Method of preparing di and poly chalcogenides of group VIIb by low
temperature precipitation from nonaqueous solution and small
crystallite size stoichiometric layered dichalcogenides of rhenium and
technetium
    41.
    发明授权
    Method of preparing di and poly chalcogenides of group VIIb by low temperature precipitation from nonaqueous solution and small crystallite size stoichiometric layered dichalcogenides of rhenium and technetium 失效
    通过从非水溶液和小微晶尺寸的低温沉淀制备Ⅶb族二元和多元硫族化合物的方法铼和锝的化学计量分层二硫属元素

    公开(公告)号:US4308171A

    公开(公告)日:1981-12-29

    申请号:US169425

    申请日:1980-07-16

    摘要: Finely divided, small particle (0.1 micron or less) small crystallite (about 50 A.times.100 A or less) chalcogenides of manganese, rhenium and technetium are described. These compositions are prepared by mixing the absence of an aqueous solvent, a manganese, rhenium or technetium salt with a source of chalcogenide yielding a precipitate. The manganese, rhenium or technetium salt and the source of chalcogen can be mixed either neat or in the presence of a nonaqueous aprotic solvent. The precipitate which results before removal of the anion salt is a finely divided product. In the case of rhenium dichalcogenide the product possesses a layered structure. The anion salt may be removed by any technique common to the art, pumping under vacuum being one such technique, washing with a suitable solvent being another.A method is described for the preparation of di- and poly-chalcogenides of the formula MX.sub.y wherein M is a metal selected from the group consisting of mangangese, rhenium and technetium, X is a chalcogen selected from the group consisting of sulfur, selenium, tellurium and mixtures thereof, and y is a number ranging from about 1.5 to about 4, preferably about 2, comprising the low temperature, nonaqueous precipitation of said MX.sub.y compounds from mixtures of the salts of said manganese, rhenium and technetium. Said precipitation occurs in the absence of aqueous solvents. The process of the instant invention permits the preparation of materials uncontaminated by water, oxygen or hydrolysis products.

    摘要翻译: 描述了细小的微粒(0.1微米或更小)的微晶(约50个Ax100A或更少)的锰,铼和锝的硫属元素。 这些组合物通过将不含水溶剂,锰,铼或锝盐与硫族化物源混合而制得,产生沉淀物。 锰,铼或锝盐和硫族元素源可以纯净或非水质非质子溶剂的存在下混合。 在除去阴离子盐之前产生的沉淀物是细分的产物。 在铼二硫属元素化合物的情况下,产物具有层状结构。 阴离子盐可以通过本领域常用的任何技术除去,在真空下泵送是一种这样的技术,用合适的溶剂洗涤另一种。 描述了用于制备式MXy的二硫和多硫族化物的方法,其中M是选自下列物质的金属,其中M为选自由锰,铼和锝组成的组,X为选自硫,硒,碲的硫属元素 y为约1.5至约4,优选约2的数值,包括所述锰,铼和锝的盐的混合物的所述MXy化合物的低温非水沉淀。 所述沉淀发生在不含水溶剂的情况下。 本发明的方法允许制备未受水,氧或水解产物污染的物质。

    Method for purifying actinides which are in low oxidation states
    42.
    发明授权
    Method for purifying actinides which are in low oxidation states 失效
    纯化处于低氧化态的锕系元素的方法

    公开(公告)号:US4021313A

    公开(公告)日:1977-05-03

    申请号:US624106

    申请日:1975-10-20

    摘要: A method is provided for purifying actinides which are present in a low oxidation state in aqueous solution. The actinides are purified of fission products by extracting the actinides from aqueous solution while confining the fission products to the aqueous solution. The actinides that are purified are selected from the group of uranium (IV), neptunium (IV) and plutonium (III). An aqueous nitric acid solution containing the actinides, hydrazine nitrate or hydroxyl ammonium nitrate, as well as fission products is initially subjected to an electrolysis voltage. If Pu (III) is involved, the electrolysis voltage is below the voltage at which oxygen develops at the anode and anodically oxidizes the Pu (III) to Pu (IV). The Pu (IV) which is formed is transferred by means of an organic extraction agent from the aqueous solution to an organic phase. The organic phase is then separated and used for the plutonium recovery process. If U (IV) and/or Np (IV) are involved, the aqueous nitric acid solution is initially subjected to an electrolysis voltage in the vicinity of the voltage at which oxygen develops at the anode or higher to anodically oxidize the U (IV) to U (VI) and the Np (IV) to Np (VI). The U (VI) and/or Np (VI) which is formed is transferred by means of an organic extraction agent from the aqueous phase to the organic phase. The organic phase is then separated and used for the uranium or neptunium recovery process.

    摘要翻译: 提供了一种用于纯化在水溶液中以低氧化态存在的锕系元素的方法。 锕系元素通过从水溶液中提取锕系元素而将裂变产物限制在水溶液中来纯化裂变产物。 纯化的锕系选自铀(IV),ium(IV)和钚(III)。 含有锕系元素,硝酸肼或硝酸铵的硝酸水溶液以及裂变产物最初经受电解电压。 如果涉及Pu(III),则电解电压低于在阳极处产生氧气的电压,并将Pu(III)阳极氧化为Pu(IV)。 形成的Pu(IV)通过有机萃取剂从水溶液中转移到有机相中。 然后将有机相分离并用于钚回收过程。 如果涉及U(IV)和/或Np(IV),则硝酸水溶液最初经受在阳极或更高氧发生的电压附近的电解电压,以阳极氧化U(IV) 到U(VI)和Np(IV)到Np(VI)。 形成的U(VI)和/或Np(VI)通过有机萃取剂从水相转移到有机相中。 然后将有机相分离并用于铀或铀回收过程。

    Uranium dioxide preparation
    43.
    发明授权
    Uranium dioxide preparation 失效
    二氧化铀制备

    公开(公告)号:US4003980A

    公开(公告)日:1977-01-18

    申请号:US579495

    申请日:1975-05-21

    摘要: An actinide dioxide, e.g. uranium dioxide, is prepared by reacting an actinide nitrate or hydrate or tetrahydrofuranate thereof, e.g. uranyl nitrate, a hydrate of uranyl nitrate or a tetrahydrofuranate of uranyl nitrate with an alkali or alkaline earth metal adduct of a monocyclic or polycyclic hydrocarbon in the presence of an inert organic solvent. Typically, the starting material may be uranyl nitrate dihydrate or uranyl nitrate ditetrahydrofuranate (the latter material is a novel composition of matter) with a reactant such as the sodium adduct of naphthalene in the presence of a solvent such as tetrahydrofuran. The resultant uranium dioxide may be further purified by heating it in the presence of hydrogen.

    摘要翻译: 二氧化, 二氧化铀是通过使硝酸锕系元素或其水合物或四氢呋喃,例如, 硝酸铀酰,硝酸铀酰的水合物或硝酸铀酰的四氢化物与单环或多环烃的碱金属或碱土金属加成物在惰性有机溶剂的存在下进行。 通常,起始原料可以是硝酸铀酰二水合物或硝酸铀酰二硝酸二铀酸盐(后者是物质的新型组合物)与反应物如萘的加合物在溶剂如四氢呋喃的存在下反应。 所得的二氧化铀可以通过在氢存在下加热来进一步纯化。