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1. 发明授权

US5112493A Zirconium-hafnium production in a zero liquid discharge process 失效
标题翻译：零液体放电过程中的ZIRCONIUM-HAFNIUM生产
公开(公告)号：US5112493A
公开(公告)日：1992-05-12
申请号：US624782
申请日：1990-12-10
申请人： Thomas S. Snyder , Ernest D. Lee
发明人： Thomas S. Snyder , Ernest D. Lee
IPC分类号： B01D15/08 , C22B3/44 , C22B34/14
CPC分类号： C22B3/44 , C22B34/14 , Y02P10/234
摘要： A simple, low cost continuous process for separating and purifying zirconium and hafnium which eliminates liquid waste and facilitates the management of RCRA and LLW wastes is provided. An aqueous zirconium and hafnium--containing feed solution is prepared and fed to a continuously rotating annular chromatograph containing a bed of acid exchange resin. An acid eluant, such as hydrochloric acid, nitric acid, phosphoric acid or the like, is fed through the acid exchange bed while chromatograph is rotating, which separates the feed into substantially pure zirconium and hafnium fractions and into RCRA and LLW waste fractions. The zirconium and hafnium are processed further into nuclear quality zirconium and hafnium metals. The acid eluant is recycled for reuse in the chromatograph, and the RCRA and LLW waste fractions are disposed of in solid form.

2. 发明授权

US5023061A Chromatographic separation of zirconium isotopes with anhydrous readily recyclable eluents 失效
标题翻译：用无水易回收的洗脱液色谱分离锆同位素
公开(公告)号：US5023061A
公开(公告)日：1991-06-11
申请号：US546982
申请日：1990-07-02
申请人： Thomas S. Snyder , Ernest D. Lee
发明人： Thomas S. Snyder , Ernest D. Lee
IPC分类号： B01D15/08 , B01D59/30 , B01J39/12 , C01G25/00 , G01N30/02 , G01N30/34 , G01N30/44 , G01N30/58 , G01N30/60 , G01N30/88
CPC分类号： B01J39/12 , B01D15/1892 , B01D59/30 , C01G25/003 , G01N30/58 , G01N30/6052 , B01D15/362 , G01N2030/342 , G01N2030/587 , G01N2030/8809 , G01N2030/8859 , G01N30/02 , G01N30/34 , G01N30/44 , G01N30/6017 , G01N30/6047
摘要： The isotopes of zirconium can be partially or completely separated by loading an essentially anhydrous alcoholic solution of an ionic compound of zirconium onto a cationic exchange resin with pentavalent phosphorus derived active groups which serves as the stationary phase of a chromatograph, eluting the compound with an essentially anhydrous alcoholic solution of hydrogen chloride and collecting distinct elution volumes representative of each isotope. In a preferred embodiment, the active groups of the cation exchange resin are derived from di-2-ethylhexyl phosphoric acid, tri-n-octyl phosphine oxide or tributyl phosphate and the chromatograph is of a type, such as a continuous annular chromatograph that it can be operated in a continuous steady state manner.

3. 发明授权

US5098678A Chromatographic separation of zirconium isotopes 失效
标题翻译： ZIRCONIUM同位素的色谱分离
公开(公告)号：US5098678A
公开(公告)日：1992-03-24
申请号：US515965
申请日：1990-04-27
申请人： Ernest D. Lee , Thomas S. Snyder , Edward J. Lahoda
发明人： Ernest D. Lee , Thomas S. Snyder , Edward J. Lahoda
IPC分类号： B01D59/30 , G01N30/58
CPC分类号： B01D59/30 , G01N30/58 , Y10S423/07
摘要： The isotopes of zirconium can be partially or completely separated by loading an aqueous solution of an ionic compound of zirconium onto a cationic exchange resin which serves as the stationary phase of a chromatograph, eluting the compound with an aqueous acid and collecting distinct elution volumes representative of each isotope. In a preferred embodiment, the eluant is a strong mineral acid, such as hydrochloric acid and the chromatograph is of a type, such as a continuous annular chromatograph that it can be operated in a continuous, steady state manner.

4. 发明授权

US5174971A Continuous anion exchange chromatography for the separation of zirconium isotopes 失效
标题翻译：用于分离ZIRCONIUM同位素的连续阴离子交换色谱
公开(公告)号：US5174971A
公开(公告)日：1992-12-29
申请号：US597948
申请日：1990-10-10
申请人： Thomas S. Snyder , Michael C. Skriba , Edward J. Lahoda , Ernest D. Lee
发明人： Thomas S. Snyder , Michael C. Skriba , Edward J. Lahoda , Ernest D. Lee
IPC分类号： B01D59/30 , G01N30/58
CPC分类号： B01D59/30 , G01N30/58 , Y10S423/07
摘要： The thermal neutron capture cross-section of zirconium may be altered by altering its natural isotope distribution through a steady state chromatographic separation of these isotopes using an anion exchange resin as the stationary phase of the chromatographic column. Zirconium is dissolved in a very strong acid which causes the formation of a zirconium anion, such as the ZrOCl.sub.4.sup.-2 anion formed in six normal hydrochloric acid, and eluted off the column with a weaker acid. Distinct elution volumes representative of each isotope are collected. In a preferred embodiment, the process also separates the zirconium from hafnium and the other impurities normally present in the product obtained by chlorinating zircon sand and utilizes a continuous annular chromatograph.
摘要翻译：通过使用阴离子交换树脂作为色谱柱的固定相，通过这些同位素的稳态色谱分离改变其天然同位素分布，可以改变锆的热中子捕获截面。将锆溶解在非常强的酸中，导致形成锆阴离子，例如在六个正常盐酸中形成的ZrOCl4-2阴离子，并用较弱的酸从柱中洗脱出来。收集代表每个同位素的不同洗脱体积。在优选的实施方案中，该方法还将锆与铪和通过氯化锆石砂获得的产物中通常存在的其它杂质分离，并使用连续的环状色谱仪。

5. 发明授权

US5110566A Chromatographic separation of zirconium isotopes with reduced waste liquor 失效
标题翻译：锆同位素的色谱分离与废液的还原
公开(公告)号：US5110566A
公开(公告)日：1992-05-05
申请号：US555342
申请日：1990-07-19
申请人： Thomas S. Snyder , Ernest D. Lee
发明人： Thomas S. Snyder , Ernest D. Lee
IPC分类号： C22B34/14 , B01D59/30 , G01N30/02 , G01N30/58 , G01N30/88
CPC分类号： B01D59/30 , G01N30/58 , G01N2030/587 , G01N2030/8809 , G01N30/02 , Y10S423/07
摘要： The isotopes of zirconium can be partially or completely separated by loading an aqueous solution of an ionic compound of zirconium onto a cationic exchange resin with pentavalent phosphorus derived active groups which serves as the stationary phase of a chromatograph, eluting the compound with an aqueous acid and collecting distinct elution volumes representative of each isotope. In a preferred embodiment, the eluant is a strong mineral acid, such as hydrochloric acid and the chromatograph is of a type, such as a continuous annular chromatograph, that it can be operated in a continuous, steady state manner.
摘要翻译：通过将锆的离子化合物的水溶液加载到具有五价磷衍生的活性基团的阳离子交换树脂上，可以部分或完全分离锆的同位素，其作为色谱的固定相，用酸水溶液洗脱化合物，收集代表每个同位素的不同洗脱体积。在优选的实施方案中，洗脱剂是强无机酸，例如盐酸，并且色谱是类型的，例如连续环状色谱仪，其可以以连续，稳定的方式操作。

6. 发明授权

US5009866A Fused salt process for purifying zirconium and/or hafnium tetrachlorides 失效
标题翻译：用于纯化锆和/或四氢化铪的熔盐方法
公开(公告)号：US5009866A
公开(公告)日：1991-04-23
申请号：US437152
申请日：1989-11-16
申请人： Ernest D. Lee
发明人： Ernest D. Lee
IPC分类号： C01G25/04 , C01G27/04
CPC分类号： C01G27/04 , C01G25/04
摘要： Continuous production of zirconium and/or hafnium metal from a fused salt bath in which one of the salts is zirconium and/or hafnium tetrachloride is carried out by feeding additional, make-up zirconium and/or hafnium tetrachloride powder into a zirconium and/or hafnium dissolution area of the bath maintained at a dissolution temperature below which the tetrachloride will vaporize, by circulating portions of the bath into and through a separate but contiguous area maintained at a temperature at which the tetrachloride will vaporize, and by recovering the vaporized tetrachloride. It is preferred that the vaporization area of the bath be wholly surrounded by and insulated from the dissolution area of the bath.
摘要翻译：从其中一种盐是锆和/或四氯化铪的熔融盐浴连续生产锆和/或铪金属，通过将另外的化妆锆和/或四氢铪粉末加入锆和/或浴的铪溶解面积保持在低于四氯化碳将蒸发的溶解温度，通过将浴的一部分循环进入并通过保持在四氯化碳将蒸发的温度的分离但连续的区域，并回收蒸发的四氯化物。优选的是，浴的蒸发区域被浴完全包围并与其隔离。

7. 发明授权

US4913778A Molten salt scrubbing of zirconium or hafnium tetrachloride 失效
标题翻译：熔盐洗涤锆或四氯化铪
公开(公告)号：US4913778A
公开(公告)日：1990-04-03
申请号：US305125
申请日：1989-01-02
申请人： Ernest D. Lee , David F. McLaughlin
发明人： Ernest D. Lee , David F. McLaughlin
IPC分类号： C01G25/04 , C01G27/04
CPC分类号： C01G27/04 , C01G25/04
摘要： Removal of aluminum and iron impurities is accomplished using an absorbing column containing potassium or sodium chloride, producing an aluminum and iron chloride-rich bottoms product and purified Zr(Hf)Cl.sub.4 vapor at the top of the column. This invention is a continuous process for removing impurities of iron or aluminum chloride or both from vaporous zirconium chloride (or hafnium chloride or a mixture thereof). When iron is being removed from zirconium tetrachloride using potassium chloride, the process comprises: introducing impure zirconium chloride vapor into a middle portion of an absorbing column containing a potassium chloride-containing molten salt phase, the molten salt phase absorbing the iron chloride impurity to produce a zirconium chloride vapor stripped of iron chloride in the top portion of the column; introducing potassium chloride into a top portion of the column; controlling the top portion of the column to between 300.degree.-375.degree. C.; heating a bottom portion of the column to 450.degree.-550.degree. C. to vaporize zirconium chloride from the molten salt; withdrawing molten salt substantially free of zirconium and hafnium chloride from the bottom portion of the column; and withdrawing zirconium chloride vapor substantially free of iron chloride impurity from the top of the column. Similarly, hafnium or hafnium-zirconium mixtures can be substituted for zirconium, or aluminum or iron-aluminum can removed rather than iron, or sodium chloride or sodium potassium chloride mixtures can be substituted for potassium chloride.
摘要翻译：使用含有氯化钾或氯化钠的吸收塔来实现铝和铁杂质的去除，产生富含铝和铁的富含氯化铁的底部产物以及柱顶部纯化的Zr（Hf）Cl4蒸气。本发明是从气态氯化锆（或氯化铪或其混合物）中除去铁或氯化铝或二者的杂质的连续方法。当使用氯化钾从四氯化锆中除去铁时，该方法包括：将不纯的氯化锆蒸气引入含有含有氯化钾的熔融盐相的吸收塔的中间部分，该熔融盐相吸收氯化铁杂质以产生在柱的顶部剥离氯化铁的氯化锆蒸气; 将氯化钾引入柱的顶部; 将塔顶部控制在300〜-375℃之间。将塔底部加热至450-550℃，以使熔融盐中的氯化锆蒸发; 从塔的底部抽出基本上不含锆和氯化铪的熔融盐; 并从塔顶排出基本上不含氯化铁杂质的氯化锆蒸汽。类似地，铪或铪锆混合物可以代替锆，或者可以除去铝或铁 - 铝而不是铁，或者氯化钠或氯化钾的混合物可以代替氯化钾。

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