CN107109516A - 从锂‑硫‑蓄电池中回收锂的方法 - Google Patents

从锂‑硫‑蓄电池中回收锂的方法 Download PDF

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CN107109516A
CN107109516A CN201580058207.7A CN201580058207A CN107109516A CN 107109516 A CN107109516 A CN 107109516A CN 201580058207 A CN201580058207 A CN 201580058207A CN 107109516 A CN107109516 A CN 107109516A
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lithium
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M-C.米勒
S.皮茨纳
H.维策
V.尼克尔
M.施泰因比尔德
J.威廉斯
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Albemarle Germany GmbH
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Abstract

本发明涉及从锂‑硫‑蓄电池中回收锂的方法，其中将所述蓄电池放电、弄碎和通过筛分或筛选预清理以分离壳体和集流体部分，将剩余的材料分散在水性介质中，将不溶性成分通过过滤除去和将电解质通过相分离除去，接着进行用于从剩余的滤液中分离锂的方法。

Description

从锂-硫-蓄电池中回收锂的方法
本发明的主题是从锂-硫-蓄电池中回收锂的方法。
移动电子设备需要功率越来越强大的可充电电池组，以确保独立的电流供应。为了这个目的，使用锂电池组，这是由于它们的以Wh/m3表示的体积能量密度、循环稳定性和低的自放电。锂-硫-蓄电池被认为是非常有希望的电池元件。这些电池组中的活性阴极材料由硫化锂复合材料组成，其中在充电过程中释放锂离子，并且将其输送到阳极中和在那里作为金属锂沉积或者以合金的形式储存在主体材料，例如硅、锡或铝中。大型的锂蓄电池用于固定式的应用（电源备份）或在汽车行业中用于牵引目的（混合动力驱动或纯电动驱动）。由于随着生产、使用和随后消耗的电池组的尺寸和数量，其中所含的有价值材料的量增加，所以需要用于回收电池中所含的锂的经济方法。
从文献US 8,557,412 B2中已知一种用于处理电池组成分的方法，其中该电池组成分包括至少一种含锂的活性阴极材料和含锂的固体电解质材料。该处理如下进行：将所述的电池组成分用诸如水的工艺流体处理以形成硫化氢，并且将锂从固体电解质材料中溶解出以及转化为硫化锂。然后分离不溶性阴极材料和回收锂组分。
已知的方法仅描述了具有嵌入电极材料的固体电解质电池的处理。
本发明的目的在于提供一种方法，通过该方法能够从锂-硫-蓄电池中回收锂。
所述目的通过从锂-硫-蓄电池中回收锂的方法实现，其中将所述蓄电池放电、弄碎和通过筛分或筛选预清理以分离壳体和集流体部分，将剩余的材料分散在水性介质中，优选分散在pH值≥7的碱性介质中以避免释放硫化氢，将不溶性成分通过过滤除去和将电解质通过相分离除去，接着进行用于从剩余的滤液中分离锂的方法。
从滤液中分离锂优选通过在100-1500℃的温度范围内的热处理而进行。所述热处理特别优选在200至500℃的温度范围内在氧的存在下进行。替代地，所述处理也可以在100至1500℃的温度范围内在排除氧的情况下进行。替代地，所述热处理也可以在相对于环境压力降低的压力下在20-500℃的温度范围内进行。
尽管在充满的介质（加压空气）中存在CO2，没有观察到碳酸盐的形成。这是令人惊奇的，因为在热处理过程中形成的氢氧化锂通常与CO2反应生成碳酸锂。同样令人惊奇地，在500℃的温度下仅少量的硫被存在的氧氧化成硫酸盐和作为主要组分形成氢氧化锂。
为此替代地，从滤液中分离锂通过化学氧化而进行。优选地，所述化学氧化通过与过氧化氢或臭氧的反应而进行。一个替代的变型方案在于通过羟基自由基的氧化。
根据本发明，从滤液中分离锂也通过在酸性条件下的处理而进行。优选地，对于在酸性条件下的处理，将含有的锂通过添加硫酸或盐酸转移到相应的盐中。将形成的多硫化合物通过萃取而分离。主要形成的硫化氢以气体形式从所述混合物中逸出。
替代地，从滤液中分离锂通过沉淀进行。在此，通过添加水溶性的碳酸盐而使锂从滤液中作为碳酸锂沉淀出。
在下文中，借助五个实施例进一步阐述本发明的方法。
实施例1
在200℃下热处理含有硫化锂的溶液
将含有硫化锂的、锂含量为大约3重量%的水溶液在具有循环空气的炉中以10 K/min的加热速率加热到200℃，其中min是分钟的缩写。在达到预定温度之后，将样品在预定温度下在连续的循环空气中保持1 h。将废气通过填充有碱性洗涤液的气体洗涤器而排出。通过X射线衍射（XRD）的相分析，将固体鉴定为氢氧化锂。分离的产率为91％。
实施例2
在500℃下热处理含有硫化锂的溶液
将含有硫化锂的、锂含量为大约3重量%的水溶液在具有循环空气的炉中以5 K/min的加热速率加热到500℃。在达到预定温度之后，将样品在预定温度下在连续的循环空气中保持1 h。将废气通过填充有碱性洗涤液的气体洗涤器而排出。残余物的主要相由氢氧化锂组成，次要相通过X射线衍射鉴定为3 LiOH x Li2SO4。分离的产率为77％。
实施例3
通过化学氧化从含有硫化锂的溶液中获得Li2SO4
将20 g的含有硫化锂的、锂含量为大约3重量%的水溶液在可调温的玻璃反应器中冷却到0℃。在稳定的搅拌下，向该冷却的溶液中在20 min内加入40 g的半浓缩的过氧化氢溶液（15重量%）。由于剧烈放热的反应，观察到温度升高到60℃。在1小时的搅拌之后，将该溶液浓缩并且干燥至恒重。通过X射线衍射的相分析，将固体鉴定为硫酸锂，其以Li2SO4和Li2SO4x H2O的形式存在。分离的产率为91％。
实施例4
通过碳酸盐沉淀从含有硫化锂的溶液中获得Li2CO3
在反应器中预先加入20 g的含有硫化锂的、锂含量为大约3重量%的水溶液。在稳定的搅拌下，将该含锂的溶液与11.5 g的碳酸钠混合。将获得的悬浮液离心分离，并且将沉淀物在80℃下干燥至恒重。通过X射线衍射的相分析，将固体鉴定为碳酸锂。分离的产率为92％。
实施例5
通过酸性处理从含有硫化锂的溶液中获得LiCl
在可调温的反应器中预先加入20 g的含有硫化锂的、锂含量为大约3重量%的水溶液。该反应器装配有蒸馏单元以及配料单元。通过废气管线连接具有碱性洗涤水溶液的气体洗涤器。在稳定的搅拌下，通过配料***在10分钟内将21.2 g的半浓缩的盐酸（15重量%）计量加入。将该混合物浓缩至干燥，并且将产物干燥至恒重。
通过X射线衍射的相分析，将获得的固体鉴定为氯化锂，其以LiCl和LiCl x H2O的形式存在。分离的产率为84％。

Claims (11)

1.从锂-硫-蓄电池中回收锂的方法，其特征在于，将所述蓄电池放电、弄碎和通过筛分或筛选预清理以分离壳体和集流体部分，将剩余的材料分散在水性介质中，将不溶性成分通过过滤除去和将电解质通过相分离除去，接着进行用于从剩余的滤液中分离锂的方法。
2.根据权利要求1的方法，其特征在于，所述水性介质的 pH值≥7。
3.根据权利要求1或2的方法，其特征在于，通过热处理从滤液中分离锂。
4.根据权利要求1或2的方法，其特征在于，通过化学氧化从滤液中分离锂。
5.根据权利要求1或2的方法，其特征在于，通过在酸性条件下的处理从滤液中分离锂。
6.根据权利要求1或2的方法，其特征在于，通过沉淀从滤液中分离锂。
7.根据权利要求3的方法，其特征在于，所述热处理在100至1500℃的温度范围内在氧的存在下进行。
8.根据权利要求3的方法，其特征在于，所述热处理在100至1500℃的温度范围内在排除氧的情况下进行。
9.根据权利要求4的方法，其特征在于，所述化学氧化通过与过氧化氢、臭氧或羟基自由基的反应而进行。
10.根据权利要求5的方法，其特征在于，所述在酸性条件下的处理通过添加硫酸或盐酸进行，将含有的锂转移到相应的盐中和将形成的多硫化合物通过萃取分离。
11.根据权利要求6的方法，其特征在于，通过添加水溶性的碳酸盐而使锂从滤液中沉淀出。
CN201580058207.7A 2014-10-31 2015-11-02 从锂‑硫‑蓄电池中回收锂的方法 Pending CN107109516A (zh)

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