Umicore Ag & Co Kg

Graz University of Technology

Roche Palo Alto LLC

F. Hoffmann-la Roche Ag

Andreas Rivas-Nass

Ralf Karch

Angelino Doppiu

Eileen Woerner

Annika Frey

Roland Winde

Joerg Sundermeyer

Wolf Schorn

Oliver Briel

Christian Slugovc

Timo Ebert

Christina Schinagl

Birgit Emrich

Beate Heil

Gerhard Peter

Jürgen Bodo Widmer

Tobias Burkert

Michelangelo Scalone

Kurt Puentener

Jörg Sundermeyer

Michael Lennartz

Bernd Kayser

Nadine Langenscheidt-Dabringhausen

Ruben Ramon Mueller

Lisa Hamel

Grant Stephen Forman

Wolfgang Hubert Meyer

David Grosse-Hagenbrock

Juergen Widmer

Tina Schneider

Albrecht Salzer

Nadine Langenscheidt

Stefanie Mayrhofer

Eileen Wörner

Robert Paul Tooze

Ralf Wilhelm Karch

The invention relates to a method for producing aqueous preparations of complexes of platinum group metals (PGM) Pt, Pd, Rh and Ir having the general formula [M/M/M(L)(HO)(O&#x2212;)(OH)](OH&#x2014;)(H), wherein M=Ptor Pd, M=Pt, M=Rh or Ir, L is a neutral monodentate or bidentate donor ligand, and a is an integer between 1 and 4 (or 2) and/or between 1 and 6 (or 3), b is an integer between 0 and 3 (or 5), c is an integer between 0 and 3 (or 4), d is an integer between 0 and 3 (or 5), e is an integer between 0 and 2 (or 3 or 4) and f is an integer between 0 and 4 (or 5). In the method according to the invention, the hydroxo complexes HP(OH)(in the case of M=Pd), HPt(OH)(in the case of M=Ptand M=Pt) or HM(OH)(for M=RhIr) are converted in the presence of the donor ligands, wherein at least one hydroxo group of the hydro complex is exchanged. Preferably, the reaction occurs at temperatures in the range of 40 to 110&#xb0; C. with a reaction time of between 2 and 24 hours, wherein, where MA=PtII, the conversion additionally occurs in the presence of a reduction agent. The method optionally further comprises an exchange of OH anions bound outside of the complex sphere with other anions (e.g. hydrogen carbonate or carbonate anions). The aqueous preparations contain PGM complexes such as [Pt(en)](OH), [Pt(EA)](OH)or [Rh(NH)](OH)and are used to produce electroplating baths, heterogeneous catalysts or metal powders, for example.

Method for producing aqueous preparations of complexes of platinum group metals

The invention relates to a method for producing aqueous preparations of complexes of platinum group metals (PGM) Pt, Pd, Rh and Ir having the general formula [M/M/M(L)(HO)(O&#x2014;)(OH)(OH&#x2014;)(H), wherein M=Ptor Pd, M=Pt, M=Rh or Ir, L is a neutral monodentate or bidentate donor ligand, and a is an integer between 1 and 4 (or 2) and/or between 1 and 6 (or 3), b is an integer between 0 and 3 (or 5), c is an integer between 0 and 3 (or 4), d is an integer between 0 and 3 (or 5), e is an integer between 0 and 2 (or 3 or 4) and f is an integer between 0 and 4 (or 5). In the method according to the invention, the hydroxo complexes HP(OH)(in the case of M=Pd), HPt(OH)(in the case of M=Ptand M=Pt) or HM(OH)(for M=RhIr) are converted in the presence of the donor ligands, wherein at least one hydroxo group of the hydro complex is exchanged. Preferably, the reaction occurs at temperatures in the range of 40 to 110&#xb0; C. with a reaction time of between 2 and 24 hours, wherein, where MA=PtII, the conversion additionally occurs in the presence of a reduction agent. The method optionally further comprises an exchange of OH anions bound outside of the complex sphere with other anions (e.g. hydrogen carbonate or carbonate anions). The aqueous preparations contain PGM complexes such as [Pt(en)](OH), [Pt(EA)](OH)or [Rh(NH)](OH)and are used to produce electroplating baths, heterogeneous catalysts or metal powders, for example.

The invention relates to a method for producing a compound of formula MXfrom a precursor compound of formula MX, where M is a metal, X is a halide selected from F, Cl, Br, J, m is a number selected from the range 2 to 8, and n is a number selected from the range 1 to 7, with the condition that n&#x3c;m, comprising a method step in which the precursor compound is reduced with a silane compound to the compound of formula MX.

Method for the reduction of metal halides

The invention relates to tetraalkylammonium-tetra- or hexahydroxometallates such as tetraethylammonium hexahydroxoplatinate, (N(alkyl)4)y[M(OH)x], a method for the production thereof, and the use thereof for producing catalysts.

Precious metal compounds

The present invention provides a method for preparing rhodium (III) 2-ethylhexanoate solutions which supplies the reaction product with higher space yield, as well as lower sodium and chloride ion content. An aqueous solution of an alkali salt of 2-ethylhexanoate is thereby initially converted with a rhodium (III) precursor. The rhodium (III) precursor is selected from rhodium (III) chloride solution, rhodium (III) chloride hydrate, and rhodium (III) nitrate. The mixture is heated for several hours. After cooling to room temperature, the rhodium (III) 2-ethylhexanoate formed is extracted from the aqueous solution with an alcohol that is immiscible in water or a carboxylic acid that is immiscible in water, and optionally washed with aqueous mineral acid. The rhodium (III) 2-ethylhexanoate solution obtainable in this way may be used directly as catalyst in hydroformylation reactions.

Preparation of rhodium(III)-2-ethylhexanoate

The invention relates to a method for the cost-effective and environmentally friendly production of alkyl indium sesquichloride in high yield and with high selectivity and purity. The alkyl indium sesquichloride produced according to the invention is particularly suitable, also as a result of the high purity and yield, for the production, on demand, of indium-containing precursors in high yield and with high selectivity and purity. As a result of the high purity, the indium-containing precursors that can be produced are particularly suitable for metal organic chemical vapour deposition (MOCVD) or metal organic vapour phase epitaxy (MOVPE). The novel method according to the invention is characterised by the improved execution of the method, in particular a rapid process control. Owing to targeted and extensive use of raw materials that are cost-effective and have a low environmental impact, the method is also suitable for use on an industrial scale.

Method for producing alkyl-indium compounds and the use thereof

The present patent application relates to a novel organometallic compound, a process for the preparation thereof, and its use.

Organometallic compound

Preparation of Rhodium(III)-2-ethylhexanoate

The invention relates to an improved process for inexpensive and environmentally benign preparation of trialkylgallium compounds of the general formula:RGain high yield and selectivity, where R is alkyl of 1 to 4 carbon atoms. Trialkylgallium is prepared according to the invention via the intermediate stage alkylgallium dichloride (RGaCl) or dialkylgallium chloride/alkylgallium dichloride mixture (RGaCl/RGaCl). The RGaClobtained or the RGaCl/RGaClmixture also forms part of the subject-matter of the present invention. The novel process of the present invention is notable for improved process management. The process intentionally makes substantial use of inexpensive starting materials and reagents of low environmental impact and so is also useful for the industrial scale. The trialkylgallium compounds obtained are very pure and so are particularly useful as organometallic precursor for metal-organic chemical vapor deposition (MOCVD) or metal-organic vapor phase epitaxy (MOVPE) in semiconductor and microsystem technology.

Method for producing trialkylgallium compounds and the use thereof

The invention relates to a process for the cost-effective and environmentally responsible preparation of alkyl indium sesquichloride in high yield and with high selectivity and purity. The alkyl indium sesquichloride prepared in accordance with the invention is particularly suitable, also as a result of its high purity and yield, for preparation of indium-containing precursors in accordance with demand, in high yield and with high selectivity and purity. As a result of the high purity, the indium-containing precursors that are preparable are particularly suitable for metal-organic chemical vapor deposition (MOCVD) or metal-organic vapor phase epitaxy (MOVPE). The novel process according to the invention is characterized by the improved execution of the process, in particular by rapid process control. Owing to targeted and extensive use of raw materials that are inexpensive and have a low level of environmental pollution, the process is also suitable for use on an industrial scale.

Process for preparing alkyl-indium compounds and the use thereof

The invention relates to a method for the cost-effective and environmentally friendly production of alkyl indium sesquichloride in high yield and with high selectivity and purity. The alkyl indium sesquichloride produced according to the invention is particularly suitable, also as a result of the high purity and yield, for the production, on demand, of indium-containing precursors in high yield and with high selectivity and purity. As a result of the high purity, the indium-containing precursors that can be produced are particularly suitable for metal organic chemical vapor deposition (MOCVD) or metal organic vapor phase epitaxy (MOVPE). The novel method according to the invention is characterized by the improved execution of the method, in particular a rapid process control. Owing to targeted and extensive use of raw materials that are cost-effective and have a low environmental impact, the method is also suitable for use on an industrial scale.

The invention relates to a method for producing aqueous preparations of complexes of platinum group metals (PGM) Pt, Pd, Rh and Ir having the general formula [M/M/M(L)(HO)(O&#x2014;)(OH)](OH&#x2014;)(H), wherein M=Ptor Pd, M=Pt, M=Rh or Ir, L is a neutral monodentate or bidentate donor ligand, and a is an integer between 1 and 4 (or 2) and/or between 1 and 6 (or 3), b is an integer between 0 and 3 (or 5), c is an integer between 0 and 3 (or 4), d is an integer between 0 and 3 (or 5), e is an integer between 0 and 2 (or 3 or 4) and f is an integer between 0 and 4 (or 5). In the method according to the invention, the hydroxo complexes HP(OH)(in the case of M=Pd), HPt(OH)(in the case of M=Ptand M=Pt) or HM(OH)(for M=RhIr) are converted in the presence of the donor ligands, wherein at least one hydroxo group of the hydro complex is exchanged. Preferably, the reaction occurs at temperatures in the range of 40 to 110&#xb0; C. with a reaction time of between 2 and 24 hours, wherein, where MA=PtII, the conversion additionally occurs in the presence of a reduction agent. The method optionally further comprises an exchange of OH anions bound outside of the complex sphere with other anions (e.g. hydrogen carbonate or carbonate anions). The aqueous preparations contain PGM complexes such as [Pt(en)](OH), [Pt(EA)](OH)or [Rh(NH)](OH)and are used to produce electroplating baths, heterogeneous catalysts or metal powders, for example.

The present invention relates to a process for preparing hydridocarbonyltris(triphenylphosphine)rhodium(I), RhH(CO)(PPh), also referred to hereinafter as 'Rh-hydrido.' An alcoholic suspension of triphenylphosphine is stirred with an Rh(III) chloride precursor at elevated temperature. The Rh(III) chloride precursor used may be rhodium(III) chloride hydrate RhCl*xHO or rhodium(III) chloride solution H[RhCl]*(HO). After cooling, alcoholic alkali metal hydroxide solution is added, and the mixture is stirred for a few hours. Finally, sparging is effected with CO gas and the Rh-hydrido formed is removed. Rh-hydrido can be prepared by this process on the industrial scale with high yields and at very good quality.

Process for preparing hydridocarbonyltris(triphenylphosphine)rhodium(I)

The invention relates to a process for preparing trialkylmetal compounds of the general formula RM (where M=metal of group IIIA of the Periodic Table of the Elements (PTE), preferably gallium or indium, and R=C-C-alkyl, preferably methyl or ethyl). The process is based on the reaction of metal trichloride (MeCl) with alkylaluminium sesquichloride (RAlCl) in the presence of at least one alkali metal halide as auxiliary base. The reaction mixture is heated to a temperature above 120&#xb0; C. and the trialkylmetal compound is separated off from the reaction mixture via a separator, with partially alkylated products being at the same time recirculated to the reaction mixture. In a further step, the reaction mixture is heated to a maximum of 350&#xb0; C. and the remaining alkylated and partially alkylated products are separated off. The products obtained in this way can optionally be recycled in the process. The process displays a high yield of trialkylmetal compound and also a high metal utilization; the products are used as precursors for MOCVD processes.

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Schriesheim, Germany

Andreas Rivas-Nass