CN107088403A - 一种氨基硫脲键合PDA@MWCNTs吸附剂及其制备方法和应用 - Google Patents
一种氨基硫脲键合PDA@MWCNTs吸附剂及其制备方法和应用 Download PDFInfo
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Abstract
本发明公开了一种氨基硫脲键合PDA@MWCNTs吸附剂及其制备方法和应用，属于复合吸附材料技术领域。本发明的技术方案要点为：一种氨基硫脲键合PDA@MWCNTs吸附剂，是通过用双氧水氧化聚多巴胺并进一步与氨基硫脲键合制得的。本发明还具体公开了该氨基硫脲键合PDA@MWCNTs吸附剂的制备方法及其从废弃电路板金属富集体王水浸出液中分离富集金的应用。本发明制备过程条件温和且操作简单，制得的氨基硫脲键合PDA@MWCNTs吸附剂吸附速率快、吸附量大且选择性强，适用于从废弃电路板金属富集体王水浸出液等复杂含金溶液中分离富集金。
Description
技术领域
本发明属于复合吸附材料技术领域，具体涉及一种氨基硫脲键合PDA@MWCNTs吸附剂及其制备方法和应用。
背景技术
随着对纳米材料研究的深入，人们发现多壁碳纳米管作为载体具有诸多优势，除了良好的耐腐蚀、耐热和抗高温等特性，其本身特有的结构又赋予了多壁碳纳米管在光学、力学、电学、热学、吸附等方面的优良性能，并得到广泛应用。但由于多壁碳纳米管表面惰性及其疏水性，影响了多壁碳纳米管的分散性能，一定程度上妨碍了其进一步应用，因此对多壁碳纳米管表面进行改性修饰显得尤为重要。改性不仅可提高多壁碳纳米管的分散性，而且可通过引入活性官能团提高其选择性。多巴胺在弱碱性pH条件下能够氧化自聚合生成粘着的黑色聚多巴胺涂层，使材料表面活性官能团数量增多，表面形貌变得粗糙且亲水性变好。
发明内容
本发明解决的技术问题是提供了一种氨基硫脲键合PDA@MWCNTs吸附剂及其制备方法，该方法通过用双氧水氧化聚多巴胺并进一步与氨基硫脲键合制得新型 TSC-PDA@MWCNTs吸附剂，制备过程条件温和且操作简单，制得的TSC-PDA@MWCNTs 吸附剂吸附速率快、吸附量大且选择性强，适用于从废弃电路板金属富集体王水浸出液等复杂含金溶液中分离富集金。
本发明为解决上述技术问题采用如下技术方案，一种氨基硫脲键合PDA@MWCNTs吸附剂的制备方法，其特征在于具体步骤为：
(1)PDA@MWCNTs的合成
称取400mg盐酸多巴胺溶于200mL pH为8.5的Tris-HCl缓冲溶液中，再称取200mg多壁碳纳米管加入到上述溶液中，在有氧条件下室温磁力搅拌24h，反应后的产物用无水乙醇反复洗涤多次，抽滤，放入真空干燥箱中于50℃烘干12h，产物记作PDA@MWCNTs；
(2)PDA@MWCNTs的氧化
称取250mg PDA@MWCNTs加入到50mL 1wt％的双氧水溶液中，在室温下磁力搅拌13h，反应后的产物用超纯水反复洗涤多次，抽滤，放入真空干燥箱中于50℃烘干12h，产物记作O-PDA@MWCNTs；
(3)氨基硫脲键合PDA@MWCNTs吸附剂的合成
将2g氨基硫脲加入到100mL Tris-HCl缓冲溶液中，水浴加热溶解后冷却至室温，然后加入200mg O-PDA@MWCNTs，在室温下磁力搅拌13h，反应后的产物用超纯水反复洗涤多次，抽滤，放入真空干燥箱中于50℃烘干12h制得氨基硫脲键合PDA@MWCNTs吸附剂，产物记作TSC-PDA@MWCNTs。
所述的氨基硫脲键合PDA@MWCNTs吸附剂，其特征在于是由上述方法制备得到。
所述的氨基硫脲键合PDA@MWCNTs吸附剂用于选择性吸附溶液中的Au(III)。
所述的氨基硫脲键合PDA@MWCNTs吸附剂用于从废弃电路板金属富集体王水浸出液中选择性吸附Au(III)。
本发明制备过程条件温和且操作简单，制得的氨基硫脲键合PDA@MWCNTs吸附剂吸附速率快、吸附量大且选择性强，适用于从废弃电路板金属富集体王水浸出液等复杂含金溶液中分离富集金。
附图说明
图1是MWCNTs、PDA@MWCNTs和TSC-PDA@MWCNTs的红外谱图，三条红外谱图曲线区别显著，PDA@MWCNTs的红外谱图中观察到聚多巴胺的特征吸收峰， TSC-PDA@MWCNTs的红外谱图中可见氨基硫脲的特征吸收峰；
图2是PDA@MWCNTs和TSC-PDA@MWCNTs的热重曲线，在200-800℃范围内， TSC-PDA@MWCNTs重量损失明显高于PDA@MWCNTs，这表明氨基硫脲成功键合到 PDA@MWCNTs上；
图3是TSC-PDA@MWCNTs吸附金的动力学曲线，实验条件：50mL浓度为100mg/L 的Au(III)溶液，10mg吸附剂TSC-PDA@MWCNTs，温度30℃，振荡速率160rpm，由图可知，TSC-PDA@MWCNTs对金的吸附速度快，2h达到吸附平衡。
具体实施方式
以下通过实施例对本发明的上述内容做进一步详细说明，但不应该将此理解为本发明上述主题的范围仅限于以下的实施例，凡基于本发明上述内容实现的技术均属于本发明的范围。
实施例1
氨基硫脲键合PDA@MWCNTs吸附剂的合成
(1)PDA@MWCNTs的合成
称取400mg盐酸多巴胺溶于200mL pH为8.5的Tris-HCl缓冲溶液中，再称取200mg多壁碳纳米管加入到上述溶液中，在有氧条件下室温磁力搅拌24h，反应后的产物用无水乙醇反复洗涤多次，抽滤，放入真空干燥箱中于50℃烘干12h，产物记作PDA@MWCNTs；
(2)PDA@MWCNTs的氧化
称取250mg PDA@MWCNTs加入到50mL 1wt％的双氧水溶液中，在室温下磁力搅拌13h，反应后的产物用超纯水反复洗涤多次，抽滤，放入真空干燥箱中于50℃烘干12h，产物记作O-PDA@MWCNTs；
(3)氨基硫脲键合PDA@MWCNTs吸附剂的合成
将2g氨基硫脲加入到100mL Tris-HCl缓冲溶液中，水浴加热，溶解后冷却至室温，然后加入200mg O-PDA@MWCNTs，在室温下磁力搅拌13h，反应后的产物用超纯水反复洗涤多次，抽滤，放入真空干燥箱中于50℃烘干12h制得氨基硫脲键合PDA@MWCNTs 吸附剂，产物记作TSC-PDA@MWCNTs。
实施例2
表1是TSC-PDA@MWCNTs吸附选择性实验。选择以下二元混合体系进行吸附实验：Au(III)-Cu(II)，Au(III)-Pb(II)，Au(III)-Cd(II)，Au(III)-Cr(VI)，Au(III)-Zn(II)，Au(III)-Ni(II)， Au(III)-Co(II)，Au(III)-Mn(II)，Au(III)-Mg(II)。Au(III)和其它金属离子的浓度均为100mg/L，体积为50mL，10mg吸附剂TSC-PDA@MWCNTs，温度30℃，振荡速度160rpm，时间 2h。由表1可知，常见金属对吸附剂TSC-PDA@MWCNTs吸附金几乎没有干扰，而且在吸附剂TSC-PDA@MWCNTs上的吸附量也非常低。这说明吸附剂TSC-PDA@MWCNTs 对金吸附选择性强，抗干扰能力强。
表1 TSC-PDA@MWCNTs吸附选择性
实施例3
表2是TSC-PDA@MWCNTs从废弃电路板金属富集体王水浸出液中选择性吸附金实验。用王水溶解5g废弃电路板金属富集体，待溶解完全后移至电加热板上蒸发至干，冷却后加少量蒸馏水，过滤，将滤液定容至100mL。取该浸出液50mL，10mg吸附剂 TSC-PDA@MWCNTs，温度30℃，振荡速度160rpm，时间2h。由表2可知，金的吸附率达到73.8％，而其它共存金属吸附率都非常低。这说明吸附剂TSC-PDA@MWCNTs能从废弃电路板金属富集体王水浸出液中选择性吸附金。
表2 TSC-PDA@MWCNTs从废弃电路板金属富集体王水浸出液中选择性吸附金
以上实施例描述了本发明的基本原理、主要特征及优点，本行业的技术人员应该了解，本发明不受上述实施例的限制，上述实施例和说明书中描述的只是说明本发明的原理，在不脱离本发明原理的范围下，本发明还会有各种变化和改进，这些变化和改进均落入本发明保护的范围内。
Claims (4)
1.一种氨基硫脲键合PDA@MWCNTs吸附剂的制备方法，其特征在于具体步骤为：
（1）PDA@MWCNTs的合成
称取400mg盐酸多巴胺溶于200mL pH为8.5的Tris-HCl缓冲溶液中，再称取200mg多壁碳纳米管加入到上述溶液中，在有氧条件下室温磁力搅拌24h，反应后的产物用无水乙醇反复洗涤多次，抽滤，放入真空干燥箱中于50℃烘干12h，产物记作PDA@ MWCNTs；
（2）PDA@MWCNTs的氧化
称取250mg PDA@MWCNTs加入到50mL 1wt%的双氧水溶液中，在室温下磁力搅拌13h，反应后的产物用超纯水反复洗涤多次，抽滤，放入真空干燥箱中于50℃烘干12h，产物记作O-PDA@ MWCNTs；
（3）氨基硫脲键合PDA@MWCNTs吸附剂的合成
将2g氨基硫脲加入到100mL Tris-HCl缓冲溶液中，水浴加热溶解后冷却至室温，然后加入200mg O-PDA@MWCNTs，在室温下磁力搅拌13h，反应后的产物用超纯水反复洗涤多次，抽滤，放入真空干燥箱中于50℃烘干12h制得氨基硫脲键合PDA@MWCNTs吸附剂，产物记作TSC-PDA@ MWCNTs。
2.一种氨基硫脲键合PDA@MWCNTs吸附剂，其特征在于是由权利要求1所述的方法制备得到。
3.权利要求2所述的氨基硫脲键合PDA@MWCNTs吸附剂用于选择性吸附溶液中的Au（III）。
4.权利要求2所述的氨基硫脲键合PDA@MWCNTs吸附剂用于从废弃电路板金属富集体王水浸出液中选择性吸附Au（III）。
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| YILI XIE等: "Mussel inspired functionalization of carbon nanotubes for heavy metal ion removal", 《RSC ADVANCES》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109482149A (zh) * | 2019-01-10 | 2019-03-19 | 海南省辐射环境监测站 | 一种新型VOCs吸附材料及其对VOCs的吸附 |
| CN112537818A (zh) * | 2019-09-20 | 2021-03-23 | 席行正 | 使用硫脲石墨烯的回收金的方法 |
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| CN107088403B (zh) | 2019-11-05 |
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