- FLUORINE REMOVAL FROM ANTIMONY FLUOROHALIDE CATALYST USING CHLOROCARBONS
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A method of chlorinating a antimony fluorohalide catalyst is disclosed. In one embodiment the method comprises contacting an antimony fluorohalide catalyst that contains one or more fluorines with a regenerating agent chosen from 2-chloro-3,3,3-trifluoropropene (1233xf), 1,1,1,3-tetrachloropropane (250fb), 2-chloro-1,1,1,2-tetrafluoropropane (HCFC-244bb) and combinations of 1233xf, 250fb, and 244bb, under conditions effective to exchange at least one fluorine in the antimony fluorohalide catalyst with chlorine. The method can be used to regenerate spent antimony fluorohalide catalyst, for example regenerating SbCl5 from SbF5.
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Paragraph 0056-0065
(2020/03/29)
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- On tetrachlorophosphonium chlorometallates of rhenium and molybdenum: Syntheses, crystal structures, and magnetism of [PCl4]2[Re2Cl10] and [PCl4]3[ReCl6]2, and the magnetic properties of [PCl4]2[Mo2Cl10]
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MoCl4, ReCl4, and ReCl5 react with PCl5 in sealed glass ampoules at temperatures between 220° and 320° to [PCl4]2[Mo2Cl10] (1) [PCl4]2[Re2Cl10] (2), and [PCL4]3[ReCl6]2 (3). 2 crystallizes isotypically to the previously reported 1 and the respective titanium and tin containing analogues. The structure (triclinic, P1 Z = 1, a = 897.3(2), b = 946.0(2), c = 687.13(9) pm, α = 95.59(2)°, β = 95.80(2)°, γ = 101.07(2)°, V = 565.4(2) 106 pm3) is built of tetrahedral [PCl4]+ and edge sharing double octahedral [Re2Cl10]2- ions and can be derived from a hexagonal closest packing of Cl- ions with tetrahedral and octahedral holes partially filled by P(V) and Re(IV), respectively. 3 crystallizes isotypically to [PCL4]3[PCl6][MCl6] (M = Ti, Sn) (tetragonal, P 42/mbc, Z = 4, a = 1496.2(1), c = 1363.2(2) pm). Because no evidence was found for the presence of [PCl6]- ions, Re in 3 has to be of mixed valency with ReIV and ReV sharing the same crystallographic site. The structure can be derived from a cubic closest packing or alternatively from an only sparsely distorted body centered cubic arrangement of Cl- ions which is rarely found for anion arrays. The tetrahedral and octahedral holes are partially filled by PV and MIV/V, respectively. Magnetic measurements show all three compounds to be paramagnetic and confirm the oxidation state IV for Mo and Re in 1 and 2 and the mixed valence (IV/V) for Re in 3.
- Beck,Mueller-Buschbaum,Wolf
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p. 975 - 981
(2008/10/08)
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- Ammoxidation of saturated hydrocarbons
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The alkanes, e.g., propane, are ammoxidized into admixtures containing α,β-unsaturated nitriles, e.g., admixture of acrylonitrile and propylene, by reacting such alkane with ammonia and oxygen, in vapor phase, in the presence of a catalytically effective amount of a solid catalyst, at least one active catalytic phase of which having the empirical formula (I): optionally also containing iron and/or gallium and/or indium, in which a is a whole or fractional number equal to or greater than 1, b is a whole or fractional number equal to or greater than 0.01, and x is a whole or fractional number provided by the oxidation number of the other elements of the at least one active catalytic phase.
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- Ammoxidation of saturated hydrocarbons
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The alkanes, e.g., propane, are ammoxidized into admixtures containing α,β-unsaturated nitriles, e.g., admixture of acrylonitrile and propylene, by reacting such alkane with ammonia and oxygen, in vapor phase, in the presence of a catalytically effective amount of a solid catalyst, at least one active catalytic phase of which having empirical formula (I): in which a is a whole or fractional number equal to or greater than 1, M is iron and/or gallium and/or indium, b is a whole or fractional number equal to or greater than 0.5, and x is a whole or fractional number provided by the oxidation number of the other elements of the at least one active catalytic phase.
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- Cationic Titanium(IV) Complexes via Halide Abstraction from : Crystal and Molecular Structure of 3*2MeCN
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Treatment of (cp=η5-C5H5) with SbCl5 as chloride abstractor in acetonitrile provided hexachloroantimonate(V) salts of (1+), (2+) and (3+) respectively.With 1:1 stoichiometry red-brown crystals of 1 are obtained and with 1:2 stoichiometry light blue crystals of 2 2.Complete removal of chloride ion from requires a six-fold excess of SbCl5 when purple-blue crystals of 3 3 can be isolated.These products were characterised by analytical and spectroscopic (IR, 1H NMR) data and, in the case of 3, by a crystal structure determination.Proton NMR studies indicate the presence of intermediate halide-bridged species in solution during the sequential halide abstractions 1 --> 2 --> 3.Crystals of complex 3, obtained as the bis(solvate) from recrystallisation in acetonitrile, are monoclinic and X-ray structural analysis confirmed the formulation.The crystal structure a=19.650(4), b=19.182(4), c=12.958(3) Angstroem, β=91.612(3) deg, Z=4, R=0.0386, R'=0.0406> shows discrete cations and anions and a pseudo-octahedral co-ordination sphere for the Ti(IV).A significant trans influence of the cyclopentadienyl ligand affects Ti-N bond lengths in the complex.
- Willey, Gerald R.,Butcher, Mark L.,McPartlin, Mary,Scowen, Ian J.
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p. 305 - 310
(2007/10/02)
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- THE LOWER OXIDES OF SULFUR AND RELATED ORGANIC SULFOXIDES
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The preparation, structures, spectra and other properties of organic sulfane oxides, R2SnO (n = 3,4), and dioxides, R2SnO2 (n = 3,4), as well as of the homocyclic sulfur oxides SnO (n=6...10) and SnO2 (n = 7,12) are discussed.All compounds are sulfoxides and contain two or more homonuclear S-S bonds.
- Steudel, Ralf
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