NEW PATENTS: January 1966
Journal Archive
NEW PATENTS: January 1966
METALS AND ALLOYS
Palladium-Silver Alloys
e. i. du pont de nemours & co British Patent 1,004,652
Pd-Ag alloys in powder form are produced by preparing a solution containing Ag and Pd nitrates and precipitating a finely divided alloy of Pd-Ag by the addition of a reducing agent, e.g. H3PO2, which reduces both metals.
Noble Metal Alloy Having High Specific Electrical Resistance
deutsche gold- und silber-scheideanstalt British Patent 1,005,292
An alloy of high specific electrical resistance consists of 18–75 wt. % Au, 20–75 wt.% Pd, 2–15 wt.% Fe and 0.4–5 wt.% of one or more of Al, B, Ga or In, any balance being unavoidable impurities.
Ruthenium Alloy of Improved Workability
the international nickel co. U.S. Patent 3,194,657
The workability of Ru metal is improved by permeating the molten Ru in a non-oxidising medium with 0.005–5 wt.% Zn, Bi, Cd, Ba, Ge, Hf or a lanthanide, maintaining the metal in a molten state until it is substantially quiescent and free from gas evolution and then allowing it to solidify.
ELECTROCHEMISTRY
Use of Platinum Anodes in Electrolytic Processes
monsanto co. U.S. Patent 3,193,475
A Pt anode and a Hg cathode have been used in various reactions involving the electrolytic coupling of olefines, hydrodimerisation of olefinic compounds, electrolysis of acrylamide and the production of adiponitrile.
ELECTRODEPOSITION AND SURFACE COATINGS
Chemical Plating Process
sperry gyroscope co. ltd. British Patent 1,003,575
Articles are chemically plated with metals by immersing the hot article in a solution of PdCl2 in a mixture of about 40% acetone and methyl salicylate, butyl formate or acetaldehyde, drying it and then immersing in the usual chemical plating bath.
Plating Bath and Process for Platinum Plating
asahi kasei kogyo kabushiki kaisha British Patent 1,003,634
Pt is electrodeposited by using a plating bath formed by dissolving NH4, K or Na sulphamate in an aqueous NH3 solution of dinitrodiamino platinic acid and carrying out the plating at about 3.0 V and pH 6.5–8.0.
Protection of Metallic Surfaces
johnson matthey & co. ltd. British Patent 1,003,848
Tarnishable and/or oxidisable metal surfaces are protected against external corrosive influences by electrodepositing a 15–50 × 10−6 inch layer of Pt and then electrodepositing 15–500 × 10−6 inch thick layer of Rh.
Protection of Metallic Surfaces
johnson, matthey & co. ltd. British Patent 1,003,849
Oxidisable metal surfaces are protected against corrosion and tarnishing by first electrodepositing on them a 15–50 × 10−6 inch thick film of Pt and then 15–500 × 10−6 inch thick Au film.
Process for Electrodeposition of a Platinum Coating and Electrolyte for the Application of Said Process
comptoir lyon-allemand, louyot & cie. British Patent 1,005,478
Up to 15μ Pt layers are electrodeposited on non-ferrous metals, e.g. Au, Ag, Ni, Cu, various alloys, etc., by using as electrolyte an aqueous solution containing 5–100 g/l fluoboric acid and 5–60 g/l Pt (II) salt or Pt (II) diaminodinitrite.
CATALYSIS
Production of Carbonyl Compounds
the distillers co. ltd. British Patent 1,001,539
Carbonyl compounds are produced by reacting a 5–8C olefine for 2 min to 5 h at 20−120°C with a mixture of a Pt group metal compound, CuCl2, H2O and a Cu salt of mono- or di-halo-acetic acid.
Catalytic Oxidation of Waste Gases
universal oil products co. British Patent 1,002,337
A waste gas stream containing combustible materials is purified by passing it, together with O2, at a suitable temperature through a bed of particulate material consisting of Al2O3 supporting 0.05–0.2 wt.% Pt and comprising 70–92 wt.% Al2O3 particles composited with 0.013−0.1 wt.% Pt and 8–30 wt.% evenly dispersed Al2O3 particles composited with 0.1–5.0 wt.% Pt.
Preparation of Alcohols
shell internationale research mij. n.v. British Patent 1,002,429
Alcohols are produced by reacting an olefinic compound with H2 and CO in an alkaline medium at 150−190°C, 400–700 psig and in the presence of a catalyst comprising a complex of Co, Ru or Rh with at least one P-containing ligand.
Conversion Process and Catalysts
union oil company of california British Patents 1,002,921–2
A catalyst system for the hydrocracking of high-boiling mineral oil fractions comprises (i) a partially decationised zeolitic aluminosilicate molecular sieve supporting a minor amount of Group VI B or VIII metal, e.g. 0.05–2 wt.% Pt or Pd and (ii) a relatively inert, powdered, refractory material of greater particle size than the crystal size of the molecular sieve.
3, 4 - Dihydro-benzoxazinones-(1,3,2) and Processes for the Production of Such Compounds
e. merck a.g. British Patent 1,003,113
3,4-Dihydro-benzoxazinone-(1,3,2) is produced by reacting 2-hydroxy-benzyl halide with a salt of cyanic acid and treating the product with H2 in the presence of supported Pd or PtO catalyst. See also 1,001,114.
Separation by Selective Catalytic Chemical Reactive Process
socony mobil oil co. inc. British Patent 1,003,251
A catalyst for the continuous separation of chemical compounds of different molecular shape but similar chemical reactivity, consists of crystalline aluminosilicate zeolite of 5–13 A pore size activated by Ag or Pt group metal.
Selective Hydrocracking
socony mobil oil co. inc. British Patent 1,003,252
A catalyst for the selective hydrocracking of hydrocarbons consists of 5–13 A crystalline aluminosilicate zeolite whose pores support catalytically active Ag, Ni, Co or Pt group metal.
Production of Organic Esters
the distillers co. ltd. British Patent 1,003,347
Organic esters are produced by reacting an olefine and an organic carboxylic acid at 50−250°C, 1–50 atm. and in the presence of a supported Pt group metal catalyst.
Tetracycline Derivatives
american cyanamid co. British Patent 1,003,474
6-Deoxy or 6-deoxy-6-demethyl tetracycline derivative containing a 7 and/or 9 amino group is prepared by reacting the corresponding 7 and/or 9 nitro derivative with 1 mole carbonyl compound and H2 in the presence of a supported Pt or Pd catalyst.
Producing Vinyl Esters of Fatty Acids
asahi kasei kogyo kabushiki kaisha British Patent 1,003,499
Vinyl esters of fatty acids are produced by flowing a mixture of an O2-containing gas, a saturated fatty acid and C2H4, at 50−300°C, over a catalyst consisting of an inert carrier supporting (i) at least one metal or oxide selected from Cu, Ag, Zn, Cd, Sn, Pb, Cr, Mo, W, Fe, Co or Ni and (ii) at least one metal selected from Pd, Pt, Rh, Ru or Ir.
Substituted Amines and Processes for Their Production
e. merck a.g. British Patent 1,003,687
New techniques for the production of substituted amines involve a hydrogenolysis stage in the presence of supported or unsupported noble metal catalysts, e.g. Pt, PtO, Pd black, etc.
Hydrocarbon Reforming and Catalyst therefor
imperial chemical industries ltd. British Patent 1,003,702
A catalyst suitable for steam reforming of hydrocarbons is produced by forming a mixture of an inert refractory oxide carrier, 1–10 wt.% alkali metal oxide or hydroxide and catalytic amount of Ni, Co, Ru, Rh, Pd, Os, Ir, Pt or their mixtures and heating at 600−900°C to increase its resistance to leaching with H2O.
Process for Hydrogen Treatment of Hydrocarbon
gulf research & development co. British Patent 1,003,715
Residual petroleum fractions are subjected to destructive hydrogenation by contacting them and H2 at 371−441°C and 35–280 kg/cm2 with a catalyst consisting of activated Al2O3 supporting minor amounts of Pt, Pd or their oxides or sulphides.
Benzophenones and Derivatives thereof
f. hoffmann-la roche & co. a.g. British Patent 1,003,936
Benzophenone derivatives are produced by reacting a 2-halo-benzophenone with benzylamine and then dibenzylating the product by hydrogenolysis in the presence of a Pd metal catalyst.
Manufacture of Naphthalene Derivatives
imperial chemical industries ltd. British Patent 1,005,024
The compounds A.CHOH.CH2.NRR′, where A is a naphthalene nucleus, R is H or Me and R′ is 1–4C alkyl are produced by reducing A.CO.CH (OH)2 in the presence of R″NRR′ (where R″ is H2 or a hydroxy radical) and preferably by catalytic hydrogenation in the presence of Pt or Raney Ni.
See also 1,005,025–7.
Process for the Preparation of 2,6-Dichloro-benzonitrile
shell internationale research mij. n.v. British Patent 1,005,067
2,6-Dichlorobenzonitrile is produced by passing a mixture of substituted 2,6-dichlorobenzenes, NH3 and O2 or O2-containing gas over a C supported Pd or Ni catalyst maintained at 150−500°C.
Oxidation of Mercurous Salts
imperial chemical industries ltd. British Patent 1,005,658
Hg(I) salts are oxidised to Hg(II) salts by reacting them with O2 in an acidic aqueous medium and in the presence of Ag, Au, Pt or Pd supported catalyst, e.g. on SiO2.
Catalytic Conversion of Hydrocarbons
standard oil co. British Patent 1,006,291
Hydrocarbons are converted to lower boiling materials by contacting them at 200–2,000 psig and 400−1,000°F with H2 in the presence of a catalyst composite comprising highly porous acid-treated Al2O3 or its mixture with a refractory metal oxide, 0.5–5 wt.% Ni, Co, Pt or Pd and 0.01–1 g atoms Group VA element/1 g atom Group VIII metal.
Dehydrogenation Catalysts
sinclair research inc. U.S. Patent 3,190,932
Methylcyclopentane is converted to C6H6 by passing it, together with molecular H2, at 800−1,000°F and 150–400 p.s.i.g. in contact with a catalyst consisting of 0.01–2 wt.% Pt group metal, preferably Pt supported on activated Al2O3.
Reduction of Isonicotinic Acid Esters
fmc corp. U.S. Patent 3,192,220
Lower alkyl esters of isonicotinic acid are reduced to the corresponding piperidine derivatives by reacting the ester with H2 at 35−150°C and up to 500 p.s.i.g. in the presence of a supported catalyst providing 0.005–2 g Pd/mole of the ester.
Improved Hydrocarbon Cracking Catalysts
socony mobil oil co. inc. U.S. Patent 3,193,491
Improved, solid, porous hydrocracking catalysts are produced by mixing aqueous solutions of Zr, Al and alkali metal silicate salts, allowing the mixture to set to a hydrosol, transforming it into a hydrogel and then combining it with a Group VI or VIII metal, oxide or sulphide, such as Pt, Pd or Mo.
Platinum Group Metal Hydrogenation Catalysts
merck & co. inc. U.S. Patent 3,193,550
Reduced cephalosporin C derivatives are produced by reducing an alkyl ester derivative of N-acyl cephalosporin C in a solvent medium with H2 at 25−100°C, 1000–30,000 p.s.i. and in the presence of a Pt metal catalyst.
Dehalogenated Platinum-on-Alumina Reforming Catalysts
air products & chemicals inc. U.S. Patent 3,194,755
Improved catalysts are produced by forming sorptive Al2O3 particles free from Cl2, impregnating them with aqueous H2PtCl6 acid solution to produce a Pt content of 0.1–2 wt.% treating them with gaseous H2S at 60−140°F and then with NH3, washing to reduce Cl2 content and drying.
Rhodium Hydrogenation Catalyst
abbott laboratories inc. U.S. Patent 3,194,839
Aromatic amino compounds are produced by hydrogenating the corresponding nitro compounds at 25−150°C, 1 atm to 150 p.s.i. and in the presence of an almost spent Rh catalyst.
Regeneration of Platinised Carbon Catalysts
halcon international inc. U.S. Patent 3,194,843
Spent Pt catalysts on C supports are regenerated by leaching with H2O until the leachings are free from organic material and then separating the regenerated material.
Olefine Hydrogenation in Alkyl Benzene Production
esso research & engineering co. U.S. Patent 3,196,174
In the production of biodegradable perhydro-bis-(isoprenyl)-alkyl aryl sulphonates, the reduction of the olefines is accomplished using Pd/C.
Reductive Cyclohexylamine Production
abbott laboratories U.S. Patent 3,196,179
Aniline is reduced to cyclohexylamine at elevated temperature and pressure over a Rh catalyst, preferably supported elemental Rh.
Catalytic 2-Oximinoindane Reduction
cuba corp. U.S. Patent 3,196,181
The reduction of this compound to 2-amino-indane is catalysed by a non-pyrophoric supported Pd catalyst in the presence of H2SO4 and acetate ions.
Improving Front End Octane Rating
socony mobil oil co. inc. U.S. Patent 3,198,728
Naphtha containing naphthenes and paraffins are treated first over a Pt group metal reforming catalyst and then over a non-noble metal sulphide dehydrogenating catalyst.
Loading Molecular Sieves with Catalysts
union carbide corp. U.S. Patent 3,200,082
Catalytic metals, including Au, Ag, and Pt metals, are more easily loaded on to zeolites in the form of their complexes with amines, e.g. tetramine platinous chloride. See also 3,200,083.
Deoxytetracycline Production
chas. pfizer & co. inc. U.S. Patent 3,200,149
The hydrogenation of 6-deoxy-6-dimethyl-6-methylene-tetracyclines over Pt metal catalysts produces the 6-epi-6-deoxytetracyclines.
Dehydrogenation Catalysts
centre national de la recherche scientifique French Patent 1,391,114
Alkylanthraquinones are dehydrogenated to alkenylanthraquinones by contacting them at 400−600°C and in an inert gas atmosphere with a Pt, Pd or their oxides catalyst.
Production of Formyl Carboxylic Acids
soc. d’electrochimie, d’electrometallurgie et des acieries electriques d’ugine French Patent 1,394,863
These γ-formyl carboxylic acids are produced by reduction of the corresponding unsaturated acids over a Pd catalyst.
Catalytic Olefine Oxidation Process
farbwerke hoechst a.g. German Patent 1,197,071
The oxidation of olefines to aldehydes, ketones or acids over a supported PdCl/CuCl2 catalyst system is effected in a plurality of catalyst beds in sequence using H2O injection for cooling.
FUEL CELLS
Fuel Cell Electrode
leesona corp. British Patents 1,001,523–5
A fuel cell electrode consists of a porous hydrophobic polymer structure, the side thereof facing the gas or liquid feed being in intimate contact with a porous ion exchange resin film and the side facing the electrolyte being coated with Ag, Au, Ru, Rh, Pd, Os, Ir, Pt or some other catalytically active metal.
Carbon-supported Fuel Cell Catalyst Electrode
esso research & engineering co. U.S. Patent 3,196,050
A C catalyst is produced by impregnating a C electrode with an aqueous solution of a catalyst metal, e.g. Pt, and then heating it at 600−900°F in a CO atmosphere to remove O2 and then at 1000−1800°F in an H2 atmosphere to reduce the metal.
ELECTRICAL AND ELECTRONIC ENGINEERING
Metal-Glass Resistance Material
beckman instruments inc. British Patent 1,002,791
A resistance device comprises a high temperature resistant, electrically non-conductive base having fired on it a resistance layer formed of 50−84 wt.% glass and 16−50 wt.% finely dispersed alloy of Ir with at least one metal selected from Au, Pd or Ag.
Metal-Glass Resistance Materials
beckman instruments inc. British Patent 1,002,793
A metal-glass resistance material designed to be fired on to a non-conductive base member consists of a finely divided mixture of 60−99 wt.% glass and 1−40 wt.% Ru or its alloy with Au, Pd, Pt or their mixtures.
Solion
general electric co. British Patent 1,003,529
An integrator assembly for solion devices comprises an envelope containing the electrolyte, a Pt metal anode, a pair of porous graphite cathodes placed on each side of the anode and connectors projecting beyond the envelope.
Methods of Manufacturing Semiconductor Devices
mullard ltd. British Patent 1,004,048
Good ohmic and p-n junctions are produced in semiconductor bodies consisting of a III–V or substituted III–V semiconductor compound by using alloys of 0.5−5 wt.% Pt and 95−99.5 wt.% Sn.
Electrical Capacitors
e. i. du pont de nemours & co. British Patent 1,004,653
A Pd-Ag alloy metallising composition, e.g. for stencil application, for use in capacitor electrode production, comprises 30−60% Pd-Ag alloy powder, which contains 95−60% Pd and 5−40% Ag, dispersed in 70−40% of an inert vehicle, preferably an organic vehicle.
Electrical Components
daystrom inc. British Patent 1,006,238
A composite resistance unit is made by depositing on the non-conductive substrate a catalytic film of Ni, Fe, Co, Ru, Ph, Pd, Os, Ir or Pt, depositing a thin film of electrically resistive material, e.g. Ni and finely divided P, by means of a chemical reduction process and then heat-treating the unit at 250−650°F for several hours to modify its temperature coefficient of resistance and to stabilise its resistance value.
Electrical Conductor
imperial chemical industries ltd. British Patent 1,006,394
An electrical conductor comprises a casing of Ti or its alloy with up to 14 wt.% Zr or up to 5 wt.% Pt, Rh or Ir, coated on its internal surface with an adherent film of Cu or Ni and a tightly fitting Cu, Al, Fe or steel core fixed by means of a fusible metal or metal alloy solder.