EP0642468A4 - Verfahren zur herstellung von mischmetalloxide. - Google Patents

Verfahren zur herstellung von mischmetalloxide.

Info

Publication number
EP0642468A4
EP0642468A4 EP93909675A EP93909675A EP0642468A4 EP 0642468 A4 EP0642468 A4 EP 0642468A4 EP 93909675 A EP93909675 A EP 93909675A EP 93909675 A EP93909675 A EP 93909675A EP 0642468 A4 EP0642468 A4 EP 0642468A4
Authority
EP
European Patent Office
Prior art keywords
metal
carbonate
cation
process according
containing compound
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP93909675A
Other languages
English (en)
French (fr)
Other versions
EP0642468A1 (de
Inventor
Terence William Turney
Karl Foger
Manh Hoang
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Commonwealth Scientific and Industrial Research Organization CSIRO
Original Assignee
Commonwealth Scientific and Industrial Research Organization CSIRO
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Commonwealth Scientific and Industrial Research Organization CSIRO filed Critical Commonwealth Scientific and Industrial Research Organization CSIRO
Publication of EP0642468A1 publication Critical patent/EP0642468A1/de
Publication of EP0642468A4 publication Critical patent/EP0642468A4/de
Withdrawn legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G53/00—Compounds of nickel
    • 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
    • B01J23/002—Mixed oxides other than spinels, e.g. perovskite
    • 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
    • B01J37/08—Heat treatment
    • B01J37/082—Decomposition and pyrolysis
    • B01J37/088—Decomposition of a metal salt
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
    • C01B13/14—Methods for preparing oxides or hydroxides in general
    • C01B13/18—Methods for preparing oxides or hydroxides in general by thermal decomposition of compounds, e.g. of salts or hydroxides
    • C01B13/185—Preparing mixtures of oxides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F17/00—Compounds of rare earth metals
    • C01F17/30—Compounds containing rare earth metals and at least one element other than a rare earth metal, oxygen or hydrogen, e.g. La4S3Br6
    • C01F17/32—Compounds containing rare earth metals and at least one element other than a rare earth metal, oxygen or hydrogen, e.g. La4S3Br6 oxide or hydroxide being the only anion, e.g. NaCeO2 or MgxCayEuO
    • C01F17/34—Aluminates, e.g. YAlO3 or Y3-xGdxAl5O12
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F5/00—Compounds of magnesium
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00—Compounds of aluminium
    • C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
    • C01F7/028—Beta-aluminas
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00—Compounds of aluminium
    • C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
    • C01F7/16—Preparation of alkaline-earth metal aluminates or magnesium aluminates; Aluminium oxide or hydroxide therefrom
    • C01F7/162—Magnesium aluminates
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00—Compounds of aluminium
    • C01F7/78—Compounds containing aluminium, with or without oxygen or hydrogen, and containing two or more other elements
    • C01F7/782—Compounds containing aluminium, with or without oxygen or hydrogen, and containing two or more other elements containing carbonate ions, e.g. dawsonite
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G25/00—Compounds of zirconium
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G25/00—Compounds of zirconium
    • C01G25/02—Oxides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G53/00—Compounds of nickel
    • C01G53/80—Compounds containing nickel, with or without oxygen or hydrogen, and containing one or more other elements
    • C01G53/82—Compounds containing nickel, with or without oxygen or hydrogen, and containing two or more other elements
    • 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
    • B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/30—Three-dimensional structures
    • C01P2002/32—Three-dimensional structures spinel-type (AB2O4)
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/50—Solid solutions
    • C01P2002/52—Solid solutions containing elements as dopants
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/12—Surface area
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/12—Surface area
    • C01P2006/13—Surface area thermal stability thereof at high temperatures

Definitions

  • a METHOD FOR PREPARING MIXED METAL OXIDES The present invention relates to a process for preparing mixed metal oxides by cation-exchange from anionic carbonate-containing compounds.
  • Mixed metal oxide phases known in the prior art have a wide variety of applications including use by themselves or as components in catalysts, corrosion resistant coatings, glazes, electrically conducting coatings, pigments, cosmetics, fillers, pharmaceuticals, plastics additives, alloy precursors and phosphors.
  • Mixed metal oxides may consist of single phases, comprised of two or more metal species in chemical combination with oxygen, or of intimate mixtures of two or more phases.
  • Industrial processes known in the prior art for preparation of mixed metal oxides include:
  • Y 2 0 3 -stabilised zirconias which have applications as high performance ceramic, are usually prepared by chemical co-precipitation of hydroxides followed by calcination at high temperature.
  • the distribution of the stabilising oxides depends on the detailed method of preparation. This process, whilst again useful, suffers from similar problems to other chemical co-precipitation processes.
  • Binary oxides such as those with spinel or perovskite structures,and which may be used in the ceramic and catalysis areas, are usually made by fusion or solid state reaction of intimately mixed powders chemical precipitation. Many of these methods afford products which are compositionally heterogeneous or have low surface areas, and hence are often unsuitable for use as catalysts.
  • a process for preparing a mixed metal oxide which process includes providing a metal carbonate-containing compound including a metal carbonate-containing anion with at least one cation; and at least a second cation; subjecting the metal carbonate-containing compound to ion exchange with the second cation to form a mixed metal-carbonate complex; and subjecting the complex to a heating step to form a mixed metal oxide.
  • the process according to the present invention is characterised in that production of mixed metal oxides requires only a simple process and the reaction conditons needed are relatively mild.
  • the complex is heated to significantly lower temperatures than required in the prior art.
  • the precursor compounds used may be relatively inexpensive to produce.
  • the ratio of the metal and second cation can be varied quantitatively as required.
  • Heating or calcining the mixed metal-carbonate complex may assist in decomposing any intermediate complex species formed, to form a mixed metal oxide.
  • the metal carbonate-containing anion in the metal carbonate compound may be of any suitable type. Most preferably, the metal carbonate-containing anion may be - A - selected from anions of the general formula:
  • M is selected from Be, Mg, Al, Ga, Sc, Y, rare earths, Ti, Zr, Hf, V, Nb, Ta, Cr, Mo, W, Mn, Sn Cd, Pb or mixtures thereof;
  • X is an anionic ligand; (typical anionic ligands include SCN, halide, phosphate, oxalate or an organic ligand) ; n, x, y, v and z are an integer or non-integer having a value between 0 and approximately 6 depending upon the metal, its oxidation state and its coordination requirements, with the proviso that v 0.
  • the metal carbonate-containing anion in the metal carbonate containing compound may be obtained from any suitable source, such as, a pure inorganic salt or co-ordination complex, a simple metal or mixed metal oxide, a mineral ore or concentrate or spent catalysts, e.g. as industrial manufacturing or waste products.
  • the cation in the metal carbonate compound may be of any suitable type.
  • the cation may be selected from one or more of NH., an alkali metal, an alkaline earth, a substituted ammonium, phosphonium or arsonium, Zn, Mg, Tl or mixtures thereof.
  • the second cation utilized in the ion exchange step may be of any suitable type.
  • the second cation contains a metal which may be selected from one or more of Co, Ni,
  • the second cation may be provided in the form of a hydroxide, oxide, carbonate, nitrate or acetate.
  • the metal carbonate-containing compound may be utilized in any suitable form.
  • the compound may be utilized alone, that is in the solid state, or in the form of a solution.
  • metal-carbonate compounds that may be utilized in the process of the present invention include the following compositions:
  • a process for preparing a mixed metal oxide which process includes providing a metal carbonate-containing compound selected from
  • the metal carbonate-containing compound is selected from; K 2 [Mg(C0 3 ) 2 ] (NH 4 )[A1(0H)(C0 3 ) 3 ] or (NH 4 )[Zr(OH)(C0 3 ) 3 ]
  • the ion exchange reaction may be performed in any suitable solvent, such as water or methanol and at a suitable temperature.
  • the temperature should be high enough to complete the exchange reaction, but low enough to deter any decomposition of the carbonate complex. Temperatures in the range of approximately 2°C to 100°C are preferred. However temperatures in the range of approximately 5°C to 40°C have been found to be most suitable.
  • the reaction product may then be heated at elevated temperatures to decompose any intermediate complex. Most suitably the heating may continue for approximately 4 to 48 hours. Temperatures in the range of approximately 25°C to 1600°C, depending upon the combination of metals selected and end use proposed. Preferably approximately 400°C to 1200°C may be used. Most preferably the temperature may be raised progressively to reach a maximum temperature of approximately 1200°C.
  • Materials which stabilise the metal carbonate in solution such as inorganic or organic ligands, ammonium carbonate, NH_ or CO ? may optionally be added.
  • the pH or acidity of the solution should be such as to minimise any solvolysis reaction or displacement of the coordinated carbonate.
  • the degree of ion exchange may be controlled by choice of a time sufficient for completion of the reaction or by repetitive exchange, or by an appropriate choice of the concentrations and ratios of the reactants.
  • the composition of the resulting mixed oxide may be controlled by full or partial ion exchange of initial cation with the second cation in the appropriate proportions.
  • the ion exchange product may be anhydrous or hydrated or mixed hydroxide, carbonate, hydroxycarbonate, or oxo complexes or a combination thereof. These, complexes may be converted into the anhydrous mixed oxide by an appropriate thermal treatment.
  • the ion exchange reaction may be performed in any suitable vessel, either in the slurry phase, or in solution. Alternatively, the metal-carbonate component may be coated onto or impregnated in any suitable porous or non-porous substrate and the ion exchange reaction performed subsequently.
  • Mixed oxides prepared by the process of the present invention may contain two or more different kinds of cations at varying proportions and may be a single phase chemical compound, a solid solution, or a mixture of compounds.
  • Typical mixed metal oxides may be selected from ⁇ aluminas, such as Ba0.6Al 2 0 3 , La_0 3 .11A1 2 0 3 , Y 2 0 3 stabilized Zirconia, Ni supported on Zirconia and Ni supported on Alumina and binary oxides such as BaZr0 3 .
  • the ⁇ aluminas may exhibit increased surface areas.
  • the Yttrium-stablized zirconia may exhibit an improved distribution of the stabilizing oxide.
  • the binary oxides may exhibit improved compositional homogeneity and increased surface area.
  • the mixed metal oxides according to the present invention may function as supported metal catalyst precursors.
  • Supported metal catalysts comprise an active metallic phase dispersed over a support material.
  • the primary role of the support is to achieve a high surface area active metal phase and to maintain this high area by stabilising the catalyst against agglomeration and coalescence.
  • the support also acts to improve the poison resistance of the catalyst and its cost.
  • support materials are acidic, basic, neutral or amphoteric oxides (exalumina, silica, silica-alumina, titania, zirconia, magnesia (MgAlO.).
  • stabilised aluminas e.g. Ba0.6Al_0_, La 2 0 3 .IlAl 2 0 3 ) are often used.
  • Supported metals are synthesised in the prior art by producing a reducible metal/support precursor (reducible metals: Co, Fe, Ni, Cu, Ag, Au, Ru, Rh, Pd, Re, Os, Ir, Pt) which is subsequently converted to the active catalyst by heat treatment in a reducing atmosphere (containing hydrogen or carbon monoxide) which produces the active metallic phase.
  • reducible metal/support precursor reducible metals: Co, Fe, Ni, Cu, Ag, Au, Ru, Rh, Pd, Re, Os, Ir, Pt
  • Catalyst precursors are commonly produced by impregnating the support with a metal compound, co-precipitation of support and metal compound, or ion exchange of a metal compound with the support.
  • the present invention provides a new method for obtaining a supported metal catalyst precursor by exchange of reducible metal ions with a metal-carbonate containing compound.
  • the metal-carbonate containing compound functions as a support precursor.
  • Subsequent heat treatment decomposes the carbonate compound to form an oxide support.
  • the active supported metal catalyst is produced by heat treatment of the obtained precursor in a reducing atmosphere.
  • a process for preparing a supported metal catalyst which process includes providing a metal carbonate-containing compound including a metal carbonate-containing anion with at least one cation; and at least a second cation; subjecting the metal carbonate-containing compound to ion exchange with the second cation to form a mixed metal-carbonate complex; subjecting the complex to a first heating step to form a mixed metal oxide; and subjecting the mixed metal oxide to a second heating step under reducing conditions to form a supported metal catalyst.
  • the temperature range and composition of the required reducing conditions is determined by the type of metal and type of precursor species. Temperatures in the range of from approximately 300°C to 1000°C may be used.
  • the second heating step may be conducted in a reducing atmosphere.
  • the reducing atmosphere may contain hydrogen or carbon monoxide.
  • mixed NiO/Zr0 2 and NiO/Al 2 0 3 phases are converted to supported Ni/Zr0 2 and
  • Ni/Al 2 0 3 catalysts by heat treatment in an atmosphere containing hydrogen in the temperature range of from approximately 400°C to 600°C.
  • Ba(OH) 2 .8H 2 0 (1.02 g) was added to a slurry of NH 4 Al(OH) 2 C0 3 nH 2 0 (7.5 g, 26.5 wt% A1 2 0 3 ) in H 2 0 (40 ml) with vigorous stirring under nitrogen at 21°C. After stirring the mixture for 3 days the solid was removed by filtration and washed with water (3 x 100 ml) . The isolated solid sample (2.3 g) was then calcined in air at 400°C for 16 hours, 600°C for 4 hours and then 800°C for 2 hours.
  • Example 2 The procedure of Example 1 was followed, except that 0.79 g of Ba(OH) 2 .8H 2 0 and 8.2 g (NH 4 )A1(0H) 2 C0 3 .nH 2 0 (26.4 wt% Al 2_0 ⁇ 3)' was used, to afford 2.4 g of product, containing 15.3 wt% BaO.
  • Example 1 The procedure of Example 1 was followed, except that La(N0 3 ) 3 .6H 2 0 (1.70 g) in ethanol (20 ml), was
  • Powder Data File (#21-1152) confirmed the presence of M ALO, as the only crystalline product.
  • the green product (0.7 g) was calcined in air at 400°C for 16 hours, 600°C for 4 hours, and 850°C for 2 hours.
  • a XRD powder pattern confirmed that NiAl_0 4 was the only crystalline phase, by comparison with the JCPDS Powder File (#10-330).

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Catalysts (AREA)
EP93909675A 1992-05-27 1993-05-17 Verfahren zur herstellung von mischmetalloxide. Withdrawn EP0642468A4 (de)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
AUPL2626/92 1992-05-27
AUPL262692 1992-05-27
PCT/AU1993/000226 WO1993024411A1 (en) 1992-05-27 1993-05-17 A method for preparing mixed metal oxides

Publications (2)

Publication Number Publication Date
EP0642468A1 EP0642468A1 (de) 1995-03-15
EP0642468A4 true EP0642468A4 (de) 1996-02-21

Family

ID=3776189

Family Applications (1)

Application Number Title Priority Date Filing Date
EP93909675A Withdrawn EP0642468A4 (de) 1992-05-27 1993-05-17 Verfahren zur herstellung von mischmetalloxide.

Country Status (3)

Country Link
EP (1) EP0642468A4 (de)
CA (1) CA2136525A1 (de)
WO (1) WO1993024411A1 (de)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6514473B2 (en) 1995-02-03 2003-02-04 Sasol Germany Gmbh Process for producing hydrotalcites and the metal oxides thereof
DE19503522A1 (de) 1995-02-03 1996-08-08 Rwe Dea Ag Herstellung gemischter schichtförmig aufgebauter Metallhydroxide sowie deren Metalloxide
RU2510620C1 (ru) * 2012-10-29 2014-04-10 Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Новосибирский национальный исследовательский государственный университет" (Новосибирский государственный университет, НГУ) Способ приготовления биметаллического катализатора окисления

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3701739A (en) * 1970-12-14 1972-10-31 Little Inc A Method for forming mixed oxide heterogenous catalysts
DD239396A1 (de) * 1985-07-15 1986-09-24 Akad Wissenschaften Ddr Verfahren zur herstellung eines stabilisierten zro tief 2-mischoxidpulvers hoher sinterfaehigkeit

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3796792A (en) * 1969-12-12 1974-03-12 Kyowa Chem Ind Co Ltd Composite metal hydroxides
US4454244A (en) * 1983-03-28 1984-06-12 Ashland Oil, Inc. New compositions
JPH01126204A (ja) * 1987-09-11 1989-05-18 W R Grace & Co 混合酸化物合成方法
US5079203A (en) * 1990-05-25 1992-01-07 Board Of Trustees Operating Michigan State University Polyoxometalate intercalated layered double hydroxides

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3701739A (en) * 1970-12-14 1972-10-31 Little Inc A Method for forming mixed oxide heterogenous catalysts
DD239396A1 (de) * 1985-07-15 1986-09-24 Akad Wissenschaften Ddr Verfahren zur herstellung eines stabilisierten zro tief 2-mischoxidpulvers hoher sinterfaehigkeit

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See also references of WO9324411A1 *

Also Published As

Publication number Publication date
WO1993024411A1 (en) 1993-12-09
CA2136525A1 (en) 1993-12-09
EP0642468A1 (de) 1995-03-15

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