E.i. Dupont De Nemours and Company

Shekhar Subramoney

Allen Capron Sievert

Velliyur Nott Mallikarjuna Rao

H David Rosenfeld

Munirpallam Appadorai Subramanian

Graciela Beatriz Blanchet-Fincher

William L Holstein

Mario Joseph Nappa

Norman Herron

Joseph V Kurian

Velliyur Nott Rao

Jing Chung Chang

John Gerard Lavin

Syed Ismat Ullah Shah

Germain Francois Rivard

Sandra G Fitzpatrick-McElligott

Tammy Georgette Amos

David H Rosenfeld

A process is disclosed for the manufacture of 1,1,1,3,3,3-hexafluoropropane and 1,1,1,2,3,3-hexafluoropropane, hexafluoropropene and/or 1,1,1,2,3,3,3-heptafluoropropane. The process involves (a) reacting HF, Cl, and at least one halopropene of the formula CXCCl&#x2550;CClX (where each X is independently F or Cl) to produce a product comprising CFCClCFand CFCClFCClF; (b) reacting CFCClCFand CFCClFCClFproduced in (a) with hydrogen, optionally in the presence of HF, to produce a product comprising CFCHCFand at least one of CHFCHFCF, CFCF&#x2550;CFand CFCFHCF; and (c) recovering from the product produced in (b), CFCHCFand at least one of CHFCHFCF, CFCF&#x2550;CFand CFCFHCF. In (a), the CFCClCFand CFCClFCClFare produced in the presence of a chlorofluorination catalyst including (i) a crystalline alpha-chromium oxide where at least 0.05 atom % of the chromium atoms in the alpha-chromium oxide lattice are replaced by divalent copper, and/or (ii) a chromium-containing composition of (i) which has been treated with a fluorinating agent.

Process or the preparation of 1,1,1,3,3,3-hexafluoro-propane and at least one of 1,1,1,2,3,3-hexafluoropropane, hexafluoropropane and 1,1,1,2,3,3,3-heptafluoropropane

A process for the manufacture of CFCH&#x2550;CFand CFCF&#x2550;CHF is disclosed. The process involves (a) reacting HF and chlorine and at least one halopropene of the formula CXCCI&#x2550;CCIX (where each X is independently F or Cl) to produce a product including both CFCCICFand CFCCIFCCIF; (b) reacting CFCCICFand CFCCIFCCIFproduced in (a) with hydrogen to produce a product including both CFCHCFand CFCHFCHF; (c) dehydrofluorinating CFCHCFand CFCHFCHFproduced in (b) to produce a product including both CFCH&#x2550;CFand CFCF&#x2550;CHF; and (d) recovering CFCH&#x2550;CFand CFCF&#x2550;CHF from the product produced in (c). In (a), both CFCCICFand CFCCIFCCIFare produced in the presence of a chlorofluorination catalyst consisting of (i) compositions comprising a crystalline alpha-chromium oxide where at least 0.05 atom % of the chromium atoms in the alpha-chromium oxide lattice are replaced by copper, and (H) compositions of (i) which have been treated with a fluorinating agent.

Process for the preparation of 1,1,3,3,3-pentafluoropropene and 1,2,3,3,3-pentafluoropropene

A process for the manufacture of CFCH&#x2550;CHF and/or CFCF&#x2550;CHis disclosed. The process involves (a) reacting HF and chlorine and at least one halopropene of the formula CXCCI&#x2550;CCIX (where each X is independently F or Cl) to produce a product including both CFCCICCIFand CFCCIFCCIF; (b) reacting CFCCICCIFand CFCCIFCCIF produced in (a) with hydrogen to produce a product including both CFCHCHFand CFCHFCHF; (c) dehydrofluorinating CFCHCHFand CFCHFCHF produced in (b) to produce a product including both CFCH&#x2550;CHF and CFCF&#x2550;CH; and (d) recovering CFCH&#x2550;CHF and/or CFCF&#x2550;CHfrom the product produced in (c). In (a), both CFCCICCIFand CFCCIFCCIF are produced in the presence of a chlorofluorination catalyst consisting of (i) compositions comprising a crystalline alpha-chromium oxide where at least 0.05 atom % of the chromium atoms in the alpha-chromium oxide lattice are replaced by copper, and (ii) compositions of (i) which have been treated with a fluorinating agent.

Process for the preparation of 1,3,3,3-tetrafluoropropene and/or 2,3,3,3-tetrafluoropropene

A process for the manufacture of CFCH&#x2550;CHF and/or CFCH&#x2550;CFis disclosed. The process involves (a) reacting HF and at least one halopropene of the formula CXCCI&#x2550;CCIX (where each X is independently F or CI) to produce a product including both CFCCI&#x2550;CFand CFCHCICF; (b) reacting CFCCI&#x2550;CFand/or CFCHCICFproduced in (a) with hydrogen to produce a product including CFCHCHFand/or CFCHCF; (c) dehydrofluorinating CFCHCHFand/or CFCHCFproduced in (b) to produce a product comprising CFCH&#x2550;CHF and/or CFCH&#x2550;CF; and (d) recovering CFCH&#x2550;CHF and/or CFCH&#x2550;CFfrom the product produced in (c). In (a), the CFCCI&#x2550;CFand CFCHCICFare produced in the presence of a fluorination catalyst comprising at least one chromium-containing component selected from (i) a crystalline alpha-chromium oxide where at least 0.05 atom % of the chromium atoms in the alpha-chromium oxide lattice are replaced by divalent copper, and (ii) a chromium-containing composition of (i) which has been treated with a fluorinating agent.

Process for the preparation of 1,3,3,3-tetrafluoropropene and/or 1,1,3,3,3-pentafluoropropene

A process for the manufacture of CFCHCHFand/or CFCHCFis disclosed. The process involves (a) reacting HF and at least one halopropene of the formula CXCCI&#x2550;CCIX (where each X is independently F or Cl) to produce a product including both CFCCI&#x2550;CFand CFCHCICF; (b) reacting CFCCI&#x2550;CFand/or CFCHCICFproduced in (a) with hydrogen to produce a product including CFCHCHFand/or CFCHCF; and (c) recovering CFCHCHFand/or CFCHCFfrom the product produced in (b). In (a), the CFCCI&#x2550;CFand CFCHCICFare produced in the presence of a fluorination catalyst comprising at least one chromium-containing component selected from (i) a crystalline alpha-chromium oxide where at least 0.05 atom % of the chromium atoms in the alpha-chromium oxide lattice are replaced by divalent copper, and (ii) a chromium-containing composition of (i) which has been treated with a fluorinating agent.

Process for the preparation of 1,1,1,3,3-penta-fluoropropane and/or 1,1,1,3,3,3-hexafluoropropane

A process is disclosed for the manufacture of CFCHCHFand CFCHFCHF. The process involves (a) reacting hydrogen fluoride, chlorine, and at least one halopropene of the formula CXCCl&#x2550;CClX (where each X is independently F or Cl) to produce a product including both CFCClCClFand CFCClFCClF; (b) reacting CFCClCClFand CFCClFCClF produced in (a) with hydrogen to produce a product including both CFCHCHF, and CFCHFCHF; and (c) recovering CFCHCHFand CFCHFCHF from the product produced in (b). In (a), the CFCClCFand CFCClFCClFare produced in the presence of a chlorofluorination catalyst including (i) a crystalline alpha-chromium oxide where at least 0.05 atom % of the chromium atoms in the alpha-chromium oxide lattice are replaced by divalent copper, and/or (ii) a chromium-containing composition of (i) which has been treated with a fluorinating agent.

Process for the preparation of 1,1,1,3,3-pentafluoropropane and 1,1,1,2,3-pentafluoropropane

A crystalline alpha-chromium oxide where from about 0.05 atom % to about 2 atom % of the chromium atoms in the alpha-chromium oxide lattice are substituted by nickel atoms, and optionally, additional chromium atoms in the alpha-chromium oxide lattice are substituted by trivalent cobalt atoms (provided that the total amount of the nickel atoms and the trivalent cobalt atoms in the alpha-chromium oxide lattice is no more than 6 atom %) is disclosed. Also disclosed is a chromium-containing catalyst composition comprising as a chromium-containing component the crystalline substituted alpha-chromium oxide; and a method for preparing a composition comprising the crystalline substituted alpha-chromium oxide. The method comprises (a) co-precipitating a solid by adding ammonium hydroxide to an aqueous solution of a soluble divalent nickel salt, a soluble trivalent chromium salt, and optionally, a soluble divalent or trivalent cobalt salt, that contains at least three moles of nitrate per mole of chromium in the solution, has a nickel concentration of from about 0.05 mole % to about 2 mole % of the total of nickel, chromium, and cobalt in the solution, and has a combined concentration of nickel and cobalt of no more than 6 mole % of the total of nickel, chromium, and cobalt in the solution; and after at least three moles of ammonium per mole of chromium has been added to the solution; (b) collecting the co-precipitated solid formed in (a); (c) drying the collected solid; and (d) calcining the dried solid. Also disclosed is a chromium-containing catalyst composition comprising a chromium-containing component prepared by treating said crystalline substituted alpha-chromium oxide with a fluorinating agent; and a process for changing the fluorine distribution (i.e., content and/or arrangement) in a hydrocarbon or halogenated hydrocarbon in the presence of a catalyst. The process involves using as the catalyst a composition comprising the crystalline substituted alpha-chromium oxide and/or the treated substituted alpha-chromium oxide.

Nickel-substituted and mixed nickel-and cobalt-substituted chromium oxide compositions, their preparation, and their use as catalysts and catalysts precursors

A chromium-containing catalyst is disclosed which includes both ZnCrOand crystalline &#x3b1;-chromium oxide. The ZnCrOcontains between about 10 atom percent and 67 atom percent of the chromium in the composition and at least about 70 atom percent of the zinc in the composition, and at least about 90 atom percent of the chromium present as chromium oxide in the composition is present as ZnCrOor crystalline &#x3b1;-chromium oxide. Also disclosed are a method for preparing this composition comprising ZnCrOand crystalline &#x3b1;-chromium oxide; and a chromium-containing catalyst composition prepared by treatment of the composition comprising ZnCrOand crystalline &#x3b1;-chromium oxide with a fluorinating agent. Also disclosed is a process for changing the fluorine distribution in a halogenated hydrocarbon, or incorporating fluorine in a saturated or unsaturated hydrocarbon, in the presence of at least one composition selected from the group consisting of (i) the ZnCrOand crystalline &#x3b1;-chromium oxide compositions and (ii) the ZnCrOand crystalline &#x3b1;-chromium oxide compositions which have been treated with a fluorinating agent.

Chromium oxide compositions containing zinc, their preparation and their use as catalysts and catalyst precursors

A crystalline alpha-chromium oxide where from about 0.05 atom % to about 6 atom % of the chromium atoms in the alpha-chromium oxide lattice are replaced by trivalent cobalt (Co) atoms is disclosed. Also disclosed is a chromium-containing catalyst composition comprising as a chromium-containing component the crystalline cobalt-substituted alpha-chromium oxide; and a method for preparing a composition comprising the crystalline cobalt-substituted alpha-chromium oxide. The method involves (a) co-precipitating a solid by adding ammonium hydroxide to an aqueous solution of a soluble cobalt salt and a soluble trivalent chromium salt that contains at least three moles of nitrate per mole of chromium in the solution and has a cobalt concentration of from about 0.05 mole % to about 6 mole % of the total concentration of cobalt and chromium in the solution; and after at least three moles E of ammonium per mole of chromium in the solution has been added to the solution, (b) collecting the co-precipitated solid formed in (a); (c) drying the collected solid; and (d) calcining the dried solid. Also disclosed is a chromium-containing catalyst composition comprising a chromium-containing component prepared by treating the crystalline cobalt-substituted alpha-chromium oxide with a fluorinating agent; and a process for changing the fluorine distribution (i.e., content and/or arrangement) in a hydrocarbon or halogenated hydrocarbon in the presence of a catalyst. The process involves using as the catalyst a composition comprising the crystalline cobalt-substituted alpha-chromium oxide and/or the treated cobalt-substituted alpha-chromium oxide.

Cobalt-substituted chromium oxide compositions, their preparation, and their use as catalysts and catalyst precursors

A process for the preparation of pentafluoroethane is disclosed which involves contacting a mixture comprising hydrogen fluoride and at least one starting material selected from haloethanes of the formula CXCHXand haloethanes of the formula CX&#x2550;CX, where each X is independently selected from the group consisting of F and Cl (provided that no more than four of X are F), with a fluorination catalyst in a reaction zone to produce a product mixture comprising HF, HCl, pentafluoroethane, underfluorinated halogenated hydrocarbon intermediates and less than 0.2 mole percent chloropentafluoroethane based on the total moles of halogenated hydrocarbons in the product mixture. The process is characterized by the fluorination catalyst comprising (i) a crystalline cobalt-substituted alpha-chromium oxide where from about 0.05 atom % to about 6 atom % of the chromium atoms in the alpha-chromium oxide lattice are replaced by trivalent cobalt (Co) and/or (ii) a fluorinated crystalline oxide of (i).

Process for the preparation of 1,1,1,2,2-pentafluoroethane

A process for preparing poly(trimethylene dicarboxylate) multifilament yarns and monofilaments. One process for preparing poly(trimethylene dicarboxylate) multifilament yarns includes (a) providing a polymer blend including poly(trimethylene dicarboxylate) and about 0.1 to about 10 weight % styrene polymer, by weight of the polymer in the polymer blend, (b) spinning the polymer blend to form poly(trimethylene dicarboxylate) multiconstituent filaments containing dispersed styrene polymer, and (c) processing the multiconstituent filaments into poly(trimethylene dicarboxylate) multifilament yarn including poly(trimethylene dicarboxylate) multiconstituent filaments containing styrene polymer dispersed throughout the filaments. Another process includes spinning at a speed of at least 3,000 m/m and processing a blend including poly(trimethylene dicarboxylate) to form partially oriented poly(trimethylene dicarboxylate) multifilament yarn. A poly(trimethylene terephthalate) yarn including poly(trimethylene terephthalate) multiconstituent filament containing styrene polymer dispersed throughout the multiconstituent filament. The invention is also directed to uses of the filament yarns and monofilament.

Process of making poly (trimethylene dicarboxylate) fibers

Annealed carbon soot is useful as an electron field emitter. Field emitting cathodes made up of annealed carbon soot attached to the surface of a substrate are also provided. The field emitters and field emitter cathodes are useful in vacuum electronic devices, flat panel computer and television displays, emission gate amplifiers, klystrons and lighting devices.

Annealed carbon soot field emitters and field emitter cathodes made therefrom

Process for making a field emitter cathode using a particulate field

A method for introducing a biological substance into a target which utilizes particles having a substantially pure carbonaceous surface to which is associated a biological substance wherein the particles are sufficiently small to penetrate the target without killing the target is described.

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Hockessin, DE, United States of America

Shekhar Subramoney