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    • 6. 发明授权
    • Process of preparing a solution of cesium and rubidium salts
    • 制备铯和铷盐溶液的方法
    • US5900221A
    • 1999-05-04
    • US649712
    • 1996-09-18
    • Hartmut HofmannKlaus KobeleHorst PrinzKlaus Schade
    • Hartmut HofmannKlaus KobeleHorst PrinzKlaus Schade
    • C01D17/00C04B7/24C07C51/41C07C53/06C07C53/10C07C59/265C22B26/10C01D3/00C22B26/00
    • C07C59/265C01D17/00C04B7/24C07C53/06C07C53/10Y02P40/145Y02P40/18
    • The process for preparing a cesium and rubidium salt-containing solution includes a hydrothermal digestion of an uncalcined pollucite and/or calcined lepidolite particulate having an average particle size up to 0.5 mm with an aqueous solution of Ca(OH).sub.2 in a suspension with a mole ratio of SiO.sub.2 to CaO of from 1:2.5 to 1:1.25 in a rotary tubular autoclave at a digestion temperature of 200 to 280.degree. C., under a pressure of from 15 to 65 bar and at a suspension density between 8 and 18% by weight for from 0.5 to 3 hours; filtering the suspension to remove insoluble solids and to form a digestion filtrate; adding at least one acid or acid anhydride to the digestion filtrate to adjust its pH to 6 and to form the cesium and rubidium salt-containing solution; and performing an evaporation after the hydrothermal digestion to obtain an increase in concentration of cesium salts and rubidium salts in the cesium and rubidium salt-containing solution and to adjust a density of the cesium and rubidium salt-containing solution to from 1.6 to 3.3 g/cm.sup.3. An optional aeration of the digestion filtrate with carbon dioxide to remove lithium and calcium ions in precipitated carbonates may be performed.
    • PCT No.PCT / EP94 / 03651 Sec。 371日期1996年9月18日 102(e)1996年9月18日PCT 1994年11月2日PCT公布。 WO95 / 13986 PCT公开 日期1995年5月26日制备含铯和铷盐的溶液的方法包括用Ca(OH)2水溶液在平均粒径达0.5mm的未煅烧的琉璃榴石和/或煅烧的石榴石颗粒进行水热消解 在旋转管式高压釜中在200至280℃的消化温度下,在15至65巴的压力和悬浮密度下,SiO 2与CaO的摩尔比为1:2.5至1:1.25的悬浮液 8至18重量%,0.5至3小时; 过滤悬浮液以除去不溶性固体并形成消化滤液; 向消化滤液中加入至少一种酸或酸酐以将其pH调节至6并形成含铯和铷盐的溶液; 在水热消解后进行蒸发,得到铯盐和铷盐溶液中的铯盐和铷盐的浓度增加,将含铯盐和铷盐溶液的密度调整为1.6〜3.3g / cm3。 可以任选地将消化滤液与二氧化碳通气以除去沉淀碳酸盐中的锂离子和钙离子。
    • 8. 发明授权
    • Method for producing a high-density saline cesium and rubidium solution
    • 生产高密度盐水铯和铷溶液的方法
    • US5593650A
    • 1997-01-14
    • US436260
    • 1995-07-17
    • Horst PrinzHartmut HofmannKlaus K obeleMarion Wegner
    • Horst PrinzHartmut HofmannKlaus K obeleMarion Wegner
    • C01D17/00C22B26/10C22B26/00
    • C01D17/00
    • The method of making a high density saline cesium and rubidium solution includes comminuting uncalcined pollucite and/or calcined lepidolite to a grain size of less than 0.1 mm; combining the comminuted material in the presence of water with Ca(OH).sub.2 at a mol ratio of SiO.sub.2 to CaO of not less than 1:2; hydro-thermally decomposing at a temperature of 200.degree. to 280.degree. C., a pressure of 20 to 40 bar and with a suspension density of 4 to 15% by weight for from 1 to 3 hours to form a suspension containing insoluble solids; filtering the insoluble solids and washing to form a filtrate and concentrating the filtrate; blowing carbon dioxide into the concentrated filtrate to precipitate calcium carbonate and lithium carbonate and filtering the concentrated filtrate to separate the precipitated carbonates from a remaining solution; and then adding an acid or acid anhydride to the remaining solution until the pH of the remaining solution reaches about 6 and concentrating by evaporation to form the high density saline cesium and rubidium solution.
    • PCT No.PCT / EP93 / 03143 Sec。 371日期:1995年7月17日 102(e)日期1995年7月17日PCT 1993年11月10日PCT公布。 公开号WO94 / 11303 日期:1994年5月26日制造高密度盐水铯和铷溶液的方法包括粉碎未煅烧的堇青石和/或煅烧碎石,粒度小于0.1mm; 在水与Ca(OH)2的存在下,以SiO 2与CaO的摩尔比不小于1:2组合粉碎材料; 在200〜280℃的温度,20〜40巴的压力和4〜15重量%的悬浮液密度下进行1〜3小时的热分解,形成含有不溶性固体的悬浮液; 过滤不溶性固体并洗涤以形成滤液并浓缩滤液; 将二氧化碳吹入浓缩的滤液中以沉淀碳酸钙和碳酸锂并过滤浓缩的滤液以将沉淀的碳酸盐与剩余的溶液分离; 然后向剩余的溶液中加入酸或酸酐直到剩余溶液的pH达到约6并通过蒸发浓缩以形成高密度盐水铯和铷溶液。