CN106915797A - 一种氯金酸辅助复合光催化剂降解罗丹明b的方法 - Google Patents
一种氯金酸辅助复合光催化剂降解罗丹明b的方法 Download PDFInfo
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Abstract
本发明属于光催化环境净化领域，特指一种氯金酸辅助复合光催化剂降解罗丹明B的方法。以Co3O4/NaTaO3纳米块为光催化剂，在罗丹明B溶液中加入少量的氯金酸(HAuCl4)溶液，在可见光下照射30分钟，罗丹明B降解率能达到78％。
Description
技术领域
本发明属于光催化环境净化领域。以Co3O4/NaTaO3纳米块为光催化剂，在罗丹明B溶液中加入少量的氯金酸(HAuCl4)溶液，在可见光下照射30分钟，罗丹明B降解率能达到78％。
背景技术
随着工业化和城镇化进程的快速推进，大量具有致癌性和神经毒性的有机染料废水被排入自然界，严重危害着人类的身体健康，也制约着经济的可持续发展。传统污水处理的方法主要有：物理法、生物降解法及化学法，但效果不理想。近些年发展的半导体光催化技术是一种先进的氧化技术，它是将半导体催化剂与某些光源结合共同作用于废水进行催化降解，相对于传统废水处理技术具有高效节能，且能彻底消除废水中绝大部分有机物的优点，因此受到环境及材料研究者们的广泛重视。钽酸钠(NaTaO3)半导体具有对环境无毒性，良好的稳定性和优异的光催化活性，在环境保护中有着广阔的应用，如空气净化，水消毒和净化等。但是钽酸钠存在着无法响应可见光的缺陷，与窄带隙的四氧化三钴(Co3O4)形成p-n异质结可以有效地响应可见光。本发明中，以Co3O4/NaTaO3纳米块为光催化剂，加入一定量的氯金酸为引发剂，对罗丹明B溶液在可见光下进行降解研究。
发明内容
本发明是一种以Co3O4/NaTaO3纳米块为光催化剂，加入少量氯金酸为引发剂在可见光下降解罗丹明B的方法。
本发明通过以下步骤实现：
(1)取钽酸钠纳米块，加入到乙酸钴溶液中，再加入浓氨水搅拌使混合均匀，搅拌结束后，将分散体系置于聚四氟乙烯内衬中，水热条件下150℃反应三小时，移出上层清液，将沉淀清洗、烘干后得到Co3O4/NaTaO3复合光催化剂，其中Co3O4为NaTaO3质量的5-40％。
所述乙酸钴溶液的浓度为1mmol/L
所述浓氨水的浓度为25wt％，浓氨水与乙酸钴溶液的体积比为16:25。
所述Co3O4为NaTaO3的质量的10％(优选)。
(2)将Co3O4/NaTaO3纳米块放入到盛有罗丹明B溶液的光反应瓶中，将光反应瓶置于暗处，在搅拌下保持30分钟，同时打开循环冷凝水，保持在室温。然后将氯金酸溶液滴加到光反应瓶中，并打开光源，进行光催化实验。每隔6min取出4mL溶液放入到5毫升离心管中，经过离心，取上清液用于总有机碳含量分析。
所述Co3O4/NaTaO3纳米块、罗丹明B溶液、氯金酸溶液的比例为：100mg：100mL：1040μL。
所述罗丹明B溶液的浓度为10mg/L。
所述氯金酸溶液浓度为3.3mg/L。
本发明区别于现有的光催化降解流程是通过在光降解罗丹明B开始前滴加少量的氯金酸作引发剂，在添加氯金酸溶液之后，罗丹明B分子富集在Co3O4/NaTaO3光催化剂表面，同时氯金酸在Co3O4/NaTaO3光催化剂表面被光还原成金纳米粒子，在金纳米粒子的Surfaceplasmon resonance(SPR)效应和Co3O4与NaTaO3异质结协调提升下，使得罗丹明B被快速降解。
附图说明
图1为所制备的Co3O4/NaTaO3复合光催化剂的XRD衍射谱图；其中，用“#”表示Co3O4的峰，用“*”表示NaTaO3的峰。
图2(a)为所制备Co3O4/NaTaO3复合光催化剂的扫描电镜照片；(b)为透射电镜图。
图3为所制备Co3O4/NaTaO3复合光催化剂的X光电子能谱图。
图4(a)为所制备不同比例的Co3O4/NaTaO3复合光催化剂的可见光催化降解罗丹明B溶液的降解率图和(b)最佳比例的Co3O4/NaTaO3在氯金酸辅助下的总有机碳量-时间关系图。
具体实施方式
实施例1 Co3O4/NaTaO3复合光催化剂的制备
一定量的钽酸钠纳米立方块和16mL浓氨水(25wt％)分别加入到25mL 1mM的乙酸钴水溶液中,磁力搅拌30min，然后转移至50mL聚四氟乙烯内衬，装釜后150℃水热反应三小时。反应结束后，移除上层清液，将所得产物用去离子水洗净，过滤，恒温干燥箱中60℃烘干。钽酸钠纳米立方块的添加量使得最终生成的Co3O4/NaTaO3复合光催化剂中，Co3O4质量占NaTaO3质量的百分比分别为5％、10％、20％、40％。
实施例2 Co3O4/NaTaO3复合光催化剂的表征分析
如图1所示，从图中可以看出明显的Co3O4和NaTaO3的特征峰，且随着Co3O4量的增加，Co3O4特征峰逐渐增强，NaTaO3的特征峰逐渐减弱，说明我们成功制备出了负载比例不同的Co3O4/NaTaO3复合光催化剂。
如图2所示，(a)图中可以Co3O4/NaTaO3为纳米块；(b)图中Co3O4纳米粒子负载在NaTaO3纳米块表面。
如图3所示，图中可以清楚看到Co3O4/NaTaO3的X-射线光电子能谱图(XPS)：(a)Ta4f,(b)Co2p,证明样品中包含Ta,Co元素。
实施例3 Co3O4/NaTaO3等离子体纳米复合光催化剂的可见光催化活性实验
(1)配制浓度为10mg/L的罗丹明B溶液，将配好的溶液置于暗处。
(2)称取Co3O4/NaTaO3复合光催化剂100mg，分别置于光催化反应器中，加入100mL步骤(1)所配好的目标降解液，磁力搅拌30min待复合光催化剂分散均匀后，加入1040μL、浓度为3.3mg/L的氯金酸溶液，打开水源，光源，进行光催化降解实验。
(3)每6min吸取反应器中的光催化降解液，离心后用于紫外可见光谱和总有机碳量分析的测量。
(4)如图4(a)为不同负载比例的Co3O4/NaTaO3在可见光下降解罗丹明B的降解率图和10％Co3O4/NaTaO3在氯金酸辅助下的总有机碳量-时间关系图。如图所示，在没有氯金酸辅助的情况下，Co3O4/NaTaO3降解罗丹明B的速率非常慢，当选取10％Co3O4/NaTaO3在氯金酸辅助下其降解速率得到显著提升，平均速率大约提升40倍。
Claims (5)
1.一种氯金酸辅助复合光催化剂降解罗丹明B的方法，其特征在于：以Co3O4/NaTaO3纳米块为复合光催化剂，加入氯金酸为引发剂在可见光下降解罗丹明B。
2.如权利要求1所述的一种氯金酸辅助复合光催化剂降解罗丹明B的方法，其特征在于，具体步骤如下：
(1)取钽酸钠纳米块，加入到乙酸钴溶液中，再加入浓氨水搅拌使混合均匀，搅拌结束后，将分散体系置于聚四氟乙烯内衬中，水热条件下150℃反应三小时，移出上层清液，将沉淀清洗、烘干后得到Co3O4/NaTaO3复合光催化剂，其中Co3O4为NaTaO3质量的5-40％；
(2)将Co3O4/NaTaO3纳米块放入到盛有罗丹明B溶液的光反应瓶中，将光反应瓶置于暗处，在搅拌下保持30分钟，同时打开循环冷凝水，保持在室温，然后将氯金酸溶液滴加到光反应瓶中，并打开光源，进行光催化降解。
3.如权利要求2所述的一种氯金酸辅助复合光催化剂降解罗丹明B的方法，其特征在于，步骤(1)中，所述乙酸钴溶液的浓度为1mmol/L；所述浓氨水的浓度为25wt％，浓氨水与乙酸钴溶液的体积比为16:25。
4.如权利要求2所述的一种氯金酸辅助复合光催化剂降解罗丹明B的方法，其特征在于，所述Co3O4为NaTaO3的质量的10％。
5.如权利要求2所述的一种氯金酸辅助复合光催化剂降解罗丹明B的方法，其特征在于，所述Co3O4/NaTaO3纳米块、罗丹明B溶液、氯金酸溶液的比例为：100mg：100mL：1040μL；所述罗丹明B溶液的浓度为10mg/L；所述氯金酸溶液浓度为3.3mg/L。
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