序号 专利名 申请号 申请日 公开(公告)号 公开(公告)日 发明人
81 Method for Producing a Lithium Hexafluorophosphate Concentrated Liquid US13703588 2011-08-15 US20130143112A1 2013-06-06 Meguru Oe; Keiji Sato; Mitsuya Ohashi; Toshinori Mitsui
Disclosed is a method for forming lithium hexafluorophosphate by reacting together phosphorus trichloride, chlorine and lithium chloride in a nonaqueous organic solvent and then making the reaction product formed in the solvent react with hydrogen fluoride. This method is characterized by that a lithium hexafluorophosphate concentrated liquid is obtained by conducting a filtration after making the reaction product formed in the solvent react with hydrogen fluoride and then subjecting the filtrate to a concentration by degassing. By this method, it is possible to easily produce a high-purity, lithium hexafluorophosphate concentrated liquid at a low cost.
82 Method for Producing Electrolyte Solution for Lithium Ion Battery, and Lithium Ion Battery Using the Electrolyte Solution US13697471 2011-04-20 US20130071760A1 2013-03-21 Meguru Oe; Keiji Sato
Disclosed is a method for producing a lithium ion battery electrolyte solution containing lithium hexafluorophosphate as an electrolyte and a lithium ion battery using the electrolyte solution. The electrolyte solution is produced by reacting lithium chloride with phosphorus trichloride and chlorine in a non-aqueous organic solvent, reacting a reaction product generated in the solvent with hydrogen fluoride, reacting unreacted remaining hydrogen fluoride with lithium chloride, and then, separating the resulting reaction solution by filtration into a filtrate and a solid residue. The filtrate is obtained as the lithium ion battery electrolyte solution. The solid product is further reacted with phosphorous trichloride and chlorine in a non-aqueous organic solvent. The reaction product generated in the solvent is reacted with hydrogen fluoride, followed by reacting unreacted remaining hydrogen fluoride with lithium chloride. It is possible to accomplish reduction in production cost with the reuse of the reaction residue as production raw material.
83 METHODS AND APPARATUSES FOR PURIFYING PHOSPHORUS PENTAFLUORIDE US13484536 2012-05-31 US20130004402A1 2013-01-03 Robert A. Smith; Daniel J. Brenner; Matthew H. Luly; Haridasan K. Nair; Bernard Pointner
Embodiments of methods and apparatuses for purifying phosphorus pentafluoride are provided. The method comprises the step of contacting a feed stream comprising phosphorus pentafluoride and impurities with anhydrous hydrogen fluoride. The anhydrous hydrogen fluoride reduces the impurities from the feed stream to form an impurity-depleted phosphorus pentafluoride effluent.
84 Method for producing electrolyte solution for lithium ion battery and battery using same US11911901 2006-04-10 US08097360B2 2012-01-17 Meguru Oe; Keiji Sato; Hiroaki Sakaguchi
A method for producing an electrolyte solution for a lithium ion battery involving reacting a lithium halide selected from the group consisting of lithium fluoride, lithium chloride, lithium bromide, lithium iodide and a mixture of at least two of these, with phosphorus pentachloride and hydrogen fluoride in a nonaqueous organic solvent, thereby producing lithium hexafluorophosphate as an electrolyte of the electrolyte solution.
85 AZEOTROPE-LIKE COMPOSITION OF PF5 AND HF US13097836 2011-04-29 US20120003138A1 2012-01-05 Ryan J. Hulse; Rajat Subhra Basu; Matthew H. Luly
Provided are azeotropic and azeotrope-like compositions of PF5 and HF, and methods of making such compositions. Such azeotropic and azeotrope-like compositions can be used, for example, in processes for producing LiPF6.
86 MANUFACTURING METHOD OF HEXAFLUOROPHOSPHATE US12525900 2008-02-05 US20100317511A1 2010-12-16 Masahide Waki; Kazuhiro Miyamoto; Kenji Aoki
In the manufacturing method of hexafluorophosphate (MPF6: M=Li, Na, K, Rb, Cs, NH4, and Ag) of the present invention, at least a HxPOyFz aqueous solution, a hydrofluoric acid aqueous solution, and MF.r (HF) are used as raw materials (wherein, r≧0, 0≦x≦3, 0≦y≦4, and 0≦z≦6). According to the above description, a manufacturing method of hexafluorophosphate can be provided which is capable of manufacturing hexafluorophosphate (GPF6: G=Li, Na, K, Rb, Cs, NH4, and Ag) at a low cost in which the raw materials can be easily obtained, the control of the reaction is possible, and the workability is excellent.
87 METHOD FOR PRODUCING ELECTROLYTE SOLUTION FOR LITHIUM ION BATTERY AND LITHIUM ION BATTERY USING SAME US12096147 2006-11-07 US20090311610A1 2009-12-17 Keiji Sato; Meguru Oe
There is provided a method for producing an electrolyte solution for lithium ion batteries, in which lithium hexafluorophosphate is used as an electrolyte, comprising the steps of (a) reacting phosphorus trichloride, chlorine and lithium chloride in a nonaqueous organic solvent; and (b) reacting a reaction product of the step (a) formed in the solvent, with hydrogen fluoride.
88 Method for producing lithium hexafluorophosphate US10149266 2000-12-11 US06955795B2 2005-10-18 Hirohisa Kikuyama; Toshirou Fukudome; Masahide Waki; Tomoyuki Deguchi
In order to provide a method for producing lithium hexafluorophosphate capable of producing lithium hexafluorophosphate of a higher purity than in the related art without the necessity for after-treatment for removal of impurities, a method is characterized by filtering lithium hexafluorophosphate coexisting with a solvent and then carrying out after-filtering drying in a gas atmosphere containing PF5.
89 Method of purifying lithium hexafluorophosphate US10336982 2003-01-06 US06884403B2 2005-04-26 Hirohisa Kikuyama; Toshirou Fukudome; Masahide Waki; Hirofumi Yazaki
A method of purifying lithium hexafluorophosphate that allows to purify lithium hexafluorophosphate, useful as lithium secondary cell electrolyte, organic synthesis medium or the like, to an extremely high purity is provided. Lithium hexafluorophosphate containing harmful impurities such as oxyfluoride, lithium fluoride is purified by adding phosphoric chloride. The purification is performed in the presence of phosphoric chloride and hydrogen fluoride of the quantity equal or superior to the equivalent amount for reacting them, and then by converting lithium fluoride lithium hexafluorophosphate with generated phosphor pentafluoride.
90 Method for producing lithium hexafluorophosphate US10149266 2002-09-25 US20030077215A1 2003-04-24 Hirohisa Kikuyama; Toshirou Fukudome; Masahide Waki; Tomoyuki Deguchi
In order to provide a method for producing lithium hexafluorophosphate capable of producing lithium hexafluorophosphate of a higher purity than in the related art without the necessity for after-treatment for removal of impurities, a method is characterized by filtering lithium hexafluorophosphate coexisting with a solvent and then carrying out after-filtering drying in a gas atmosphere containing PF5.
91 Method for making lithium hexafluorophosphate US09763188 2001-03-23 US06500399B1 2002-12-31 Philippe Joubert
The process consists in manufacturing LiPF6 by reacting LiF with PF5 in liquid sulphur dioxide (SO2). The LiPF6, obtained in a yield of 99.5% relative to the LiF reacted, has a purity of greater than or equal to 99.90% according to the assays carried out.
92 Electrolytic solution for lithium cell and method for producing same US09572887 2000-05-18 US06197205B1 2001-03-06 Shouichi Tsujioka; Mituo Takahata; Hisakazu Itou; Tadayuki Kawashima; Keiji Sato; Hiromi Sasaki; Sunao Yamamoto
The present invention relates to a method for producing an electrolytic solution containing a solute of lithium hexafluorophosphate. This method includes a step of (a) reacting lithium fluoride with phosphorus pentafluiride, in a nonaqueous organic solvent that is used for producing a lithium cell's electrolytic solution, thereby to form the lithium hexafluorophosphate dissolved in the solvent. According to this method, both yield and purity of the reaction product are sufficiently high, and the reaction can easily be managed. According to need, after the step (a), the nonaqueous organic solvent may be replaced with another nonaqueous organic solvent. The present invention further relates to a method for purifying an electrolytic solution used for a lithium cell. This electrolytic solution contains an acid impurity having at least one hydrogen atom in the molecule. this method includes steps of (a) adding at least one hydrogen-free halide selected from chlorides, bromides and iodides, to the electrolytic solution, such that the acid impurity is reacted with the at least one hydrogen-free halide, thereby to form at least one hydrogen halide selected from hydrogen chloride, hydrogen bromide and hydrogen iodide; and (b) purging the at least one hydrogen halide from the electrolytic solution to purify the electrolytic solution. The acid impurity concentration of the electrolytic solution is substantially reduced by this method.
93 Process for removing acids from lithium salt solutions US246531 1999-02-08 US6033808A 2000-03-07 Dennis J. Salmon; D. Wayne Barnette
The present invention provides a process for generating acid-free lithium salt solutions for lithium and lithium ion batteries and for preparing high purity lithium salts. The invention comprises removing acid species from lithium salt solutions such as lithium hexafluorophosphate solutions using weak base resins. The process does not require the addition of a base such as ammonia which when added to the electrolytic solution generally must be removed from the final product. Once the lithium salt has been treated by the weak base resin, the substantially acid-free lithium salt solution may be recovered from the weak base resin to provide a solution which may be used as an electrolytic solution or which may be used to prepare high purity lithium salts.
94 Preparation of lithium hexafluorophosphate solutions US172690 1993-12-23 US5378445A 1995-01-03 Dennis J. Salmon; D. Wayne Barnette; Rebecca A. Barnett
A process for preparing solutions of lithium hexafluorophosphate comprising reacting, under basic conditions, a lithium salt with a salt selected from sodium, potassium, ammonium, or organo ammonium hexafluorophosphate salt in a low boiling, non-protic organic solvent to produce a solution of lithium hexafluorophosphate and a precipitated sodium, potassium, ammonium, or organo ammonium salt containing the anion of the reactant lithium salt.
95 Tetraacetonitrilolithium hexafluorophosphate tetraacetonitrilolithium hexafluoroarsenate and method for the preparation thereof US3654330D 1970-05-01 US3654330A 1972-04-04 WIESBOECK ROBERT A
TETRAACETONITRILOLITHIUM HEXAFLUOROPHOSPHATE AND TETRAACETONITRILOLITHIUM HEXAFLUOROARSENATE, NEW COMPOUNDS, AND THEIR PREPARATION FROM LITHIUM FLUOIDE AND PF5 OR PREVIOUSLY PREPARED LIPF6 WITH EXCESS CH3CN, AND LIASF6 WITH EXCESS CH3CN, RESPECTIVELY, ARE DISCLOSED. TETRAACETONITRILOLITHIUM HEXAFLUOROPHOSPHATE AND TETRAACETONITRILOLITHIUM HEXAFLUOROARSENATE ARE USEFUL FOR THE PRODUCTION OF HIGH PURITY EXCEPTIONALLY ACTIVE LIPF6 AND LIASF6. THE PREPARATIONS OF THESE NEW COMPOSITIONS ARE ALSO DISCLOSED.
96 AZEOTROPE-LIKE COMPOSITION OF PF5 AND HF PCT/US2011041945 2011-06-27 WO2012012107A3 2012-04-12 HULSE RYAN J; BASU RAJAT SUBHRA; LULY MATTHEW H
Provided are azeotropic and azeotrope-like compositions of PF5 and HF, and methods of making such compositions. Such azeotropic and azeotrope-like compositions can be used, for example, in processes for producing LiPF6.
97 METHOD FOR PRODUCING A LITHIUM HEXAFLUOROPHOSPHATE CONCENTRATED LIQUID EP11818175.9 2011-08-15 EP2608307B1 2017-03-01 OE, Meguru; SATO, Keiji; OHASHI, Mitsuya; MITSUI, Toshinori
98 CHLORIDARMER ELEKTROLYT EP14716348.9 2014-04-10 EP2984038A2 2016-02-17 LINDER, Thomas; BOLL, Matthias; KUCKERT, Eberhard
The present invention relates to a method for producing low-chloride lithium hexafluorophosphate starting from lithium fluoride and phosphorus pentafluoride and the use thereof in an electrolyte.
99 Chloridarmer Elektrolyt EP13163517.9 2013-04-12 EP2789583A1 2014-10-15 Boll, Matthias; Kuckert, Eberhard; Linder, Thomas

Die vorliegende Erfindung betrifft ein Verfahren zur Herstellung von chloridarmem Lithiumhexafluorophosphat ausgehend von Lithiumfluorid und Phosphorpentafluorid und seine Verwendung in einem Elektrolyt.

100 MANUFACTURE OF MIXTURES COMPRISING LIPO2F2 AND LIPF6 EP12741336.7 2012-07-31 EP2744753A1 2014-06-25 GARCIA-JUAN, Placido; SCHULZ, Alf
Mixtures comprising LiPO 2F 2 and LiPF 6 both of which are electrolyte salts or additive for, i.a., Li ion batteries, are manufactured by the reaction of POF 3 and LiF. The mixtures can be extracted with suitable solvents to provide solutions containing LiPO 2F 2 and LiPF 6 which can be applied for the manufacture of Li ion batteries, Li-air batteries and Li-sulfur batteries. Equimolar mixtures comprising LiPO 2F 2 and LiPF 6 are also described, as well as a method for the manufacture of electrolyte compositions obtained by the extraction of equimolar mixtures comprising LiPO 2F 2 and LiPF 6.
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