CN1121705A - 从铯矾制备铯盐的方法 - Google Patents

从铯矾制备铯盐的方法 Download PDF

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CN1121705A
CN1121705A CN94191890A CN94191890A CN1121705A CN 1121705 A CN1121705 A CN 1121705A CN 94191890 A CN94191890 A CN 94191890A CN 94191890 A CN94191890 A CN 94191890A CN 1121705 A CN1121705 A CN 1121705A
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calcium
cesium
caesium
alum
water
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CN1055677C (zh
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哈特穆特·霍夫曼
克劳斯·科贝勒
赫斯特·普林茨
贝尔恩德·菲利普
格尔德·哈姆斯
亚历山大·席德特
乌尔里克·海克特尔
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Keime Starr Ltd By Share Ltd
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Metal Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/41—Preparation of salts of carboxylic acids
    • C07C51/412—Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D17/00—Rubidium, caesium or francium compounds

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
  • Transition And Organic Metals Composition Catalysts For Addition Polymerization (AREA)
  • Medicines That Contain Protein Lipid Enzymes And Other Medicines (AREA)
  • Processing Of Solid Wastes (AREA)
  • Inorganic Insulating Materials (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Catalysts (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

本发明涉及一种从铯矾制备铯盐的方法，该方法是在一单一容器中，在水存在下使铯矾与氢氧化钙反应，氢氧化钙的用量与铯矾中的铝的摩尔数相等，并使铯矾与易溶于水的钙盐反应，易溶于水的钙盐的摩尔用量与铯矾中的铯的摩尔数相等，采用过滤或离心分离的方法分离出氢氧化铝和硫酸钙沉淀。

Description

从铯矾制备铯盐的方法
本发明涉及一种从铯矾制备铯盐的方法。
美国专利3,489,509公开了一种制备具有高纯度的铯化合物的方法。该方法中，铯矾(cesium-aluminum-alum)用氢氧化钡处理，接着与二氧化碳反应。随后加入化学计量的卤化钡，以得到纯卤化铯。为了从铯矾得到卤化铯，需要使用氢氧化钡和卤化钡，这将导致费用高昂，并且要发生与二氧化碳的中和反应。
本发明的一个目的是提供一种能克服如上所述的缺点的方法。
按照本发明，上述目的是这样达到的：在一单一容器中，将铯矾和氢氧化钙反应，氢氧化钙的用量与铯矾中的铝的摩尔数相等，然后和与水溶性钙盐反应，水溶性钙盐的用量与铯矾中的铯的摩尔数相等，经过滤或离心分离分离出氢氧化铝和硫酸钙沉淀。在本发明的方法中，不使用比钙化合物昂贵的钡化合物，并且不用进行与二氧化碳的中和反应；其一个进一步的优点是，由反应直接得到的铯盐溶液的浓度大于10％。这将大大降低在制备浓缩的铯盐溶液以及在制备固体盐的过程中从溶液中除去水的工作量。
对于按照下述方程式使铯矾与化学计量的氢氧化钙的直接反应CsAl(SO4)2＋2Ca(OH)2→CsOH＋Al(OH)3＋2CaSO4是周知的，但是该反应不能以很满意的收率得到氢氧化铯。这可能是因为产生的氢氧化铝和石膏沉淀掩蔽了悬浮的氢氧化钙的表面，以致于其不能参与反应。另一方面，也不能通过使用氢氧化钙来补偿被掩蔽的氢氧化钙，因为补加的氢氧化钙的量必须精确控制方能避免目的产物氢氧化铯的被污染，而被污染的产品中的氢氧化钙很难除去。因为这一原因，本领域中通常是使用氢氧化钡；其更易溶于水但也非常昂贵。
采用本发明的方法，令人惊奇地发现，可在一单一的容器中制备出纯的铯盐。甲酸钙、乙酸钙、柠檬酸钙、氯化钙或溴化钙可用作所述的水溶性钙盐。
优选是以以下方式从铯矾制备铯盐：所述的反应在80～120℃的范围内进行，并且在反应开始时，悬浮液的每升水中的不溶性固体物为100～500克。所述的不溶性固体物由反应开始时不溶的那部分Ca(OH)2、铯盐和铯矾所组成。
下面用下述实施例更详细地说明本发明。实施例1 甲酸铯的制备
向一可加热和可搅拌的容积为500升的容器中加入290升水、17千克氧化钙和13千克甲酸钙。将得到的悬浮液在搅拌下加热至其沸点，然后加入111千克铯矾。将反应混合物在其沸点温度搅拌2小时，随后将其冷却和过滤。滤液含有约11％的甲酸铯、0.1％的钙离子、0.05％的铝离子和1％的硫酸根离子。滤渣再用水洗涤。在合并的滤液中检测出约有95％的原料中的铯被转化成了甲酸铯。实施例2 乙酸铯的制备
使用与实施例1中相类似的容器，只是其容积为1000升。向其中加入375千克水、43.8千克氧化钙和45.8千克乙酸钙。将得到的悬浮液加热至其沸点，然后加入296千克铯矾。随后将该悬浮液在其沸点温度下搅拌2小时并使其冷却，然后过滤。得到的溶液中含有约20％的乙酸铯，其中含有58％的原料中的铯。将滤渣再洗涤，回收得到乙酸铯水溶液，其中又含有原料中的铯的37％。

Claims (3)

1、从铯矾制备铯盐的方法，其特征在于：
在一单一容器中，在水存在下使铯矾与氢氧化钙反应，氢氧化钙的用量与铯矾中的铝的摩尔数相等，并使铯矾与易溶于水的钙盐反应，易溶于水的钙盐的摩尔用量与铯矾中的铯的摩尔数相等，采用过滤或离心分离的方法分离出氢氧化铝和硫酸钙沉淀。
2、如权利要求1所述的方法，其特征在于：所述的易溶于水的钙盐为甲酸钙、乙酸钙、柠檬酸钙、氯化钙或溴化钙。
3、如权利要求1和2所述的方法，其特征在于：所述的反应是在一悬浮液中，在80～120℃温度范围内进行，所述的悬浮在反应开始时的密度相当于每升水含有100～500克不溶性固体物。
CN94191890A 1993-04-24 1994-04-19 从铯矾制备铯盐的方法 Expired - Lifetime CN1055677C (zh)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE4313480A DE4313480C1 (de) 1993-04-24 1993-04-24 Verfahren zur Herstellung von Cäsiumsalzen aus Cäsium-Aluminium-Alaun
DEP4313480.7 1993-04-24

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CN1121705A true CN1121705A (zh) 1996-05-01
CN1055677C CN1055677C (zh) 2000-08-23

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EP (1) EP0695286B1 (zh)
JP (1) JP4079991B2 (zh)
KR (1) KR100303251B1 (zh)
CN (1) CN1055677C (zh)
AT (1) ATE161818T1 (zh)
AU (1) AU679528B2 (zh)
BR (1) BR9406214A (zh)
CA (1) CA2161245C (zh)
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DE (2) DE4313480C1 (zh)
DK (1) DK0695286T3 (zh)
FI (1) FI112204B (zh)
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NO (1) NO303984B1 (zh)
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RO (1) RO113983B1 (zh)
SK (1) SK280404B6 (zh)
WO (1) WO1994025422A1 (zh)
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110172575A (zh) * 2019-07-05 2019-08-27 新疆有色金属研究所 一种铯矾原料的处理方法
CN110256232A (zh) * 2019-06-28 2019-09-20 百杰瑞(荆门)新材料有限公司 一种甲酸铯生产方法

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6015535A (en) * 1995-04-06 2000-01-18 Cabot Corporation Process for producing purified cesium compound from cesium alum
DE69629285T2 (de) * 1995-04-06 2004-01-29 Cabot Corp Verfahren zur herstellung von caesiumverbindungen
US6652820B2 (en) 2001-04-02 2003-11-25 Cabot Corporation Methods of making cesium salts and other alkali metal salts
RU2408534C2 (ru) * 2005-01-27 2011-01-10 Шеметалл Гмбх Способ получения растворов гидроксида цезия
US7759273B2 (en) * 2005-04-20 2010-07-20 Cabot Corporation Methods of forming an alkali metal salt

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2481455A (en) * 1948-06-01 1949-09-06 Dow Chemical Co Cesium bromide separation
GB949483A (en) * 1961-05-25 1964-02-12 Atomic Energy Authority Uk Improvements in or relating to the recovery of caesium
US3207571A (en) * 1962-04-09 1965-09-21 San Antonio Chemicals Inc Process for preparing cesium compounds from cesium alum
US3130010A (en) * 1962-12-04 1964-04-21 Dow Chemical Co Process for production of high purity cesium metal and cesium compounds
DE1253252B (de) * 1963-03-01 1967-11-02 Atomic Energy Commission Verfahren zum Abtrennen von radioaktivem Caesium aus waessrigen Loesungen
US3489509A (en) * 1967-05-18 1970-01-13 Kewanee Oil Co Process for recovery of cesium compounds of high purity

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110256232A (zh) * 2019-06-28 2019-09-20 百杰瑞(荆门)新材料有限公司 一种甲酸铯生产方法
CN110256232B (zh) * 2019-06-28 2022-05-03 百杰瑞(荆门)新材料有限公司 一种甲酸铯生产方法
CN110172575A (zh) * 2019-07-05 2019-08-27 新疆有色金属研究所 一种铯矾原料的处理方法

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LV11540B (en) 1996-12-20
PL311231A1 (en) 1996-02-05
CZ287380B6 (en) 2000-11-15
AU6679294A (en) 1994-11-21
HUT72014A (en) 1996-03-28
SK280404B6 (sk) 2000-01-18
HU214206B (hu) 1998-01-28
CZ273795A3 (en) 1996-12-11
EP0695286A1 (de) 1996-02-07
US5605669A (en) 1997-02-25
EP0695286B1 (de) 1998-01-07
AU679528B2 (en) 1997-07-03
NO303984B1 (no) 1998-10-05
ZA942813B (en) 1995-10-23
KR100303251B1 (ko) 2001-11-22
DE4313480C1 (de) 1994-04-14
NO954134D0 (no) 1995-10-17
CN1055677C (zh) 2000-08-23
BR9406214A (pt) 1996-01-09
RO113983B1 (ro) 1998-12-30
ATE161818T1 (de) 1998-01-15
LV11540A (lv) 1996-10-20
DE59404963D1 (de) 1998-02-12
FI955049A (fi) 1995-10-23
JPH08509235A (ja) 1996-10-01
WO1994025422A1 (de) 1994-11-10
HU9503041D0 (en) 1995-12-28
PL177619B1 (pl) 1999-12-31
FI955049A0 (fi) 1995-10-23
ZW4994A1 (en) 1994-11-23
SK131195A3 (en) 1996-04-03
NO954134L (no) 1995-10-17
DK0695286T3 (da) 1998-02-09
CA2161245C (en) 2001-04-10
CA2161245A1 (en) 1994-11-10
FI112204B (fi) 2003-11-14
JP4079991B2 (ja) 2008-04-23

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