CN103752259A - 用于去除放射性锶的硅基钛酸盐复合吸附剂及其制备方法 - Google Patents

用于去除放射性锶的硅基钛酸盐复合吸附剂及其制备方法 Download PDF

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CN103752259A
CN103752259A CN201410002637.4A CN201410002637A CN103752259A CN 103752259 A CN103752259 A CN 103752259A CN 201410002637 A CN201410002637 A CN 201410002637A CN 103752259 A CN103752259 A CN 103752259A
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titanate
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吴艳
韦悦周
陈梓
三村均
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Shanghai Jiaotong University
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Abstract

本发明属于放射性元素处理技术领域，具体为一种用于去除放射性锶的硅基钛酸盐复合吸附剂及其制备方法。本发明中的复合吸附剂以多孔性的颗粒状二氧化硅为载体，钛酸盐负载于所述二氧化硅微孔道里；其中：所述二氧化硅载体粒径大小为30～600μm，孔径大小为10～600nm，孔隙率为20～80%；钛酸盐的负载率为2～80%。上述复合吸附剂通过溶胶-凝胶法制备，其制备方法简单，本发明所述的复合吸附剂对锶的吸附选择性好，吸附速度快，吸效率高，二次废物少，适合于各种含锶放射性废水的高效处理。

Description

用于去除放射性锶的硅基钛酸盐复合吸附剂及其制备方法
技术领域
本发明属于放射性元素处理技术领域，具体涉及一种去除放射性锶用硅基钛酸盐复合吸附剂及其制备方法。
背景技术
中国的核电事业正处于一个高速发展的时期，在享受核电给社会经济进步带来巨大贡献的同时，能够有效处理其产生的放射性废水是迫切需要解决的问题。90Sr是存在于放射性废水中的一种高释热核素，其半衰期为28.6年，放射强度大，是放射性废水中主要放射性和释热的来源之一。在放射性废液最终处置之前，必须针对性地将其去除。
对于放射性废水中90Sr的去除，主要的技术手段有溶剂萃取法和离子交换法。溶剂萃取法采用大环超分子化合物如冠醚类，通过分子识别作用选择性的分离锶。然而，此类化合物合成成本高，使用时需要大量的稀释剂和洗涤剂，导致大量有机废液的产生，增大处理难度。
离子交换方法处理锶，效率高，二次废液少，设备简单且便于操作，即使对于微量的放射性，也能够高效的去除。离子交换剂包括有机离子交换树脂和无机离子交换剂。与有机离子交换树脂相比较无机离子交换剂，具有明显的离子交换容量大，耐辐照，易于固化处理等特点。常用除锶无机离子交换剂是沸石类吸附剂。然而，该类吸附剂的吸附速率慢，吸附性能受高酸高盐分环境的影响大，会增大二次废物的产生量。此外，锑酸盐、钛酸盐类的无机离子交换剂对锶的吸附效果好，但由于这类材料是微晶状结构，机械性能较差，不适合应用于工业规模的高流速柱子操作。（高晓雷，郭探，张慧芳，李权，叶秀深，吴志坚.吸附法分离提取锶的研究进展[J].中国矿业,2011,20(12):103-107.）。
发明内容
针对上述的技术难点，本发明的目的是提供一种去除放射性锶用硅基钛酸盐复合吸附剂及其制备方法。本发明制备方法简单，得到的复合吸附剂具有对锶的选择性好，吸附速率快，离子交换容量大和处理效率高等特点。
本发明采用的技术方案具体描述如下。
本发明提供一种用于去除放射性锶的硅基钛酸盐复合吸附剂，该复合吸附剂由多孔二氧化硅和负载的无机离子交换剂复合而成；无机离子交换剂负载于所述二氧化硅微孔道里；无机离子交换剂的负载率为2～80%。本发明中，无机离子交换剂为钛酸盐，所述的二氧化硅载体为多孔性颗粒状，粒径大小为30～600μm，孔径大小为10～600nm，孔隙率为20～80%。
所述的钛酸盐为K2Ti6O13，K2Ti4O9，K2Ti2O5，Na2Ti6O13，Na2Ti4O9或Na2Ti2O5中的一种或几种。
所述的二氧化硅载体为多孔性颗粒状，粒径为50～100μm，孔径为50nm，孔隙率为60～70%；所述的无机离子交换剂的负载率为25～70%。
本发明还提供一种用于去除放射性锶的硅基钛酸盐类复合吸附剂的制备方法，其以多孔二氧化硅为载体，通过溶胶凝胶法将去除锶的钛酸盐负载到二氧化硅微孔道里，制得复合吸附剂。具体步骤如下：
将二氧化硅载体、有机钠盐或有机钾盐和钛酸四丁酯溶解于稀释剂中，搅拌3～4小时，蒸发去除稀释剂后，用蒸馏水或乙醇清洗二氧化硅表面，在400～1100℃高温下烧结制得复合吸附剂；二氧化硅与钛酸四丁酯的重量比为1：（0.5～50）。
所述的有机钠盐或有机钾盐和钛酸四丁酯的摩尔比为1:（1～10）。
所述的有机钠盐或有机钾盐和钛酸四丁酯的摩尔比为1:（1～3）；二氧化硅与钛酸四丁酯的重量比为1：（1.7～5.1）。
所述的有机钠盐为醋酸钠和硝酸钾；所述的有机钾盐为醋酸钾和硝酸钠。
所述的稀释剂选自乙二醇甲醚、乙酸或酒精中任一种。
本发明的有益效果在于：
（1）本发明提供的硅基钛酸盐类复合吸附剂，粒径小孔径大，使得离子交换扩散的距离大大缩小，吸附速度快，处理效率高；
（2）使用多孔性的二氧化硅作为载体，使得复合吸附剂的机械强度高，适合使用工业规模的处理流程；
（3）合成方法简单，步骤少，可在通用设备中完成，具有良好的经济效益。
附图说明
图1在不同时间下K2Ti6O13硅基钛酸盐复合吸附剂对锶的吸附。
图2在不同pH下K2Ti6O13硅基钛酸盐复合吸附剂对锶、铯、钙和镁的吸附。
图3在不同时间下Na2Ti4O9硅基钛酸盐复合吸附剂对锶的吸附。
图4在不同pH下Na2Ti4O9硅基钛酸盐复合吸附剂对锶、铯、钙和镁的吸附。
具体的实施方式
下面结合具体实施例，进一步阐述本发明。应理解，这些实施例仅用于说明本发明而不用于限制本发明的范围。此外应理解，在阅读了本发明讲授的内容之后，本领域技术人员可以对本发明作各种改动或修改，这些等价形式同样落于本申请所附权利要求书所限定的范围。
实施例1
将10g二氧化硅（二氧化硅为多孔性球状颗粒，平均粒径为50μm，孔径为50nm，孔隙率为60～70%，日本理工科学株式会社生产）、0.05mol的醋酸钾、0.15mol的钛酸四丁酯溶于乙二醇甲醚中，充分溶解搅拌3小时，蒸发干燥后，用蒸馏水清洗二氧化硅表面，预制的粉末在马弗炉中1100℃温度下烧结，钛酸盐在二氧化硅的纳米孔道中结晶，得到复合吸附剂，并在室温保存。
本实例得到的硅基钛酸盐复合吸附剂，孔径为10～25nm。合成的钛酸盐为K2Ti6O13，其负载率为50～70%。
实施例2
将10g二氧化硅（二氧化硅为多孔性球状颗粒，平均粒径为50μm，孔径为50nm，孔隙率为60～70%，日本理工科学株式会社生产）、0.05mol的醋酸钠、0.1mol的钛酸四丁酯溶于酒精中，充分溶解搅拌4小时，蒸发干燥后，用乙醇清洗二氧化硅表面，预制的粉末在马弗炉中800℃温度下烧结，钛酸盐在二氧化硅的纳米孔道中结晶，得到复合吸附剂，并在室温保存。
本实例得到的硅基钛酸盐复合吸附剂，孔径为10～30nm。合成的钛酸盐为Na2Ti4O9，其负载率为40～60%。
实施例3
将10g二氧化硅（二氧化硅为多孔性球状颗粒，平均粒径为100μm，孔径为50nm，孔隙率为60～70%，日本理工科学株式会社生产）、0.05mol的醋酸钾、0.05mol的钛酸四丁酯溶于乙酸中，充分溶解搅拌4小时，蒸发干燥后，用蒸馏水或乙醇清洗二氧化硅表面，预制的粉末在马弗炉中400℃温度下烧结，钛酸盐在二氧化硅的纳米孔道中结晶，得到复合吸附剂，并在室温保存。
本实例得到的硅基钛酸盐复合吸附剂，孔径为15～35nm。合成的钛酸盐为K2Ti2O5，其负载率为25～30%。
应用实例1
将实例1中制备的复合吸附剂0.1g与5ml锶浓度为20ppm的溶液充分混合，置于恒温振荡器中，分别振荡2min，5min，10min，20min，30min,40min,60min后，固液分离，用ICP测试剩余锶的浓度，计算在不同时间下，锶的吸附率。
由图1可知，复合吸附剂对锶的吸附速率非常快，吸附动力学非常好，基本上在2min之内就可以达到平衡，同时吸附效率可达到100%。由此可见，此吸附剂有望应用于放射性废水的处理工艺，提高处理效率，减少二次废物。
应用实例2
将实例1中制备的样品0.1g与5ml含锶、铯、钙、镁离子浓度为20ppm不同pH的溶液充分混合，置于恒温振荡器中，达到吸附平衡后，固液分离，用ICP和原子吸收光度计测试剩余溶液中的锶、铯、钙和镁离子浓度。铯、钙、镁是为了模拟海水系的核事故废水中的共存离子，从而考察此复合吸附剂对锶的吸附选择性。
由图2可知，复合吸附剂在不同pH的锶、铯、钙、镁离子混合体系中，随着pH的升高，复合吸附剂对各离子的吸附性能增强。在pH5～6的范围下，对各离子吸附性能的顺序为锶>>铯,钙>镁，复合吸附剂对锶的吸附远远大于其他离子，对锶的吸附选择性好，且吸附效率几乎达到100%。上述反应是通过离子交换反应进行，反应方程式如下：M为金属离子。由此可见，此复合吸附剂对锶有着较好的优先吸附能力，有望实现放射性废水中的锶的去除。
应用实例3
将实例2中制备的样品0.1g与5ml锶浓度为20ppm的溶液充分混合，置于恒温振荡器中，分别振荡5min，10min，20min，30min,40min,60min后，固液分离，用ICP测试剩余锶的浓度，计算在不同时间下，锶的吸附效率。
由图3可知，实例2中制备的样品对锶的吸附速率同样也是非常快，吸附动力学非常好，基本上在5min之内就可以达到平衡。
应用实例4
将实例2中制备的样品0.1g与5ml含锶、铯、钙、镁离子浓度为20ppm不同pH的溶液充分混合，置于恒温振荡器中，达到吸附平衡后，固液分离，用ICP和原子吸收光度计测试剩余溶液中的锶、铯、钙和镁离子浓度。考察了不同形态的钛酸盐在模拟海水系的核事故中，吸附剂对锶的吸附性能。实验结果如图3所示。
图3可知，复合吸附剂在不同pH的锶、铯、钙、镁离子混合体系中，随着pH的升高，复合吸附剂对各离子的吸附性能增强。在pH5～6的范围下，同样的，对各离子吸附效率的顺序为锶>铯,钙>镁，此吸附剂同样也表现出对锶较好的选择性。
综上所述，钛酸盐复合吸附剂在低酸度下能够比较优异的吸附和选择性能，非常优越的吸附动力学性能，未来可以在处理放射性的废水中发挥极大的优势。

Claims (8)

1.一种用于去除放射性锶的硅基钛酸盐复合吸附剂，其特征在于：其以多孔性的颗粒状二氧化硅为载体，钛酸盐负载于所述二氧化硅微孔道里；其中：所述二氧化硅载体粒径为30～600μm，孔径为10～600nm，孔隙率为20～80%；钛酸盐的负载率为2～80%。
2.根据权利要求1所述的硅基钛酸盐复合吸附剂，其特征在于：所述钛酸盐为K2Ti6O13，K2Ti4O9，K2Ti2O5，Na2Ti6O13，Na2Ti4O9或Na2Ti2O5中的一种或者几种。
3.根据权利要求1所述的硅基钛酸盐复合吸附剂，其特征在于：所述二氧化硅载体粒径为50～100μm，孔径为50nm，孔隙率为60～70%。
4.根据权利要求1所述的硅基钛酸盐复合吸附剂，其特征在于：所述钛酸盐的负载率为25～70%。
5.一种用于去除放射性锶的硅基钛酸盐复合吸附剂的制备方法，其特征在于，具体步骤如下：将二氧化硅载体、有机钠盐或有机钾盐和钛酸四丁酯溶解于稀释剂中，搅拌3～4小时，蒸发去除稀释剂后，用蒸馏水或乙醇清洗二氧化硅表面，在400～1100℃高温烧结制得复合吸附剂；其中有机钠盐或有机钾盐和钛酸四丁酯的摩尔比为1:（1～10），二氧化硅与钛酸四丁酯的重量比为1：（0.5～50）。
6.根据权利要求5所述的制备方法，其特征在于：所述有机钠盐或有机钾盐和钛酸四丁酯的摩尔比为1：（1～3），二氧化硅与钛酸四丁酯的重量比为1：（1.7～5.1）。
7.根据权利要求5所述的制备方法，其特征在于：所述的有机钠盐为醋酸钠和硝酸钾；所述的有机钾盐为醋酸钾和硝酸钠。
8.根据权利要求5所述的制备方法，其特征在于：所述的稀释剂为乙二醇甲醚、乙酸或酒精中任一种。
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