GB1109890A - Preparation of finely divided metals - Google Patents

Preparation of finely divided metals

Info

Publication number
GB1109890A
GB1109890A GB5417765A GB5417765A GB1109890A GB 1109890 A GB1109890 A GB 1109890A GB 5417765 A GB5417765 A GB 5417765A GB 5417765 A GB5417765 A GB 5417765A GB 1109890 A GB1109890 A GB 1109890A
Authority
GB
United Kingdom
Prior art keywords
iii
ammonium
oxalate
ruthenium
ruthenate
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.)
Expired
Application number
GB5417765A
Inventor
Ivor John Buckland
George William Walkiden
Colin John Nelson Tyrrell
Gadhireddy Satyanarayan Reddy
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.)
Inco Ltd
Original Assignee
Inco Ltd
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 Inco Ltd filed Critical Inco Ltd
Priority to GB5417765A priority Critical patent/GB1109890A/en
Priority to FR88210A priority patent/FR1505252A/en
Priority to NL6617910A priority patent/NL6617910A/xx
Priority to DE19661533088 priority patent/DE1533088B2/en
Priority to BE691550D priority patent/BE691550A/xx
Priority to SE1747266A priority patent/SE304251B/xx
Publication of GB1109890A publication Critical patent/GB1109890A/en
Expired legal-status Critical Current

Links

Classifications

    • 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
    • B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
    • B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
    • B01J23/42—Platinum
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/30—Making metallic powder or suspensions thereof using chemical processes with decomposition of metal compounds, e.g. by pyrolysis
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B11/00—Obtaining noble metals
    • 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
    • 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
    • B01J37/03—Precipitation; Co-precipitation

Abstract

Finely-divided iridium or ruthenium is produced by thermally decomposing, under non-oxidizing conditions and at a temperature not exceeding 400 DEG C., a halogen-free compound containing iridium or ruthenium in a complex in which the complexing groups comprise at least one of ammonia or oxalate groups, the balance of the compound consisting of groups that decompose and volatilize at the decomposition temperature to leave no residue. Suitable compounds are:- trisoxalato iridous-III acid ammonium trisoxalato iridite-III and ruthenate-III ammonium bis-oxalato bis-hydroxo ruthenate-III ammonium oxalato bis-carbonate ruthenate-III ammonium oxalato tetra-nitrito ruthenate-III hexammino ruthenium-III oxalate oxalato tetrammino ruthenium-III oxalate. tetrammino bis-aquo ruthenium-III oxalate. Decomposition may be effected under hydrogen with or without nitrogen, or carbon monoxide. Supported catalysts may be produced by impregnating carbon or g -alumina with a solution of the complex, drying to deposit the complex and then heating to decompose the complex. Mixed catalysts consisting of iridium-ruthenium or containing other platinum-group metals may be produced by thermally decomposing mixtures of complexes. Suitable ammonium compounds of palladium, platinum and rhodium containing oxalate groups are disclosed. The finely-divided iridium and ruthenium are also useful in the production of coatings and sintered compacts.ALSO:Organic Ru and Ir compounds which may be thermally decomposed to yield finely-divided metal are prepared as follows:- (1) Ammonium trisoxalato ruthenate-III: (NH4)3[Ru(C2O4)3]. Ruthenium dioxide is dissolved in aqueous ammonium acid oxalate by heating, excess of the latter is precipitated by n-propanol after the solution has cooled, and acetone then added. (2) Ammonium bis-oxalato bis-hydroxo ruthenate-III: (NH4)3[Ru(C2O4)2(OH2)]. As (1) except that n-propanol is added to hot solution. (3) Ammonium oxalato bis-carbonato ruthenate-III: (NH4)3[Ru(C2O4)(CO3)2]. A solution of compound (1) is heated with lead carbonate and ethanol subsequently added. (4) Ammonium oxalato tetra-nitrito ruthenate-III: (NH4)3[Ru(C2O4)(NO2)4]. A solution of compound (1) is heated with silver nitrite. (5) Hexammino ruthenium-III oxalate: [Ru(NH3)6]2(C2O4)3. Ammonia gas is passed through a solution of compound (1). (6) Oxalato tetrammino ruthenium-III oxalate: [Ru(NH3)4(C2O4)]2(C2O4). Ammonia gas is passed through an aqueous suspension of compound (5). (7) Tetrammino bis-aquo ruthenium-III oxalate: <FORM:1109890/C2/1> Ethanol is added to an aqueous solution of compound (6). (8) Trisoxolato iridous-III acid: H3[Ir(C2O4)3]. Iridium dioxide is heated with aqueous oxalic acid. (9) Ammonium trisoxolato iridite-III: (NH4)3[Ir(C2O4)3] A solution of compound (8) is neutralized with potassium bicarbonate, shaken with a sulphonated polystyrene cation exchange resin in the calcium form to precipitate excess oxalate, passed through the same resin to remove potassium ions, and then passed through the resin in ammonium form.ALSO:Supported catalysts are produced by impregnating carbon or g -alumina with a solution of a halogen-free compound containing Ir or Ru in a complex in which the complexing groups comprise at least one of ammonia or oxalate groups, drying to deposit the complex, and then heating to decompose it and deposit the Ir or Ru. Suitable compounds are:- trisoxalato iridous-III acid ammonium trisoxalato iridite-III and ruthenate-III ammonium bis-oxalato bis-hydroxo ruthenate-III ammonium oxalato bis-carbonato ruthenate-III ammonium oxalato tetra-nitrito ruthenate-III hexammino ruthenium-III oxalate oxalato tetrammino ruthenium-III oxalate tetrammino bis-aquo ruthenium-III oxalate Mixed catalysts consisting of Ir-Ru or containing other Pt-group metals may be produced by thermally decomposing mixtures of complexes. Suitable ammonium compounds of Pd, Pt and Rh containing oxalate groups are also disclosed.
GB5417765A 1965-12-21 1965-12-21 Preparation of finely divided metals Expired GB1109890A (en)

Priority Applications (6)

Application Number Priority Date Filing Date Title
GB5417765A GB1109890A (en) 1965-12-21 1965-12-21 Preparation of finely divided metals
FR88210A FR1505252A (en) 1965-12-21 1966-12-20 Preparation of finely divided metals
NL6617910A NL6617910A (en) 1965-12-21 1966-12-20
DE19661533088 DE1533088B2 (en) 1965-12-21 1966-12-20 Process for the production of fine-grain iridium and ruthenium
BE691550D BE691550A (en) 1965-12-21 1966-12-21
SE1747266A SE304251B (en) 1965-12-21 1966-12-21

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
GB5417765A GB1109890A (en) 1965-12-21 1965-12-21 Preparation of finely divided metals

Publications (1)

Publication Number Publication Date
GB1109890A true GB1109890A (en) 1968-04-18

Family

ID=10470173

Family Applications (1)

Application Number Title Priority Date Filing Date
GB5417765A Expired GB1109890A (en) 1965-12-21 1965-12-21 Preparation of finely divided metals

Country Status (6)

Country Link
BE (1) BE691550A (en)
DE (1) DE1533088B2 (en)
FR (1) FR1505252A (en)
GB (1) GB1109890A (en)
NL (1) NL6617910A (en)
SE (1) SE304251B (en)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2154248A (en) * 1984-01-31 1985-09-04 Permelec Electrode Ltd Improvements in the manufacture of electrodes
GB2229453A (en) * 1989-02-02 1990-09-26 Nat Res Dev Forming a metal coating
EP0508757A1 (en) * 1991-04-08 1992-10-14 Mitsubishi Gas Chemical Company, Inc. Process for the production of fine powder
EP1283274A2 (en) * 2001-08-04 2003-02-12 OMG AG & Co. KG Chlorine-free platinum and platinum alloy powder with increased specific surface area and nitrate melting process for making the same
WO2007048311A1 (en) * 2005-10-24 2007-05-03 The University Of Hong Kong Pharmaceutical composition having a ruthenium oxalato compound and method of using the same
US11607734B2 (en) 2018-05-30 2023-03-21 Hela Novel Metals Llc Methods for the production of fine metal powders from metal compounds

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108421986B (en) * 2018-05-17 2021-06-08 贵研铂业股份有限公司 Preparation method of high-purity iridium powder

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2154248A (en) * 1984-01-31 1985-09-04 Permelec Electrode Ltd Improvements in the manufacture of electrodes
GB2229453A (en) * 1989-02-02 1990-09-26 Nat Res Dev Forming a metal coating
EP0508757A1 (en) * 1991-04-08 1992-10-14 Mitsubishi Gas Chemical Company, Inc. Process for the production of fine powder
US5250101A (en) * 1991-04-08 1993-10-05 Mitsubishi Gas Chemical Company, Inc. Process for the production of fine powder
EP1283274A2 (en) * 2001-08-04 2003-02-12 OMG AG & Co. KG Chlorine-free platinum and platinum alloy powder with increased specific surface area and nitrate melting process for making the same
EP1283274A3 (en) * 2001-08-04 2003-02-26 OMG AG & Co. KG Chlorine-free platinum and platinum alloy powder with increased specific surface area and nitrate melting process for making the same
US6814777B2 (en) 2001-08-04 2004-11-09 Umicore Ag & Co. Kg Platinum and platinum alloy powders with high surface areas and low chlorine content and processes for preparing these powders
WO2007048311A1 (en) * 2005-10-24 2007-05-03 The University Of Hong Kong Pharmaceutical composition having a ruthenium oxalato compound and method of using the same
US11607734B2 (en) 2018-05-30 2023-03-21 Hela Novel Metals Llc Methods for the production of fine metal powders from metal compounds

Also Published As

Publication number Publication date
FR1505252A (en) 1967-12-08
SE304251B (en) 1968-09-23
BE691550A (en) 1967-06-21
DE1533088A1 (en) 1969-12-04
NL6617910A (en) 1967-06-22
DE1533088B2 (en) 1974-05-22

Similar Documents

Publication Publication Date Title
Halpern et al. Formation and properties of some chlorocarbonyl complexes of ruthenium (II) and ruthenium (III)
Hawthorne et al. The Preparation and Rearrangement of the Three Isomeric B20H18-4 Ions
US4359406A (en) Highly dispersed supported group VIII metal-phosphorus compounds, and highly dispersed, supported group VIII metal-arsenic and a process for making said compounds
Asperger et al. Isomers of the Dichlorobis (l-cyclohexanediamine) cobalt (III) Ion
Allen et al. Inorganic nitrogen fixation. Nitrogen compounds of the transition metals
Jordan et al. The Preparation and Properties of Some Pentaamminecobalt (III) Complexes
GB1109890A (en) Preparation of finely divided metals
Blanchard The Volatile Metal Carbonyls.
Khan et al. Catalytic fixation of nitrogen by the photocatalytic CdS/Pt/RuO2 particulate system in the presence of aqueous [Ru (Hedta) N2]⊖ complex
CN114478648A (en) Pyridine-like pyrrole ruthenium complex, preparation method thereof and application of complex as electrocatalytic ammonia oxidation catalyst
Keenan et al. Platinum oxide catalysts
ES405711A1 (en) Process for the electrochemical manufacture of silver containing catalysts
Halpern 31 Homogeneous Catalytic Activation of Molecular Hydrogen by Metal Ions
Dollimore et al. The thermal decomposition of oxalates: Part 23. An isothermal kinetic study into the effect of the environmental atmosphere on the thermal decomposition of silver oxalate
Muro Metal Complexes with Terdentate Ligauds. I. Synthesis of Copper (II) and Nickel (II) Complexes having Salicylaldehydesemicarbazone and Related Compounds as Ligands
Chan et al. 178. Preparation and properties of cyanobisethylenediaminecobalt (III) complexes, and the role of cyanide as a substituting agent
Fesik et al. Solid-state thermal transformations in mixtures of platinum (II) tetraammine with ammonium chromate and ammonium dichromate
King 251. Researches on ammines. Part IX. Diaquo-, hydroxoaquo-, and acidohydroxo-diammines of bivalent platinum
Wendlandt et al. The thermal decomposition of metal complexes—XIII: Some tetramminepalladium (II) complexes
Krumholz A Tridentate Ligand from Pyridine-2-aldehyde and Ammonia
Broomhead et al. Ruthenium nitrosyl complexes from solutions of ruthenium (III) ammines in dilute perchloric acid
US3372006A (en) Halogen derivatives of polyhedral boron compounds
Minochi et al. The catalytic activities of methanol reforming catalysts and their preparations
Watt et al. Evidence for the Existence of an Ammine of Platinum (0)
Patil et al. Preparation and characterization of hydrazine derivatives. Part-II: Reaction of transition metal ammonium double sulphates with hydrazine hydrate