CN104157892B - 一种全钒液流电池的硫酸氧钒电解液除磷方法 - Google Patents
一种全钒液流电池的硫酸氧钒电解液除磷方法 Download PDFInfo
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Abstract
一种全钒液流电池的硫酸氧钒电解液除磷方法，经钒渣及石煤浸出、反萃取、树脂解析所得硫酸氧钒溶液经多级逆流萃取除杂后，硫酸氧钒浓度为0.5~2.0mol/L，含杂质磷常大于20mg/L，其特征是以下步骤组成：过滤多级逆流萃取除杂后的硫酸氧钒溶液，以转速200~400rpm搅拌滤液，搅拌时间10~60min，搅拌后溶液静置60~150min；静置后的溶液以转速为3000~5000rpm离心处理5~20min；将离心后的清液导入填充吸附介质的吸附柱吸附除磷。本发明提供一种全钒液流电池的硫酸氧钒电解液的除磷方法，可去除硫酸氧钒电解液所含的磷，能有效提高电解液的综合电性能。该方法工艺简单，成本低廉，可实现规模生产。
Description
技术领域
本发明涉及一种电池电解液的除磷方法，特别全钒液流电池的硫酸氧钒电解液的除磷方法。
背景技术
全钒氧化还原液流电池是一种优秀的储能装置。该电池容量取决于电解液的量和钒离子浓度，电解液可以与电池分开放置，电池寿命长，可靠性高，可快速充放电。在光伏发电、风力发电、削峰填谷等方面有很大发展前景。全钒液流电池没有固态反应，电池非常稳定，可以反复充电2万次，性能几乎不受影响，寿命估计长达几十年。
硫酸氧钒电解液是钒电池电化学反应的活性物质和电能的载体，是全钒液流电池的关键材料，对电池性能有直接影响。硫酸氧钒电解液的制取和提纯过程中，磷元素是易进入且难分离的非金属杂质之一，磷元素在硫酸氧钒电解液中存在形式较复杂，以磷酸根形式存在的磷来自含钒原料，以有机磷形式的磷，来自硫酸氧钒溶液萃取提纯过程中萃取剂分离不彻底的夹杂所带入。
吸附法是去除低含量磷的方法之一，各种功能优良的无机吸附剂、生物吸附剂正被不断发现。
CN200910094605.0公开了以石煤为原料，酸性浸出，浸出液还原中和后，萃取和反萃取制得硫酸氧钒富集溶液，蒸发脱水得到硫酸氧钒。该方法未提及如何深度去除硫酸氧钒萃取过程所夹带的有机磷。
CN101428922公开了一种从污水中除磷的方法，采用高铁酸盐氧化工艺和光化工艺处理工业污水或生活污水，使达到国家排放标准，该方法因引入高铁酸盐进入水体中，不适合去除硫酸氧钒电解液中低含量的磷。
发明内容
本发明的目的是提供一种全钒液流电池的硫酸氧钒电解液的除磷方法，本发明的方法可去除硫酸氧钒电解液所含的磷，能有效提高电解液的综合电性能。
经钒渣及石煤浸出、反萃取、树脂解析所得硫酸氧钒溶液经多级逆流萃取除杂后，硫酸氧钒浓度为0.5~2.0mol/L，含金属杂质量已经达到电解液性能指标要求，含磷量大于20mg/L，去除该硫酸氧钒溶液所含的磷，能进一步提高钒电池的储能效率和循环充放电性能。
本发明的方法由以下步骤组成：过滤多级逆流萃取除杂后的硫酸氧钒溶液，以转速200~400rpm搅拌滤液，搅拌时间10~60min，搅拌后溶液静置60~150min；静置后的溶液以转速为3000~5000rpm离心处理5~20min；将离心后的清液导入填充吸附介质的吸附柱吸附除磷。
本发明的吸附介质是将医用脱脂棉用75%酒精溶液浸泡2小时后，再用0.5mol/L的硫酸铵溶液或硫酸钠溶液浸泡24小时，烘干后用纯水洗涤两遍，装入吸附柱。当吸附介质吸附磷的量达到饱和时，取出用30~60℃的碳酸钠或醋酸钠溶液溶液浸泡再生，循环使用。
过滤溶液初步分离硫酸氧钒溶液中所含残留有机相。利用机械力搅动溶液，产生气浮过程，解决硫酸氧钒溶液中磷及其它杂质的机械夹杂问题。静置后，离心分离硫酸氧钒溶液是利用离心机的旋转离心作用破坏溶液的微乳化问题。离心过程中不会再次引入新的杂质，充分保证溶液中残留的有机相与水相彻底分开，解决微量有机相残留而导致溶液含有机磷问题。离心后，离心后的清液导入吸附柱，利用吸附介质有效吸附溶液中的磷。
本发明以经多段萃取及反萃取所获得的硫酸氧钒溶液为对象，通过过滤、搅拌、静置、离心以及吸附等过程去除硫酸氧钒溶液中存在的磷，该方法工艺简单，成本低廉，可实现规模生产。
具体实施方式
实施例1
取1000ml浓度为1.0mol/L经多级萃取反萃取纯化后的硫酸氧钒溶液，该溶液不含铁、锰、铬、铝、钛、镁和钙等金属杂质，含磷量为30mg/L。用低速滤纸过滤硫酸氧钒溶液，滤液转入烧杯中搅拌30分钟，搅拌速度为350rpm，搅拌完毕静置90分钟。将静置后的溶液放入台式低速离心机离心，离心机转速为3000rpm，离心时间为10分钟。将医用脱脂棉用75%酒精溶液浸泡2小时后，再用0.5mol/L的硫酸铵溶液浸泡24小时，烘干后用纯水洗涤两遍，装入玻璃管吸附柱，由上部导入离心后的清液吸附除磷，最终得到980ml硫酸氧钒电解液，含磷量0.8mg/L，过程中磷的去除率大于97%。
实施例2
取500ml浓度为1.5mol/L经多级萃取反萃取纯化后的硫酸氧钒溶液，该溶液不含铁、锰、铬、铝、钛、镁和钙等金属杂质，含磷量为42mg/L。用中速滤纸过滤硫酸氧钒溶液，滤液转入烧杯中搅拌40分钟，搅拌速度为300rpm，搅拌完毕静置120分钟。将静置后的溶液放入台式低速离心机离心，离心机转速为4000rpm，离心时间为12分钟。将医用脱脂棉用75%酒精溶液浸泡2小时后，再用0.5mol/L的硫酸钠溶液浸泡24小时，烘干后用纯水洗涤两遍，装入玻璃管吸附柱，串联组装成两个吸附柱，由上部导入离心后的清液吸附除磷，经过一次除磷的溶液再经过第二个吸附柱，最终得到480ml硫酸氧钒电解液，含磷量0.9mg/L，过程中磷的去除率大于97%。
Claims (1)
1.一种全钒液流电池的硫酸氧钒电解液除磷方法，经钒渣及石煤浸出、反萃取、树脂解析所得硫酸氧钒溶液经多级逆流萃取除杂后，硫酸氧钒浓度为0.5~2.0mol/L，含杂质磷常大于20mg/L，其特征是以下步骤组成：过滤多级逆流萃取除杂后的硫酸氧钒溶液，以转速200~400rpm搅拌滤液，搅拌时间10~60min，搅拌后溶液静置60~150min；静置后的溶液以转速为3000~5000rpm离心处理5~20min；将离心后的清液导入填充吸附介质的吸附柱吸附除磷；所述吸附介质是将医用脱脂棉用75%酒精溶液浸泡2小时后，再用0.5mol/L的硫酸铵溶液或硫酸钠溶液浸泡24小时，烘干后用纯水洗涤两遍，装入吸附柱。
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