are kept at ⁇ 20 ml/min.
  • the nitrogen in the feed gas acts as the internal standard.
  • 50 mg of the catalyst Prior to the DRM reaction, 50 mg of the catalyst is placed in the fixed-bed reactor and plugged with quartz wool.
  • the catalytic activity of the catalyst is determined by the conversion of methane and carbon dioxide to synthesis gas.
  • the feed composition (with a total flow rate of 50 ml/min) is as follows: 5 mol% CO, 25 mol% H 2 0, and 70 mol% He.
  • the effluent gases are analyzed by a Gas Chromatograph equipped with a Hayesep D column.
  • the catalytic activity of the catalyst is measured by the conversion of carbon monoxide into carbon dioxide and hydrogen.
  • Example 1 Preparation and characterization of 10 wt% Cu/Si0 2 catalyst
  • Cu wt% wt(Cu/(Cu+Si0 2 ))xl 00%.
  • Ni wt% in Examples 2 and 3 and Cu wt% in Examples 7-9 are calculated by the same formula.
  • the catalyst was used in the WGSR reaction at 300 °C and the CO conversion rate was 47%.
  • Example 2 Preparation and characterization of 5 wt% Ni/Si0 2 catalyst
  • Example 3 Preparation and characterization of 5 wt% Ni/Si0 2 catalyst
  • Example 4 Preparation and characterization of 5 wt% Ni-1 wt% La20 3 /Si02 catalyst
  • La 2 0 3 wt% wt(La 2 O 3 /(Ni+La 2 O 3 +SiO 2 ))xl00%.
  • Ni wt% and Sm 2 0 3 wt% in Example 5 Ni wt% and Ce0 2 wt% in Example 6, as well as Cu wt% and Ce0 2 wt% in Example 10, are calculated by the same formula.
  • the nickel crystallite size as measured by XRD, was 3.4 nm.
  • the catalyst was used in the DRM reaction at 700 °C and the CH 4 and CQ 2 conversion rates were around 79% and 85%, respectively.
  • TEM images also showed that there was no carbon deposited on the spent catalyst and the nickel particles were still highly dispersed on the support.
  • Example 5 Preparation and characterization of 5 wt% Ni-1 wt% Sm 2 0 3 /Si0 2 catalyst
  • Example 6 Preparation and characterization of 5 wt% Ni-1 wt% Ce0 2 /Si0 2 catalyst
  • the catalyst was reduced at 700 °C for one hour. Note that Ce0 2 was not reduced under this condition.
  • the catalyst thus prepared was used in the DRM reaction at 700 °C and the CH 4 and
  • Example 7 Preparation and characterization of 10 wt% Cu/Si0 2 catalyst
  • Example 8 Preparation and characterization of 10 wt% Cu/Si0 2 catalyst
  • the sample was impregnated at 60°C for > 6 hours before dried overnight at 100°C.
  • the dried sample was calcined at 450 °C for 4 hours.
  • the catalyst was reduced at 300°C for one hour.
  • the average copper particle size, as measured by N 2 0 chemisotption, was 2.2 nm.
  • the catalyst thus prepared was used in the WGSR reaction at 300 °C and the CO conversion rate was 46%.
  • Example 10 Preparation and characterization of 10 wt% Cu-10 wt% CeO?/SiQ7
  • the 10 wt%Cu/10 wt%Ce0 2 /Si0 2 catalyst thus obtained was reduced at 300 °C for one hour.
  • the catalyst thus prepared was used in the WGSR reaction at 300°C and the CO conversion rate was 67%.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Combustion & Propulsion (AREA)
  • Inorganic Chemistry (AREA)
  • Catalysts (AREA)

Abstract

La présente invention concerne un procédé permettant de préparer un catalyseur métallique supporté à forte dispersion. Le procédé comprend les étapes consistant à mélanger un sel métallique, un acide organique monofonctionnel et une poudre d'oxyde inerte pour former un mélange ; à sécher et à calciner le mélange pour donner au moins un oxyde métallique sur la surface de la poudre ; et à réduire l'oxyde métallique en un métal particulaire.
PCT/SG2014/000108 2013-03-06 2014-03-06 Procédé de préparation d'un catalyseur métallique supporté à forte dispersion WO2014137293A1 (fr)

Applications Claiming Priority (2)

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US201361773242P 2013-03-06 2013-03-06
US61/773,242 2013-03-06

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WO2014137293A1 true WO2014137293A1 (fr) 2014-09-12

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2018203836A1 (fr) * 2017-05-05 2018-11-08 National University Of Singapore Procédé de préparation d'un catalyseur à base de d'oxyde de silicium et de métal
CN114768859A (zh) * 2022-05-27 2022-07-22 西安交通大学 适用于甲烷干重整的镍硅催化剂及其制备方法
CN116161964A (zh) * 2023-04-24 2023-05-26 德仕能源科技集团股份有限公司 一种废弃油藏制氢用填料及其制备方法

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2003068396A1 (fr) * 2002-01-29 2003-08-21 Exxonmobil Research And Engineering Company Activation d'un catalyseur supporte fischer-tropsch
WO2007073044A1 (fr) * 2005-12-23 2007-06-28 Sk Energy Co., Ltd. Catalyseur a base de platine pour la reaction d'oxydoreduction et son utilisation
WO2008109877A1 (fr) * 2007-03-08 2008-09-12 Virent Energy Systems, Inc. Synthèse de combustibles et de produits chimiques liquides à partir d'hydrocarbures oxygénés
US20110251055A1 (en) * 2010-04-13 2011-10-13 Millennium Inorganic Chemicals, Inc. Supported Precious Metal Catalysts Via Hydrothermal Deposition

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2003068396A1 (fr) * 2002-01-29 2003-08-21 Exxonmobil Research And Engineering Company Activation d'un catalyseur supporte fischer-tropsch
WO2007073044A1 (fr) * 2005-12-23 2007-06-28 Sk Energy Co., Ltd. Catalyseur a base de platine pour la reaction d'oxydoreduction et son utilisation
WO2008109877A1 (fr) * 2007-03-08 2008-09-12 Virent Energy Systems, Inc. Synthèse de combustibles et de produits chimiques liquides à partir d'hydrocarbures oxygénés
US20110251055A1 (en) * 2010-04-13 2011-10-13 Millennium Inorganic Chemicals, Inc. Supported Precious Metal Catalysts Via Hydrothermal Deposition

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2018203836A1 (fr) * 2017-05-05 2018-11-08 National University Of Singapore Procédé de préparation d'un catalyseur à base de d'oxyde de silicium et de métal
CN114768859A (zh) * 2022-05-27 2022-07-22 西安交通大学 适用于甲烷干重整的镍硅催化剂及其制备方法
CN114768859B (zh) * 2022-05-27 2023-08-15 西安交通大学 适用于甲烷干重整的镍硅催化剂及其制备方法
CN116161964A (zh) * 2023-04-24 2023-05-26 德仕能源科技集团股份有限公司 一种废弃油藏制氢用填料及其制备方法
CN116161964B (zh) * 2023-04-24 2023-08-15 德仕能源科技集团股份有限公司 一种废弃油藏制氢用填料及其制备方法

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