Sulfur Containing Patents (Class 423/303)
  • Patent number: 11799126
    Abstract: A method of preparing a solid electrolyte and an all-solid battery including a solid electrolyte prepared by the method, the method including: contacting a first solvent and a first starting material comprising an alkali metal, sulfur, phosphorus, an element M, or a combination thereof to form a first solution; precipitating a first precursor from the first solution; contacting a second solvent, the first precursor, and a second starting material comprising an alkali metal, sulfur, phosphorus, an element M, or a combination thereof to form a second solution; precipitating a second precursor from the second solution; and heat treating the second precursor to prepare the solid electrolyte, wherein the element M comprises an element of Group 14 of the Periodic Table of the Elements, and the element M and the alkali metal in the first starting material and the second starting material are the same or different.
    Type: Grant
    Filed: May 29, 2020
    Date of Patent: October 24, 2023
    Assignee: SAMSUNG ELECTRONICS CO., LTD.
    Inventors: Tomoyuki Tsujimura, Yuichi Aihara, Nobuya Machida
  • Patent number: 9884764
    Abstract: The present invention relates to a new and simple purification process of phosphorus decasulfide (P4S10), also called phosphorus pentasulfide (P2S5), which is used as thionating agent for the syntheses of various organic compounds, particularly the organic compounds having sulfur heteroatom(s).
    Type: Grant
    Filed: June 2, 2015
    Date of Patent: February 6, 2018
    Assignee: TUBITAK
    Inventors: Erdal Ertaş, Turan Öztürk, Ipek Ösken
  • Publication number: 20150093652
    Abstract: A sulfide solid electrolyte including a sulfide product prepared by mixing at least Li2S and P2S5 in an organic solvent, wherein the organic solvent includes a tetrahydrofuran compound optionally substituted with a C1-C6 hydrocarbon group or a C1-C6 hydrocarbon group including an ether group, or a C2-C7 non-cyclic ether compound.
    Type: Application
    Filed: October 2, 2014
    Publication date: April 2, 2015
    Inventors: Yuich AIHARA, Nobuya MACHIDA, Seitaro ITO
  • Publication number: 20150037687
    Abstract: A main object of the present invention is to provide a sulfide solid electrolyte material having favorable ion conductivity and low reduction potential. The present invention solves the above-mentioned problem by providing a sulfide solid electrolyte material including an M1 element (such as a Li element), an M2 element (such as a Ge element, a Si element and a P element) and a S element, wherein the material has a peak at a position of 2?=29.58°±0.50° in X-ray diffraction measurement using a CuK? line; and when a diffraction intensity at the peak of 2?=29.58°±0.50° is regarded as IA and a diffraction intensity at a peak of 2?=27.33°±0.50° is regarded as IB, a value of IB/IA is less than 0.50, and M2 contains at least P and Si.
    Type: Application
    Filed: February 5, 2013
    Publication date: February 5, 2015
    Inventors: Ryoji Kanno, Masaaki Hirayama, Yuki Kato, Takamasa Otomo, Mitsuru Sakano
  • Publication number: 20150017548
    Abstract: The main object of the present invention is to provide a sulfide solid electrolyte material having favorable ion conductivity and high stability against moisture. The present invention solves the above-mentioned problem by providing a sulfide solid electrolyte material comprising an M1 element (such as Li element), an M2 element (such as Ge element, Sn element and P element) and a S element, and having a peak at a position of 2?=29.58°±0.50° in X-ray diffraction measurement using a CuK? ray, characterized in that when a diffraction intensity at the above-mentioned peak of 2?=29.58°±0.50° is regarded as IA and a diffraction intensity at a peak of 2?=27.33°±0.50° is regarded as IB, a value of IB/IA is less than 0.50, and the M2 contains at least P and Sn.
    Type: Application
    Filed: February 5, 2013
    Publication date: January 15, 2015
    Inventors: Yuki Kato, Takamasa Otomo, Mitsuru Sakano
  • Publication number: 20150004775
    Abstract: Disclosed is a method for preparing a semiconductor nanocrystal, comprising: forming a reaction mixture comprising injecting one or more first semiconductor nanocrystal precursors including one or more Group V elements and one or more Group VI elements into a mixture including one or more second semiconductor nanocrystal precursors including one or more Group II elements and one or more Group III elements at a first temperature; and reacting the first and second semiconductor nanocrystal precursors in the reaction mixture at a second temperature for a period time sufficient to form a semiconductor nanocrystal core comprising at least a portion of the one or more Group II elements, one or more Group III elements, one or more Group V elements, and one or more Group VI elements included in the first and second semiconductor nanocrystal precursors, wherein the second temperature is greater than the first temperature.
    Type: Application
    Filed: June 4, 2014
    Publication date: January 1, 2015
    Inventors: DIYUN HUANG, JONATHAN S. STECKEL
  • Publication number: 20140315103
    Abstract: A solid electrolyte including as constituent components, lithium, phosphorous and sulfur; wherein, in the 31P-NMR, the solid electrolyte has a peak (first peak) in a region of 81.0 ppm or more and 88.0 ppm or less, the solid electrolyte does not have a peak in regions other than the region of 81.0 ppm or more and 88.0 ppm or less, or even if it has a peak in other regions than the region of 81.0 ppm or more and 88.0 ppm or less, the peak intensity thereof relative to the first peak is 0.5 or less, and the solid electrolyte has an ionic conductivity of 5×10?4 S/cm or more.
    Type: Application
    Filed: November 29, 2012
    Publication date: October 23, 2014
    Applicant: IDEMITSU KOSAN CO., LTD.
    Inventor: Hiroyuki Higuchi
  • Publication number: 20140272602
    Abstract: A solid-state lithium ion conductor includes: Li, P, and S; and at least one metal element selected from Sc, Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Zr, Hf, V, Nb, Ta, Cr, Mo, W, Mn, Re, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt, Zn, Cd, and Hg.
    Type: Application
    Filed: March 18, 2014
    Publication date: September 18, 2014
    Applicant: TDK CORPORATION
    Inventors: Tokuhiko HANDA, Chieko SHIMIZU
  • Publication number: 20130164632
    Abstract: An object of the present invention is to provide a sulfide solid electrolyte glass producing a tiny amount of hydrogen sulfide. The present invention attains the above-mentioned object by providing a sulfide solid electrolyte glass including Li3PS4, characterized in that Li4P2S7 is not detected by 31P NMR measurement and the content of Li2S as determined by XPS measurement is 3% by mol or less.
    Type: Application
    Filed: July 22, 2010
    Publication date: June 27, 2013
    Applicant: TOYOTA JIDOSHA KABUSHIKI KAISHA
    Inventors: Yuki Kato, Koji Kawamoto, Shigenori Hama, Takamasa Otomo
  • Patent number: 8367069
    Abstract: The invention provides a polypeptide having a sequence of amino acids consisting of IXDFGLAKL (SEQ ID NO: 1), as well as a nucleic acid encoding the polypeptide, vector comprising the nucleic acid, cell comprising the vector, and compositions thereof. The invention also provides a method of inducing a T-cell response in a patient with epithelial cancer, and a method inhibiting epithelial cancer, wherein the methods comprise administering the composition of the invention. The invention further provides a method of stimulating a cell with the inventive polypeptide and a cell so stimulated.
    Type: Grant
    Filed: December 2, 2010
    Date of Patent: February 5, 2013
    Assignee: University of Pittsburgh—of the Commonwealth System of Higher Education
    Inventors: Robert L. Ferris, Pedro Andrade, Andres Lopez-Albaitero
  • Patent number: 8182779
    Abstract: The disclosure provides a process for removing phosphorus-containing colloids and their precursors from an iron chloride solution comprising: (a) heating the iron chloride solution comprising impurities selected from the group consisting of phosphorus-containing colloid, phosphorus-containing colloid precursor, and mixtures thereof, at a temperature of about 100° C. to about 300° C., at least autogenous pressure and for a period of time sufficient to transform the impurities into a filterable solid; and (b) separating the solid from the iron chloride solution. In one embodiment, the iron chloride solution is a byproduct of the chloride process for making titanium dioxide.
    Type: Grant
    Filed: April 14, 2010
    Date of Patent: May 22, 2012
    Assignee: E. I. du Pont de Nemours and Company
    Inventor: Peter Hill
  • Patent number: 8053075
    Abstract: The invention relates to a crystalline ion-conducting material made of LiMPO4 nanoparticles, wherein M is selected from Cr, Mn, Co, Fe and Ni, in addition to mixtures thereof and the nanoparticles have an essentially flat prismatic shape. The invention also relates to a method for producing said type of crystalline ion-conducting material which consists of the following steps: a precursor component is produced in a solution front a lithium compound of a component containing metal ions M and a phosphate compound, the precursor compound is subsequently precipitated from the solution and, optionally, a suspension of the precursor compound is formed, the precursor compound and/or the suspension is dispersed and/or ground, and the precursor compound and/or the suspension is converted under hydrothermal conditions and subsequently, the crystalline material is extracted.
    Type: Grant
    Filed: March 9, 2006
    Date of Patent: November 8, 2011
    Assignee: Sued-Chemie AG
    Inventors: Norbert Schall, Gerhard Nuspl, Christian Vogler, Lucia Wimmer, Max Eisgruber
  • Patent number: 8012631
    Abstract: A solid electrolyte including a lithium (Li) element, a phosphorus (P) element and a sulfur (S) element, the 31P MAS NMR spectrum thereof having a peak ascribed to a crystal at 90.9±0.4 ppm and 86.5±0.4 ppm; and the ratio (xc) of the crystal in the solid electrolyte being from 60 mol % to 100 mol %.
    Type: Grant
    Filed: November 28, 2006
    Date of Patent: September 6, 2011
    Assignee: Idemitsu Kosan Co., Ltd
    Inventors: Yoshikatsu Seino, Masaru Nakagawa, Minoru Senga, Masatoshi Shibata
  • Patent number: 7960059
    Abstract: Methods for producing an electrode active material precursor, comprising; a) producing a mixture comprising particles of lithium hydrogen phosphate, having a first average particle size, and a metal hydroxide, having a second average particle size; and b) grinding said mixture in a jet mill for a period of time suitable to produce a generally homogeneous mixture of particles having a third average size smaller than said first average size. The precursor may be used as a starting material for making electrode active materials for use in a battery, comprising lithium, a transition metal, and phosphate or a similar anion.
    Type: Grant
    Filed: March 12, 2008
    Date of Patent: June 14, 2011
    Assignee: Valence Technology, Inc.
    Inventors: George Adamson, Jeremy Barker, Allan Dirilo, Titus Faulkner, M. Yazid Saidi, Jeffrey Swoyer
  • Publication number: 20100290969
    Abstract: The invention relates to lithium argyrodite of the general formula (I): Li+(12-n-x)Bn+X2?6-xY?x(I), where Bn+ is selected from the group P, As, Ge, Ga, Sb, Si, Sn, Al, In, Ti, V, Nb, and Ta, X2? is selected from the group S, Se, and Te, Y? is selected from the group Cl, Br, I, F, CN, OCN, SCN, N3, and where 0?x?2, and a method for the production thereof, and the use thereof as a lithium-ion electrolyte in primary and secondary electrochemical energy storage.
    Type: Application
    Filed: October 7, 2008
    Publication date: November 18, 2010
    Applicant: Universitat Siegen
    Inventors: Hans-Jörg Deiseroth, Shiao-Tong Kong, Marc Schlosser, Christof Reiner
  • Publication number: 20100202950
    Abstract: Efficient heterogeneous catalysts were prepared by derivatization and palladation of commercially available chloromethylated polystyrene, and derivatization and palladation of functionalized silica gels with benzylchloride pendant groups. Both polymer based and silica based heterogeneous catalysts exhibited catalytic activity. Catalytic activity was studied using methanolysis of commercially available P?S pesticides. Catalytic activity of catalysts immobilized on silica gel was greater than catalyst immobilized on polymer.
    Type: Application
    Filed: November 4, 2009
    Publication date: August 12, 2010
    Inventors: Alexei A. Neverov, R. Stanley Brown, Mark F. Mohamed
  • Publication number: 20090291499
    Abstract: A method of producing a biological tissue-reinforcing material, which is applicable to a site required to be reinforced and which enables to improve the working properties for transplantation, comprising the step S1 of coprecipitating ammonium hydrogen phosphate with calcium nitrate in the presence of sulfuric acid.
    Type: Application
    Filed: July 14, 2006
    Publication date: November 26, 2009
    Applicants: OLYMPUS CORPORATION
    Inventors: Toshie Tsuchiya, Masato Tamai, Yasuharu Hakamatsuka, Tomoaki Tamura
  • Patent number: 7150943
    Abstract: A sulfide-based inorganic solid electrolyte that suppresses the reaction between silicon sulfide and metallic lithium even when the electrolyte is in contact with metallic lithium, a method of forming the electrolyte, and a lithium battery's member and lithium secondary battery both incorporating the electrolyte. The electrolyte comprises Li, P, and S without containing Si. It is desirable that the oxygen content vary gradually from the electrolyte to the lithium-containing material at the boundary zone between the two members when analyzed by using an XPS having an analyzing chamber capable of maintaining a super-high vacuum less than 1.33×10?9 h Pa and that the oxygen-containing layer on the surface of the lithium-containing material be removed nearly completely. The electrolyte can be formed such that at least part of the forming step is performed concurrently with the step for etching the surface of the substrate by irradiating the surface with inert-gas ions.
    Type: Grant
    Filed: February 22, 2002
    Date of Patent: December 19, 2006
    Assignee: Sumitomo Electric Industries, Ltd.
    Inventors: Hirokazu Kugai, Nobuhiro Ota
  • Patent number: 6821677
    Abstract: A nonaqueous electrolyte battery includes a positive electrode containing a positive electrode active material, a negative electrode containing a sulfide containing Fe, and a nonaqueous electrolyte including a nonaqueous solvent and a solute dissolved in the nonaqueous solvent, the nonaqueous solvent containing a first solvent containing a cyclic carbonate and a second solvent containing a chain carbonate, wherein the content of the first solvent in the nonaqueous solvent falls within a range of between 4.8 and 29% by volume and the content of the second solvent in the nonaqueous solvent falls within a range of between 71 and 95.2% by volume.
    Type: Grant
    Filed: March 29, 2002
    Date of Patent: November 23, 2004
    Assignee: Kabushiki Kaisha Toshiba
    Inventors: Hiroki Inagaki, Norio Takami
  • Publication number: 20040005504
    Abstract: A sulfide-based inorganic solid electrolyte that suppresses the reaction between silicon sulfide and metallic lithium even when the electrolyte is in contact with metallic lithium, a method of forming the electrolyte, and a lithium battery's member and lithium secondary battery both incorporating the electrolyte. The electrolyte comprises Li, P, and S without containing Si. It is desirable that the oxygen content vary gradually from the electrolyte to the lithium-containing material at the boundary zone between the two members when analyzed by using an XPS having an analyzing chamber capable of maintaining a super-high vacuum less than 1.33×10−9 h Pa and that the oxygen-containing layer on the surface of the lithium-containing material be removed nearly completely. The electrolyte can be formed such that at least part of the forming step is performed concurrently with the step for etching the surface of the substrate by irradiating the surface with inert-gas ions.
    Type: Application
    Filed: March 19, 2003
    Publication date: January 8, 2004
    Inventors: Hirokazu Kugai, Nobuhiro Ota
  • Patent number: 6613926
    Abstract: Novel compounds are provided in the form of nucleoside pyrophosphate and triphosphate analogs. In these analogs, the pyrophosphate or triphosphate group is replaced with a moiety that is isosterically and electronically identical thereto, but is hydrolytically and enzymatically more stable. The compounds are useful as therapeutic agents, e.g., as antiviral agents, anticancer agents, metabolic moderators and the like. The invention also provides pharmaceutical compositions containing a compound of the invention as an active agent, and in addition provides methods of treating disease, including viral infections, cancer, bacterial infections, inflammatory and/or autoimmune diseases, and the like, by administering a compound of the invention to a patient in need of such treatment.
    Type: Grant
    Filed: November 1, 2000
    Date of Patent: September 2, 2003
    Assignee: SRI International
    Inventors: Jeffrey C. Bottaro, Robert J. Schmitt, Mark A. Petrie, Paul E. Penwell
  • Patent number: 6328929
    Abstract: A method of delivering disinfectant in an absorbent substrate. A first step involves intermixing a first reactant chemical with a first ink. A second step involves intermixing a second reactant chemical with a second ink. A third step involves printing a first pattern on an absorbent substrate with the first ink. A fourth step involves printing a second pattern on the absorbent substrate with the second ink. The second pattern is positioned in close proximity to the first pattern, such that when the first pattern and second pattern are exposed to water an intermixing of the first reactant chemical and the second reactant chemical occurs to produce an aerosol disinfectant.
    Type: Grant
    Filed: August 16, 1999
    Date of Patent: December 11, 2001
    Inventor: Kenneth Reay Code
  • Patent number: 6251350
    Abstract: The present invention relates to an improved process for the preparation of thiophosphoryl chloride which is useful as an intermediate for the synthesis of insecticidally active compounds. The improvement comprises the presence in the reaction mixture of a catalytic amount of a nitroxide free radical of the following general formula: wherein R1, R2, R3 and R4 represent an alkyl group.
    Type: Grant
    Filed: June 21, 1999
    Date of Patent: June 26, 2001
    Assignee: Bayer Corporation
    Inventors: Jacqueline M. Applegate, Peter E. Newallis, Vidyanatha A. Prasad
  • Patent number: 6019955
    Abstract: An nickel hydroxide positive electrode active material which can be made by an ultrasonic precipitation method. The nickel hydroxide active material is characterized by the composition: ##EQU1## where x, the number of water ligands surrounding each Ni cation, is between 0.05 and 0.4 and y is the charge on the anions.
    Type: Grant
    Filed: March 8, 1996
    Date of Patent: February 1, 2000
    Assignee: Energy Conversion Devices, Inc.
    Inventors: Stanford R. Ovshinsky, Rosa T. Young, Liwei Xu, Suresh Kumar
  • Patent number: 6004898
    Abstract: The present invention is directed to a catalyst composition comprising a non-zeolitic molecular sieve and one or more alkaline earth metals selected from the group consisting of strontium, calcium, barium, and mixtures thereof, wherein said non-zeolitic molecular sieve has a pore diameter size of less than about 5 Angstroms.
    Type: Grant
    Filed: September 15, 1998
    Date of Patent: December 21, 1999
    Assignee: Exxon Chemicals Patent Inc.
    Inventor: Hsiang-ning Sun
  • Patent number: 5855809
    Abstract: This invention relates generally to inorganic ionic liquids which function as electrolytes and do not crystallize at ambient temperature. More specifically, this invention is directed to quasi-salt inorganic ionic liquids which comprise the reaction product of a strong Lewis acid with an inorganic halide-donating molecule. This invention is further directed to quasi-salt inorganic ionic liquid mixtures which comprise combinations of electrolyte additives and quasi-salt inorganic ionic liquids. These quasi-salt inorganic ionic liquid mixtures are useful electrolytes.
    Type: Grant
    Filed: November 12, 1996
    Date of Patent: January 5, 1999
    Assignee: Arizona Board Of Regents
    Inventors: Charles Austen Angell, Sheng-Shui Zhang, Kang Xu
  • Patent number: 5824433
    Abstract: This invention relates generally to electrolyte solvents for use in liquid or rubbery polymer electrolyte solutions as are used, for example, in electrochemical devices. More specifically, this invention relates to sulfonyl/phospho-compound electrolyte solvents and sulfonyl/phospho-compound electrolyte solutions incorporating such solvents.
    Type: Grant
    Filed: November 12, 1996
    Date of Patent: October 20, 1998
    Assignee: Arizona Board of Regents
    Inventors: Charles Austen Angell, Sheng-Shui Zhang, Kang Xu
  • Patent number: 5663402
    Abstract: There is disclosed a novel process for preparing products of the reaction of elemental phosphorus and elemental sulfur under reaction conditions wherein the phosphorus and sulfur are combined in a pre-mix at temperatures below the reaction temperature. The pre-mix may contain a diluent which is preferably the product of the reaction. Phosphorus pentasulfide can be prepared by heating the pre-mix to reaction temperatures wherein lower exotherm temperatures and reduced vibration are observed. Organophosphorus and thionated products can be prepared by the reaction of elemental sulfur and elemental phosphorus together with an organic compound wherein the ratio of phosphorus and sulfur generally corresponding to P.sub.2 S.sub.5. The process obviates the need for separately preparing phosphorus pentasulfide to prepare thiohated and organophosphorus compounds.
    Type: Grant
    Filed: March 27, 1995
    Date of Patent: September 2, 1997
    Assignee: G.D. Searle & Company
    Inventors: Edward J. Griffith, Toan M. Ngo
  • Patent number: 5543128
    Abstract: A method for treatment of process waste obtained from the synthesis of thiophene or its derivatives, which method produces phosphorus pentasulfide of sufficiently high purity for recycling in said synthesis process, as well as a residue material suited for use as a raw material for fertilizers. In the treatment method, the process waste is subjected to vacuum evaporation in a combination heating/evaporation reactor at 500.degree.-700.degree. C. and under a partial vacuum of 0.01-0.2 atm. To improve the yield of the evaporating phosphorus pentasulfide, sulfur is added to the process waste. The evaporating phosphorus pentasulfide is condensed, and when desired, pulverized. The usable, phosphorus- and potassium-containing evaporation residue is removed from the reactor and cooled for further use.
    Type: Grant
    Filed: April 12, 1994
    Date of Patent: August 6, 1996
    Assignee: Neste Oy
    Inventors: Heikki Tuovinen, Jorma Saari, Antti Roine, Hannu Holma, Matti Kalliokoski
  • Patent number: 5534349
    Abstract: Uniform, free-flowing, non-friable P.sub.2 S.sub.5 granules having a predetermined reactivity can be produced by accretion by spraying molten P.sub.2 S.sub.5 Sonto cascading, smaller solid particles of P.sub.2 S.sub.5. The process can be used to produce any reactivity grade of P.sub.2 S.sub.5 by adjusting processing conditions. The process can also be used to produce P.sub.2 S.sub.5 in a form suitable for bulk shipping.
    Type: Grant
    Filed: May 24, 1995
    Date of Patent: July 9, 1996
    Inventors: Jean M. Bacardi, Robert L. Camerer, Andrew M. Huey, Arthur R. Shirley, Jr.
  • Patent number: 5505885
    Abstract: Uniform, free-flowing, non-friable P.sub.2 S.sub.5 granules having a predetermined reactivity can be produced by accretion by spraying molten P.sub.2 S.sub.5 onto cascading, smaller solid particles of P.sub.2 S.sub.5. The process can be used to produce any reactivity grade of P.sub.2 S.sub.5 by adjusting processing conditions. The process can also be used to produce P.sub.2 S.sub.5 in a form suitable for bulk shipping.
    Type: Grant
    Filed: June 29, 1993
    Date of Patent: April 9, 1996
    Inventors: Jean M. Bacardi, Robert L. Camerer, Andrew M. Huey, Arthur R. Shirley, Jr.
  • Patent number: 5464601
    Abstract: There is disclosed a novel process for preparing products of the reaction of elemental phosphorus and elemental sulfur under reaction conditions wherein the phosphorus and sulfur are combined in a pre-mix at temperatures below the reaction temperature. The pre-mix may contain a diluent which is preferably the product of the reaction. Phosphorus pentasulfide can be prepared by heating the pre-mix to reaction temperatures wherein lower exotherm temperatures and reduced vibration are observed.
    Type: Grant
    Filed: March 29, 1994
    Date of Patent: November 7, 1995
    Assignee: Monsanto Company
    Inventors: Edward J. Griffith, Toan M. Ngo
  • Patent number: 5340557
    Abstract: .sup.32 P-Thiophosphates of the general formula: ##STR1## wherein n =1, 2 or 3 and each M, which may be the same or different, is H or a cation, are prepared by heating H.sub.3.sup.32 PO.sub.4 or a salt thereof with at least an equivalent amount of a thiophosphoryl halide and then treating the reaction product with an aqueous medium to hydrolyse the reaction product and form the .sup.32 P thiophosphate.
    Type: Grant
    Filed: August 25, 1993
    Date of Patent: August 23, 1994
    Assignee: British Technology Group Limited
    Inventors: Andrew M. Creighton, William A. Jeffery
  • Patent number: 5198202
    Abstract: The tetraphosphorus polysulfides of the formula P.sub.4 S.sub.x, wherein x is at least 3, especially tetraphosphorus decasulfide, P.sub.4 S.sub.10, are prepared by (a) establishing a continuously circulating closed loop of a liquid reaction mixture which comprises desired final product tetraphosphorus polysulfide, (b) continuously introducing liquid phosphorus and liquid sulfur into such continuously circulating reaction mixture and therein continuously reacting the liquid phosphorus with the liquid sulfur, and (c) continuously separating desired final product tetraphosphorus polysulfide, in gaseous state, from such continuously circulating reaction mixture.
    Type: Grant
    Filed: January 24, 1991
    Date of Patent: March 30, 1993
    Assignee: Atochem
    Inventors: Philippe Engel, Alain Courant
  • Patent number: 4732745
    Abstract: Phosphorus pentasulfide is made. To this end gaseous nitrogen is introduced into the pipes feeding a reactor with a phosphorus melt and sulfur melt and/or into the outlet pipe for the phosphorus pentasulfide melt, the nitrogen being admitted under a pressure lower than the static pressure exerted in the pipes by the quantity of melt upstream of the gas inlets.
    Type: Grant
    Filed: November 26, 1986
    Date of Patent: March 22, 1988
    Assignee: Hoechst Aktiengesellschaft
    Inventors: Herbert Diskowski, Heinz Stephan, Hermann Niermann
  • Patent number: 4579724
    Abstract: A low-temperature synthesis of M.sup.II PS.sub.3 (M preferably Fe, Co or Ni) comprises mixing M.sup.2+ cation with P.sub.2 S.sub.6.sup.4- anion; if insoluble, M.sup.II PS.sub.3 precipitates; otherwise, M.sup.2+ cation can be supplied off an M.sup.2+ -cation-exchange resin through which Na.sub.4 P.sub.2 S.sub.6 solution is trickled. The product is X-ray amorphous, and is brought to a desirable degree of partial order by heating at 350.degree. C. for 3 hours. In this form it can reversibly intercalate lithium and, mixed with binder and graphite, is a cathode for a lithium rechargeable cell.
    Type: Grant
    Filed: August 6, 1984
    Date of Patent: April 1, 1986
    Assignee: National Research Development Corporation
    Inventors: Peter J. S. Foot, Brian A. Nevett
  • Patent number: 4557914
    Abstract: In order to obtain substances that are optically transparent in the infrared range, usable in the manufacture of optical fibers or radiation emitters, a metal or metalloid chalcogenide other than an oxide is produced by a double-substitution reaction between a starting chalcogen compound--particularly a hydride such as H.sub.2 S, H.sub.2 Se or H.sub.2 Te--and a salt of the desired metal or metalloid, e.g. a chloride. The starting compound and the reactant salt preferably are vaporized at a temperature below the melting point of the resulting metal chalcogenide which thereupon precipitates in the reaction chamber.
    Type: Grant
    Filed: June 29, 1984
    Date of Patent: December 10, 1985
    Assignee: CSELT - Centro Studi e Laboratori Telecomunicazioni S.p.A.
    Inventor: Eros Modone
  • Patent number: 4518573
    Abstract: A dry differential flotation reagent for molybdenum-bearing ore is disclosed comprising from about 1 to about 30 percent by weight of NaSH, 0 to 20 percent by weight of NaOH, 60 to 90 percent by weight of a mixture of sodium thiophosphates comprising, as major components thereof, Na.sub.3 PS.sub.4, Na.sub.3 PS.sub.3 O, Na.sub.3 PS.sub.2 O.sub.2, and Na.sub.3 PO.sub.3 S, with Na.sub.3 PS.sub.4 further comprising from about 15 mole percent to about 70 mole percent of the phosphate mixture. The flotation reagent can be prepared by reacting P.sub.4 S.sub.10 with NaOH and NaSH in a molar ratio of about 1:16. When added to a flotation vessel containing molybdenum concentrate, the flotation reagent promotes suppression of lead and copper sulfides, even without the addition of sodium cyanide, to permit the improved recovery of molybdenum with a lower level of impurities.
    Type: Grant
    Filed: July 16, 1984
    Date of Patent: May 21, 1985
    Assignee: Occidental Chemical Corporation
    Inventors: John A. Peterson, Mohan S. Saran, Joseph S. Wisnouskas
  • Patent number: 4499327
    Abstract: The process for the production of light olefins from a feedstock comprising methanol, ethanol, dimethyl ether, diethyl ether or mixtures thereof comprising contacting said feedstock with a silicoaluminophosphate molecular sieve at effective process conditions to produce light olefins.
    Type: Grant
    Filed: October 4, 1982
    Date of Patent: February 12, 1985
    Assignee: Union Carbide Corporation
    Inventor: Steven W. Kaiser
  • Patent number: 4473538
    Abstract: The invention provides a process and an apparatus for removing molten phosphorus pentasulfide, via an overflow, from a reactor, wherein phosphorus is reacted with sulfur at temperatures higher than 300.degree. C.To this end, the reactor is supplied with phosphorus and sulfur from dosing vessels which are given the dimensions necessary (a) to receive the quantity of phosphorus and sulfur, respectively, which are required to produce phosphorus pentasulfide with a preselected quantitative ratio of P:S, (b) to provide a total filling volume corresponding to that of a P.sub.2 S.sub.5 -receiving tank. The quantity of the phosphorus and sulfur feed materials in the respective dosing vessels is in each case fully emptied into the reactor and a corresponding quantity of molten P.sub.2 S.sub.5 is simultaneously discharged directly from the reactor, via the overflow, into the respective P.sub.2 S.sub.5 -receiving tank, whose filling volume exactly corresponds, to that of the dosing vessels.
    Type: Grant
    Filed: April 29, 1983
    Date of Patent: September 25, 1984
    Assignee: Hoechst Aktiengesellschaft
    Inventors: Johannes Krause, Franz Mainzer, Gunter Reichert, Hermann Niermann
  • Patent number: 4439301
    Abstract: Photoelectrochemical cells employing chalcogenophosphate (MPX.sub.3) photoelectrodes are disclosed, where M is selected from the group of transition metal series of elements beginning with scandium (atomic number 21) through germanium (atomic number 32) yttrium (atomic number 39) through antimony (atomic number 51) and lanthanum (atomic number 57) through polonium (atomic number 84); P is phosphorus; and X is selected from the chalogenide series consisting of sulfur, selenium, and tellurium. These compounds have bandgaps in the desirable range of 2.0 eV to 2.2 eV for the photoelectrolysis of water and are stable when used as photoelectrodes for the same.
    Type: Grant
    Filed: October 7, 1982
    Date of Patent: March 27, 1984
    Assignee: The United States of America as represented by the Administrator of the National Aeronautics and Space Administration
    Inventors: Benjamin Reichman, Charles E. Byvik
  • Patent number: 4419104
    Abstract: Phosphorus pentasulfide of low reactivity is made by solidifying molten phosphorus pentasulfide on a cooling cylinder that delivers the solidified product at a temperature of 150.degree. to 220.degree. C., and that product is immediately introduced into a heat-insulated container and freed therein from its immanent or sensible heat by cooling at a rate of at most 30.degree. C. per hour without the expenditure of any energy to control the cooling.
    Type: Grant
    Filed: July 2, 1981
    Date of Patent: December 6, 1983
    Assignee: Hoechst Aktiengesellschaft
    Inventors: Hermann Niermann, Gunter Reichert, Hans Ebert, Friedrich Neumann
  • Patent number: 4396581
    Abstract: The invention relates to an apparatus for making P.sub.2 S.sub.5 comprised of a plurality of reactors connected by pipe structures to a collecting tank which is common to all of them. By means of partitions, the cooling tank is subdivided into a plurality of separate chambers. Outlet pipes open thereinto and terminate in collecting devices. The pipe structures running to the collecting tank are pivotably arranged above the various chambers and permit liquid P.sub.2 S.sub.5 to be introduced thereinto at will.
    Type: Grant
    Filed: December 14, 1981
    Date of Patent: August 2, 1983
    Assignee: Hoechst Aktiengesellschaft
    Inventors: Hans-Dieter Benscheidt, Friedrich Neumann, Gunter Reichert, Hermann Niermann
  • Patent number: 4386020
    Abstract: The present invention provides a process for the production of solid ion ductor materials (electrolytes) based on lithium or sodium compounds which stand in thermodynamic equilibrium with their alkali metal and have a high decomposition voltage, wherein two or more binary lithium or sodium compounds with an anion which is formed from one or more elements of the group consisting of nitrogen, phosphorus, arsenic, oxygen, sulphur, selenium, tellurium, hydrogen, fluorine, chlorine, bromine and iodine and which stand in thermodynamic equilibrium with their alkali metal are reacted together in such amounts and for such a period of time that a radiographically phase-pure product is formed.The present invention also provides ion conductor materials based on lithium or sodium compounds, which have the general formula:A.sub.3u+2v+w X.sub.u Y.sub.v Z.sub.
    Type: Grant
    Filed: May 1, 1980
    Date of Patent: May 31, 1983
    Assignee: Max Planck Gesellschaft zur Forderung der Wissenschaften E.V.
    Inventors: Peter Hartwig, Werner Weppner, Winfried Wichelhaus
  • Patent number: 4374706
    Abstract: Process for the purification of phosphorus pentasulphide by means of distillation under vacuum at a residual pressure of about 6 mmHg and carried out according to a "thermal profile" comprising, immediately before and immediately after the liquid-vapor-liquid double passage of state, two stationary stages wherein said pentasulphide is maintained in the liquid state at a temperature very close to the boiling temperature of the pentasulphide itself.
    Type: Grant
    Filed: March 2, 1981
    Date of Patent: February 22, 1983
    Assignee: Saffa S.p.A.
    Inventor: Pietro Molla
  • Patent number: 4301014
    Abstract: The process disclosed in this invention takes the waste solids, gases, and water from a phosphorus pentasulfide manufacturing facility and hydrolyzes the phosphorus pentasulfide by heating. The phosphorus portion is converted to a soluble phosphate and the sulfur portion to a mixture of sulfide, sulfite and sulfate. The soluble fraction is then treated with a calcium hydroxide solution precipitating the phosphate and sulfates which are removed. The gaseous portion of the hydrolysis is fed to a catalytic oxidizer which converts the sulfides to sulfur, which is removed and the gas, free of sulfur containing species, is exhausted to the atmosphere. The filtrate from the precipitation reaction can be recycled to the plant, or may be chlorinated and discharged.
    Type: Grant
    Filed: June 5, 1980
    Date of Patent: November 17, 1981
    Assignee: Hooker Chemicals & Plastics Corp.
    Inventors: Harry E. Buckholtz, Joseph J. Moritz, Joseph S. Wisnouskas
  • Patent number: 4267157
    Abstract: A process for producing relatively pure metal phosphorus trisulfides of the formula MPS.sub.3 wherein M is a metal selected from the group consisting of Mg, Ca, Sr, V, Mn, Fe, Co, Ni, Pd, Zn, Cd, Hg, Sn, Pb, Sm, Eu, Yb and mixtures thereof, said process comprising contacting in a reaction zone, phosphides of said metals of the formula M.sub.x P.sub.y, wherein the ratio of y/x ranges between 1/8 to 5/1, with one or more compounds of the formula PS.sub.z wherein z ranges from 1-3 and is preferably 2, said PS.sub.z being present in the reaction zone in an amount sufficient to exceed the amount of P and S stoichiometrically required to form the desired MPS.sub.3, at a temperature ranging from about 300.degree.-600.degree. C. and confined so as to maintain the PS.sub.z present in the reaction zone as a gas in equilibrium with its liquid for a time sufficient to produce said relatively pure metal phosphorus trisulfide.
    Type: Grant
    Filed: November 14, 1979
    Date of Patent: May 12, 1981
    Assignee: Exxon Research and Engineering Company
    Inventors: Edward T. Maas, Jr., John J. Steger
  • Patent number: 4248602
    Abstract: The invention provides a process wherein a mixture prepared from starting materials comprised of P.sub.2 S.sub.5 of high reactivity and low reactivity, respectively, is converted to phosphorus pentasulfide of predetermined reactivity lying between that of the high reactivity P.sub.2 S.sub.5 and that of the low reactivity P.sub.2 S.sub.5 starting materials. To this end, the starting materials are mixed in quantitative proportions which are selected in accordance with the respective reactivity of the starting materials and the resulting mixture is ground.
    Type: Grant
    Filed: August 15, 1979
    Date of Patent: February 3, 1981
    Assignee: Hoechst Aktiengesellschaft
    Inventors: Hermann Niermann, Gunter Reichert, Hans Ebert, Friedrich Neumann
  • Patent number: 4173621
    Abstract: The reactivity of phosphorus pentasulfide produced by reacting phosphorus and sulfur at a temperature higher than the melting point of phosphorus pentasulfide and allowing the resulting melt to cool and solidify on a cooling device is improved. To this end, liquid phosphorus pentasulfide is placed on, or introduced into, a cooling device; an upper liquid P.sub.2 S.sub.5 -layer portion A is separated immediately from a solidified lower P.sub.2 S.sub.5 -layer portion B which is in direct contact with the cooling surface area of the cooling device; the upper P.sub.2 S.sub.5 -layer portion A is recycled to a P.sub.2 S.sub.5 melt; the lower P.sub.2 S.sub.5 -layer portion B is removed from the cooling device and collected as final product; the reactivity of the collected P.sub.2 S.sub.5 -layer portion B is increased to the same extent as the quantitative ratio of the P.sub.2 S.sub.5 -layer portion A to the P.sub.2 S.sub.5 -layer portion B is increased.
    Type: Grant
    Filed: December 22, 1977
    Date of Patent: November 6, 1979
    Assignee: Hoechst Aktiengesellschaft
    Inventors: Johannes Krause, Gunter Reichert, Franz Mainzer, Hermann Niermann
  • Patent number: 4097583
    Abstract: Production of phosphorus pentasulfide from phosphorus and sulfur at elevated temperature in a reactor of which the walls are in heat exchange with a substance kept at the temperature necessary for cooling or heating reaction mixture.The heat exchange in the bottom portion of the reactor is more particularly effected with the use of a system functioning separately and independently from the heat exchange system surrounding the lateral walls of the reactor.
    Type: Grant
    Filed: March 14, 1977
    Date of Patent: June 27, 1978
    Assignee: Hoechst Aktiengesellschaft
    Inventors: Hermann Niermann, Franz Mainzer