CN1192423A - 获取氪和氙的方法 - Google Patents

获取氪和氙的方法 Download PDF

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CN1192423A
CN1192423A CN98100589A CN98100589A CN1192423A CN 1192423 A CN1192423 A CN 1192423A CN 98100589 A CN98100589 A CN 98100589A CN 98100589 A CN98100589 A CN 98100589A CN 1192423 A CN1192423 A CN 1192423A
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krypton
xenon
concentrate
crust
sorbent material
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卡尔·鲍尔·米夏埃尔·华拉
拉尔夫·斯波里
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Abstract

本发明涉及一种在深冷空分装置中获取氪和/或氙的方法,其中氪和氙被浓集成氪－氙浓缩物,通过对蒸馏氪－氙浓缩物再得到氪和/或氙。为了脱除含氟和/或含氯的杂质、特别是氟代烃CF4和/或SF6,此氪－氙浓缩物和/或氪和/或氙在含有叶硅酸盐的固体吸附剂上进行净化。

Description

获取氪和氙的方法
本发明涉及一种在深冷空分装置中获取氪和/或氙的方法，其中氪和氙被浓集成氪-氙浓缩物，再通过蒸馏从此氪-氙浓缩物获取氪和/或氙。
惰性气体含量仅约1ppm Kr和0.09ppm Xe的空气在一个空分装置中经过大量空气的处理后获得了氪和氙。氪和氙的沸点为120K和165K，即远高于氮、氧和其他惰气的沸点，因而在一般的双柱精馏器中氪和氙和各种碳氢化合物一起被浓集在液氧中。
为了获取Kr/Xe，从主冷凝器中引出一部分浓集有Kr/Xe的液氧，送到一个氪浓集柱中去。从此浓集柱可得到氪-氙浓缩物，它含有1％Kr、约0.5％碳氢化合物和0.1％氙，主要组份是氧。
留在浓缩物中的碳氢化合物，特别是甲烷，它的着火浓度确定了氪和氙的最大浓缩程度。由于碳氢化合物的挥发性低，精镏时它们也浓集在液氧中。在氧存在下，若越过着火浓度，对甲烷是5体积％含量，即生成爆炸混合物。为了在装置停车、在失效和局部浓集情况下不产生危险的甲烷浓缩，在实践中至少设计有10倍的安全因子，即甲烷含量限制在最大为0.5体积％。
从氪浓集柱得到的浓缩物在超临界压力下蒸发，加热到大约500℃，然后加入催化剂，使碳氢化合物分解为水蒸气和二氧化碳。通过分子筛将水蒸气和二氧化碳从浓缩物中去除。然后在另一个蒸镏柱中脱除氧得到高浓氪-氙浓缩物。通过一个紧接着的氪-氙精镏在精镏柱顶部取出氪，在底部取出纯的无氪的氙。
在所述的由深冷空分装置获取氪和氙的方法中，氪和氙浓缩了约106倍和108倍。而空气中的痕量杂质也同时被浓缩了，这里首先要提到温室气如CF4、CFCl3、CF2Cl2、C2F6和SF6。
含氟和氯的碳氢化合物(FCKW)热稳定性是非常高的，例如CF4在大气压下的热分解要到温度超过900℃时才发生。用催化剂可以把分解温度降下来，但是氟碳物质的分解对催化剂有损害。吸附脱除FCKW也被证明不适宜用于深冷空分装置，因为已知的分子筛对FCKW吸附得很差，而且还损害吸附剂。
氪和氙因而还含有可测到量的杂质，这些杂质至今仍不能通过催化分解或通过吸附而除去。
因而本发明的目的是提出一种上述类型的方法，此法能够获取高纯的、特别是不含氟和/或氯杂质，如氟代烃CF4和SF6的氪和/或氙。
该目的是如下解决的：氪-氙浓缩物和/或氪和/或氙用含有叶硅酸盐(phyllosilikate)的固态吸附剂进行净化，由此从氪-氙浓缩物和/或氪和/或氙中脱除含氟和/或含氯的杂质，特别是氟代烃CF4和/或SF6。
采用含有叶硅酸盐的吸附剂方法来自另一技术领域，即排除卤代烃，如从冰箱中排除FCKW冷冻剂，它在DE-A-4404329中是已知的。令人惊异地发现，用这类吸附剂对在制备惰气的深冷空分装置中得到的氪-氙浓缩物、氪和/或氙能很好地进行净化。
按本发明浓集的氪-氙浓缩物和/或经蒸镏后的氪和/或氙产品将通过含有叶硅酸盐的吸附剂。氪、氙或其混合物中存在的含氟或含氯的杂质将因化学吸附被留在此吸附剂中。特别是用目前催化剂在高温和高含氧时不能破坏的氟代烃，如CF4、CCl2F2或CCl3F和SF6，此吸附剂也能将它们分解或固定住。在化学反应中于吸附剂中产生的含氟分解产物也同样能不可逆地、牢固地被吸附住。由吸附剂出来的惰性气体或惰气混合物因而不含有至今不能或很难脱除的氟和氯化合物。目前的氪产品含杂质达100ppm CF4，氙含杂质达100ppm SF6。通过采用本发明的方法，有可能获得高纯的最终产品。含氟和/或含氯杂质的脱除既可以在有氧存在下也可以在无氧存在下完成，优选在无氧存在下完成。
氟碳化合物在吸附剂中进行化学反应时生成作为副产物的二氧化碳。另外，吸附剂载体材料中也散布出痕量氧和水。由吸附剂出来的氪和/或氙被二氧化碳、水和氧污染。为了得到高纯的最终产品，经吸附剂净化后的氪-氙浓缩物和/或氪和/或氙还要再脱除水，二氧化碳和/或氧。
最好用分子筛脱除水和/或二氧化碳。一般采用两个可交替操作的分子筛吸附器，其中一个吸附二氧化碳和水气，而另一个进行再生。工作着的即在吸附的分子筛吸附器的温度有意控制在略高于水的冰点，以降低吸附水蒸气含量。
按本发明净化后，在氪、氙或氪-氙浓缩物中存在的氧优选用Ni-Cu催化剂从气体或气体混合物中脱除。
如果氪-氙浓缩物和/或氪和/或氙在1巴和10巴之间的压力下进行净化，能获得特别好的净化效果，优选在2巴和3巴之间的压力下。
对于温度范围，氪-氙浓缩物和/或氪和/或氙在300℃和600℃之间温度下进行净化已证明是有利的，优选在450℃和550之间。
按本发明用含有叶硅酸盐的吸附剂的净化方法优选在氪-氙浓缩物分离成氪和氙之前进行净化。这样可以在一个净化级中既脱除了氪中的也脱除了氙中的含氟和/或氯的杂质，由此可以免去双重实施本发明净化方法所需的所有设备。
按本发明方法净化单个产品氪和氙而不是净化两种惰气浓缩的混合物也有其好处。在净化浓缩混合物时，在吸附剂中吸附了不同的物质如CF4和SF6。如果吸附剂被此类物质中之一种物质如CF4所饱和，那么即使此吸附剂还能接受其他杂质如SF6，此吸附剂也必须去解吸。与此相反，在氪-氙分离后在净化单个产品时，对氪主要是CF4、对氙是SF6必须脱除。这种场合，吸附剂可设计为专用吸附剂，而且此吸附剂的接受容量也能被全部利用。
本发明以及本发明的其他优点可由下面简图所展示的实施例来详细说明。
这里展示的是能获取氪-氙的空分装置流程图的一部份。
由未示出的氪浓集柱得到的氪-氙浓缩物被加热到约500℃并引往贵金属燃烧催化剂，以使浓缩物中存在的甲烷完全分解。在此反应中产生的产物水和二氧化碳紧接着被分子筛吸附掉。
此氪-氙浓缩物然后在换热器1中被冷却后引向第一个氪柱2。氧的沸点比氪和氙低，所以可以在柱2的顶部3取出。在氪柱2的底部4取出高度浓缩的经进一步脱氧的氪-氙混合物，但是它仍含有空气中的痕量杂质如CF4或SF6，它们不能被前置的催化剂和吸附器所脱除因而同样被浓缩了。
此氪-氙浓缩物被引向吸附剂5，它至少含有10％、优选大于50％的叶硅酸盐。在此浓缩物中含有的杂质被吸附剂5的不可逆化学吸附固定住。反应在压力2和3巴之间，优选在2.5巴下进行，温度选择在450℃和550℃之间优选500℃。在吸附剂5中浓缩物脱除了所有残留的杂质。
在吸附剂5中的化学反应产生了分解产物二氧化碳，从吸附剂5中还释放出水蒸气和氧。为脱除二氧化碳和水，此浓缩物被引到两个交替操作的分子筛吸附器6中，其中一个工作时另一个进行再生。
分子筛吸附器6的再生优选用氧来完成。再生后此分子筛吸附器6在气瓶(Gasballon)排空并抽空。气瓶中捕集的气体重返空分系统。这样使再生的损失降低，特别是氪和氙的损失。
浓缩物接着被引向Ni-Cu催化剂7，在此脱除氪-氙浓缩物中残留的痕量氧。净化后的浓缩物再送到另一个精馏柱8中，可以从柱顶9取出高纯的氪，从柱底10取出高纯的氙。

Claims (5)

1.在深冷空分装置中制取氪和/或氙的方法，其中，氪和氙被浓缩为氪-氙浓缩物，然后通过蒸馏从此氪-氙浓缩物获取氪和/或氙，其特征在于，氪-氙浓缩物和/或氪和/或氙在含有叶硅酸盐的固体吸附剂上进行净化，这样使氪-氙浓缩物和/或氪和/或氙中的含氟和含氯杂质、特别是氟代烃CF4和/或SF6得以脱除。
2.按权利要求1的方法，其特征在于，经吸附剂净化后，氪-氙浓缩物和/或氪和/或氙中的水、二氧化碳和/或氧得以脱降。
3.按权利要求2的方法，其特征在于，藉助于分子筛脱除水和/或二氧化碳。
4.按权利要求1到3中任一项的方法，其特征在于，氪-氙浓缩物和/或氪和/或氙在1巴和10巴之间、优选2巴和3巴之间的压力下进行净化。
5.按权利要求1到4中任一项的方法，其特征在于，氪-氙浓缩物和/或氪和/或氙在300℃和600℃之间、优选在450℃和550℃之间的温度下进行净化。
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