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公开(公告)号：US06514474B1
公开(公告)日：2003-02-04
申请号：US09600231
申请日：2000-09-05
IPC分类号： C01B2510
CPC分类号： C01D15/005
摘要： A method of purifying lithium hexafluorosphate 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 to lithium hexafluorophosphate with generated phosphor pentafluoride.
摘要翻译： 提供了一种纯化六氟磷酸锂的方法，其可以将用作锂二次电池电解质，有机合成介质等的六氟磷酸锂纯化至极高纯度。 含有氟化氢，氟化锂等有害杂质的六氟磷酸锂通过加入磷酸盐进行纯化。 在磷酸盐和氟化氢存在下进行纯化，其量等于或优于反应它们的当量，然后通过用产生的五氟化磷将氟化锂转化为六氟磷酸锂。
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公开(公告)号：US06309619B1
公开(公告)日：2001-10-30
申请号：US09353194
申请日：1999-07-14
IPC分类号： C01B2510
CPC分类号： C08G79/025
摘要： A method for making poly(dichlorophosphazene) using solid state reactants is disclosed and described. The present invention improves upon previous methods by removing the need for chlorinated hydrocarbon solvents, eliminating complicated equipment and simplifying the overall process by providing a “single pot” two step reaction sequence. This may be accomplished by the condensation reaction of raw materials in the melt phase of the reactants and in the absence of an environmentally damaging solvent.
摘要翻译： 公开并描述了使用固态反应物制备聚（二氯膦腈）的方法。 通过提供“单锅”两步反应顺序，本发明通过去除对氯化烃溶剂的需要，消除复杂的设备和简化整个过程来改进先前的方法。 这可以通过原料在反应物的熔融相中和在没有环境破坏性溶剂的情况下的缩合反应来实现。
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公开(公告)号：US06251350B1
公开(公告)日：2001-06-26
申请号：US09337088
申请日：1999-06-21
IPC分类号： C01B2510
CPC分类号： C01B25/10
摘要： 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.
摘要翻译： 本发明涉及一种制备硫代磷酰氯的改进方法，其可用作合成杀虫活性化合物的中间体。 改进包括在反应混合物中存在催化量的以下通式的氮氧自由基：其中R1，R2，R3和R4表示烷基。
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公开(公告)号：US06500399B1
公开(公告)日：2002-12-31
申请号：US09763188
申请日：2001-03-23
申请人： Philippe Joubert
发明人： Philippe Joubert
IPC分类号： C01B2510
CPC分类号： C01D15/005
摘要： 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.
摘要翻译： 该方法包括通过在液态二氧化硫（SO2）中使LiF与PF5反应来制备LiPF6。相对于反应的LiF，产率为99.5％的LiPF 6根据测定法具有大于或等于99.90％的纯度 执行。
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公开(公告)号：US06322764B1
公开(公告)日：2001-11-27
申请号：US09375791
申请日：1999-08-17
申请人： W. Novis Smith , Joel McCloskey
发明人： W. Novis Smith , Joel McCloskey
IPC分类号： C01B2510
CPC分类号： C01B25/10
摘要： A process for the preparation of anhydrous high purity phosphorus pentafluoride in high yield. The process uses an excess of hydrogen fluoride in a reaction with a phosphoric acid to form hexafluorophosphoric acid followed by reaction with a sulfur based acid reactant in a reaction medium containing an excess of hydrogen fluoride.
摘要翻译： 一种以高产率制备无水高纯度五氟化磷的方法。 该方法在与磷酸反应中使用过量的氟化氢以形成六氟磷酸，随后在含有过量氟化氢的反应介质中与硫酸反应物反应。
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公开(公告)号：US06645451B1
公开(公告)日：2003-11-11
申请号：US08876529
申请日：1997-06-16
申请人： Alf Schulz , Dirk Seffer , Matthias Rieland , Werner Rudolph
发明人： Alf Schulz , Dirk Seffer , Matthias Rieland , Werner Rudolph
IPC分类号： C01B2510
CPC分类号： C01B25/10
摘要： The preparation of phosphorus pentafluoride and arsenic pentafluoride by reacting corresponding trihalides with elemental chlorine, bromine or iodine and also with hydrogen fluoride.
摘要翻译： 通过使相应的三卤化物与元素氯，溴或碘反应，并与氟化氢反应制备五氟化磷和五氟化砷。
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公开(公告)号：US06409978B1
公开(公告)日：2002-06-25
申请号：US09615212
申请日：2000-07-13
IPC分类号： C01B2510
摘要： A process for removing impurities contained in the crystal lattice of minerals, comprising the steps of forming a mixture of a mineral capable of structurally reorganizing its crystal lattice which contains an impurity in its crystal lattice and a halogen anion, and water; heating the mixture to the mineral's structural reorganization transition temperature; holding the mixture at the structural reorganization transition temperature for a sufficient period of time to allow the impurity to freely migrate from the lattice to combine with the halogen anion; and separating the combined impurity and anion from the mixture to render the mineral essentially free of the impurity. The process is applicable to numerous minerals and impurities, but is especially useful to remove arsenic from fluorspar. Numerous halogen anions can be employed, such as chlorides, fluorides, bromides and iodides, but the preferred halogen anion is a metal chloride such as calcium chloride. Various matrix-forming additives may also be employed with the mixture to provide a receptor which immobilizes the impurity. Preferred additives are silicates, added in the form of bentonite, or other clays as well as organic compounds such as lignosulfonates, starches and starch hydrolyzates.
摘要翻译： 一种去除矿物晶格中杂质的方法，包括以下步骤：形成能够结构上重组其晶格中含有杂质的晶格和卤素阴离子的矿物和水的混合物; 将混合物加热至矿物的结构重组转变温度; 将混合物在结构重组转变温度下保持足够的时间以允许杂质从晶格自由迁移以与卤素阴离子结合; 并从混合物中分离出杂质和阴离子，使矿物基本上不含杂质。 该方法适用于许多矿物质和杂质，但特别适用于从萤石中除去砷。 可以使用许多卤素阴离子，例如氯化物，氟化物，溴化物和碘化物，但优选的卤素阴离子是氯化钙等金属氯化物。 也可以在混合物中使用各种基质形成添加剂以提供固定杂质的受体。 优选的添加剂是以膨润土或其它粘土形式加入的硅酸盐，以及有机化合物如木质素磺酸盐，淀粉和淀粉水解产物。
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公开(公告)号：US06387340B1
公开(公告)日：2002-05-14
申请号：US09475074
申请日：1999-12-29
申请人： Doo-Chan Na , Byung-Won Woo , Soon-Hong Park , Jun-Ho Lee
发明人： Doo-Chan Na , Byung-Won Woo , Soon-Hong Park , Jun-Ho Lee
IPC分类号： C01B2510
CPC分类号： H01M10/0525 , C01D15/005 , H01M10/0568
摘要： A method of preparing lithium hexafluoro phosphate (LiPF6) using phosphorous pentachloride (PCl5), lithium chloride (LiCl), and hydrogen fluoride (HF) as raw materials. The method includes the steps of: (a) reacting the phosphorous pentafluoride with the hydrogen fluoride to prepare phosphorous pentafluoride (PF5), and (b) reacting the phosphorous pentafluoride with the lithium chloride in a hydrogen fluoride to prepare the lithium hexafluoro phosphate. Also, in this method, anhydrous hydrogen fluoride, from which moisture was removed by treating with F2 gas, is used in the steps (a) and (b), and the step (b) further comprises contacting the reaction system of the step (b) with F2 gas. Accordingly, as the method adopts relatively cheap raw materials, such as PCl5, LiCl and the like, while a highly pure F2 obtained by an electrolysis is used in the reaction system, it has an advantage in that it enables lithium hexafluoro phosphate (LiPF6) to be prepared at a high yield and purity.
摘要翻译： 以五氯化磷（PCl5），氯化锂（LiCl）和氟化氢（HF）为原料制备六氟磷酸锂（LiPF 6）的方法。 该方法包括以下步骤：（a）使五氟化磷与氟化氢反应制备五氟化磷（PF5），和（b）使氟化氢中的五氟化磷与氯化锂反应以制备六氟磷酸锂。 此外，在该方法中，在步骤（a）和（b）中使用通过用F2气体处理除去水分的无水氟化氢，并且步骤（b）还包括使步骤 b）用F2气。 因此，由于该方法采用比较便宜的原料，例如PCl5，LiCl等，而在反应体系中使用通过电解获得的高纯度的F2，其优点在于能够使六氟磷酸锂（LiPF 6） 以高产率和纯度制备。
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9.发明授权Solid state thermal method for the synthesis of lithium hexafluoro phosphate (LiPF)6 as battery electrolyte 失效用于合成锂六氟磷酸锂（LiPF）6的固态热法作为电池电解质公开(公告)号：US06824754B2
公开(公告)日：2004-11-30
申请号：US10095520
申请日：2002-03-13
IPC分类号： C01B2510
CPC分类号： C01D15/005
摘要： The present invention provides a method for the preparation of LiPF6 (lithium hexafluoro phosphate) wherein equimolar quantities of pure dry AR lithium source such as Li2O or Li2CO3 or LiNO3 is mixed with (very pure dry and AR samples) diammonium hydrogen phosphate in solid state.
摘要翻译： 本发明提供了制备LiPF 6（六氟磷酸锂）的方法，其中将等摩尔量的纯的干燥的AR锂源如Li 2 O或Li 2 CO 3或LiNO 3与固体状态的（非常纯的干燥和AR样品）的磷酸氢二铵混合。
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公开(公告)号：US06685904B1
公开(公告)日：2004-02-03
申请号：US09061754
申请日：1998-04-16
IPC分类号： C01B2510
CPC分类号： C01B25/10
摘要： Disclosed is a process for producing phosphorous trichloride, phosphorous pentachloride, or phosphorous tribromide by reacting phosphine gas with chlorine gas or bromine gas, in a mixture with hydrogen gas. The phosphine is dried and the reaction is performed at a temperature up to about 250° C. The phosphorous trichloride or phosphorous tribromide product can be reacted with oxygen to form phosphorous oxychloride or phosphorous oxybromide, respectively.
摘要翻译： 公开了一种通过使磷氢气与氯气或溴气在氢气的混合物中反应生成三氯化磷，五氯化磷或三溴化磷的方法。 将磷化氢干燥，反应在高达约250℃的温度下进行。三氯化磷或三溴化磷产物可与氧反应，分别形成三氯氧化磷或三溴氧化磷。
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