CN113828328A - 一种AgFeO2/TiO2异质结光催化剂的制备方法及其应用 - Google Patents
一种AgFeO2/TiO2异质结光催化剂的制备方法及其应用 Download PDFInfo
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Abstract
本发明公开了一种AgFeO2/TiO2异质结光催化剂的制备方法及其应用，属于光催化材料及水体污染物净化技术领域。本发明的技术方案要点为：以制备的TiO2纳米片为基体，具有加大的比表面积，为AgFeO2纳米颗粒提供了充足的生长位点，有效抑制了AgFeO2纳米颗粒的团聚，增大了TiO2和AgFeO2的接触面积，促进了广生电荷的有效分离，提高了AgFeO2/TiO2异质结光催化剂的光催化活性，能够用于光催化降解去除水体中污染物。
Description
技术领域
本发明属于光催化材料及水体污染物净化技术领域，具体涉及一种AgFeO2/TiO2异质结光催化剂的制备方法及其应用。
背景技术
工业废水、医药废水和畜禽废水等有机废水的大量排放对有限的水资源造成污染，严重影响了水资源的利用，传统的污水处理技术难以将有机污染物有效去除。而光催化技术作为一种高效、环保、无污染的去除水中有机污染物的方法，可以将污染物彻底去除。在众多半导体光催化材料中，TiO2由于其良好的光催化活性，被广泛应用于废水处理。但其禁带宽度较大（约3.2eV），只能吸收波长小于387nm的紫外光，且光生电子空穴对复合严重，因此，大大限制了它的实际应用。将其与窄带隙半导体复合被认为是一种高效的提高TiO2光催化活性的方法。
Ag系半导体光催化材料带隙能较小，可以很好的吸收利用可见光，这是因为Ag+具有4d10电子轨道，可以通过轨道重建，使不同的Ag系半导体价带位置升高或者导带位置降低，从而改变半导体的带隙能。而且，Ag单质具有表面等离子体共振效应，可以吸收可见光。同时，由于其光生空穴和电子的有效质量较小，光生电荷迁移较快。因此，将TiO2与银系半导体复合可以有效提高材料的光催化活性。
AgFeO2的禁带宽度为1.7eV，是一种可见光响应的光催化剂。研究发现，AgI/AgFeO2和AgCl/Ag/AgFeO2异质结光催化剂在60分钟内对罗丹明B的降解率分别为98.3%和97.5%，表明材料具有较高的光催化活性。AgFeO2/g-C3N4 异质结的光催化活性也较高，在可见光条件下对刚果红的降解率高达94.0%。但是，纯AgFeO2光照下易腐蚀，光生载流子复合迅速。这些缺点降低了其光催化活性，限制了其广泛应用。
发明内容
为了解决上述背景技术的不足，本发明提供了一种合成简单、操作方便且光催化活性优异的AgFeO2/TiO2异质结光催化剂的制备方法及其应用，该AgFeO2/TiO2异质结光催化剂中TiO2为薄片状，具有加大的比表面积，为AgFeO2纳米颗粒提供了充足的生长位点，有效抑制了AgFeO2纳米颗粒的团聚，增大了TiO2和AgFeO2的接触面积，促进了广生电荷的有效分离，提高了材料的光催化活性，能够用于光催化降解去除水体中污染物。
本发明为解决上述技术问题采用如下技术方案：一种AgFeO2/TiO2异质结光催化剂的制备方法，其特征在于具体步骤为：
步骤S1：将HF加入到钛酸四丁酯液体中，搅拌，转移至反应釜中，于180oC反应36h，分别用无水乙醇和蒸馏水洗涤，得到的沉淀转移至NaOH溶液中搅拌，随后水洗至中性，烘干，得到TiO2纳米片；
步骤S2：将步骤S1得到的TiO2纳米片加入到蒸馏水中，搅拌，加入硝酸银溶液，避光搅拌，再加入硝酸铁溶液，调节混合体系的pH值为12，继续搅拌2h，用蒸馏水和无水乙醇分别洗涤三次，离心，于80oC烘干，得到AgFeO2/TiO2异质结光催化剂。
作为本发明进一步的改进，步骤S1中所述NaOH溶液的浓度为0.1M。
作为本发明进一步的改进，步骤S2中所述硝酸银溶液的浓度为0.4337g/mL；所述硝酸铁溶液的浓度为0.4121g/mL。
本发明所述的AgFeO2/TiO2异质结光催化剂在光催化降解去除水体中污染物中的应用。
本发明与现有技术相比具有以下有益效果：
（1）本发明中，将HF加入到钛酸四丁酯液体中的目的是使材料定向生长制备TiO2纳米片。
（2）本发明得到的TiO2纳米片表面光滑，长约50nm，均一性好。
（3）本发明中TiO2纳米片具有较大的比较面积，AgFeO2和TiO2接触面积大，有利于广生载流子的分离。
（4）本发明中AgFeO2/TiO2异质结光催化剂在实际水体中有良好的光催化性能，循环性能优异，在实际废水处理中有巨大的应用潜力。
附图说明
图1是本发明实施例制得的TiO2、AgFeO2和AgFeO2/TiO2的XRD图；
图2是本发明实施例制得的TiO2、AgFeO2和AgFeO2/TiO2的TEM图；
图3是本发明实施例制得的TiO2、AgFeO2和AgFeO2/TiO2的UV-vis图谱；
图4是本发明实施例制得的样品对BPA的降解效果图；
图5是本发明实施例制得的AgFeO2/TiO2对环丙沙星（CIP）、甲硝唑（MZ）和氧四环素（OTC）的降解效果图；
图6是本发明实施例制得的AgFeO2/TiO2对不同水源中双酚A（BPA）的降解效果图；
图7是本发明实施例制得的AgFeO2/TiO2光催化降解BPA循环效果图。
具体实时方式
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
AgFeO2/TiO2异质结光催化剂的制备：
取6mL HF逐滴加入到钛酸四丁酯（50mL）中，搅拌120分钟，随后将液体转移至100mL反应釜中，于180oC保持36h，用无水醇洗涤六次，再用蒸馏水洗涤三次，离心，将沉淀物加入到NaOH溶液（0.1M）中搅拌8h，水洗至中性，在烘箱中于80oC烘干，得到TiO2纳米片；
将上述制备的TiO2纳米片（0.2g）分散到100mL蒸馏水中，搅拌30min，加入19.0μL硝酸银溶液（0.4337g/mL），避光搅拌60min，继续加入50μL硝酸铁溶液（0.4121g/mL），然后调节混合体系的pH值为12，继续搅拌2h，分别用蒸馏水和无水乙醇洗涤三次，于80oC烘干，得到AgFeO2/TiO2异质结光催化剂。
图1是实施例制得的TiO2、AgFeO2和AgFeO2/TiO2的XRD图。纯TiO2在25.27°、37.70°和47.98°处有特征衍射峰，对应于锐钛矿TiO2的（101）、（004）和（200）晶面（JCPDS No. 71-1167）。纯AgFeO2的特征峰位于14.27°、28.78°、34.83°处，分别对应于AgFeO2的（002）、（004）、（101）晶面（JCPDS No. 25-0765）。AgFeO2/TiO2光催化剂中只观察到了TiO2的衍射峰，未观察到AgFeO2的特征峰，这可能是因为AgFeO2含量较低。
图2是本实施例制得的TiO2、AgFeO2和AgFeO2/TiO2的TEM图。纯TiO2为单片状结构，表面光滑。而纯AgFeO2团聚在一起，分散性差。与纯AgFeO2相比，AgFeO2/TiO2异质结光催化剂中的AgFeO2均匀分散在TiO2纳米片表面，且粒径明显减小，这是因为TiO2纳米片具有较大的比表面积，为AgFeO2提供了充足的生长位点，有效抑制了AgFeO2的团聚。
图3是本实施例制得的TiO2、AgFeO2和AgFeO2/TiO2的UV-vis图谱。TiO2只能吸收波长小于400nm的紫外光，而纯AgFeO2既可以吸收紫外光，又可以吸收可见光。与纯TiO2相比，AgFeO2/TiO2异质结光催化剂的吸收带边明显红移，表明其对可见光的吸光能力增强。
AgFeO2/TiO2异质结光催化剂的应用：
将AgFeO2/TiO2异质结光催化剂投入到有机废水中，AgFeO2/TiO2异质结光催化剂的浓度为0.5g/L，有机废水的浓度为20mg/L，有机废水中污染物分别为BPA、CIP、OTC和MZ。此外，还考察了AgFeO2/TiO2异质结光催化剂对自来水、黄河水、象湖水、龙湖水和贾鲁河水中BPA的降解效果。
图4是本实施例制得的TiO2、AgFeO2和AgFeO2/TiO2对BPA的降解效果图。在不加催化剂的情况下，光照40分钟时BPA几乎没有讲解，表明BPA不易光解。加入TiO2和AgFeO2后，BPA的降解率分别为39.0%和27.5%，降解率较低。而加入AgFeO2/TiO2异质结光催化剂后BPA的降解率达到99.2%，表明AgFeO2/TiO2异质结光催化剂的光催化活性显著提高。
图5为本实施例制得的AgFeO2/TiO2对CIP、MZ和OTC的降解效果图。光照60分钟时，CIP、MZ、OTC的降解率分别为68.0%、51.1%和70.1%，表明AgFeO2/TiO2异质结光催化剂对这三种抗生素药物也具有较高的光催化降解活性。
图6是本实施例制得的AgFeO2/TiO2对不同水源中BPA的降解效果图。由图可知，在自来水、龙湖、象湖、黄河、贾鲁河水中，AgFeO2/TiO2异质结光催化剂对BPA有令人满意的降解效果，降解率分别为99.0%、90.1%、86.5%、86.0%和80.1%，表明异质结光催化剂在实际水体中有较强的水体净化能力。
图7是本实施例制得的AgFeO2/TiO2光催化降解BPA循环效果图。由图可以看出制得的AgFeO2/TiO2异质结光催化剂经过四次循环后对BPA的降解率仍然达到90%以上，进而说明AgFeO2/TiO2异质结光催化剂具有很好的循环性能。
本领域的技术人员在不脱离权利要求书确定的本发明的精神和范围的条件下，还可以对以上内容进行各种各样的修改。因此本发明的范围并不仅限于以上的说明，而是由权利要求书的范围来确定的。
Claims (4)
1.一种AgFeO2/TiO2异质结光催化剂的制备方法，其特征在于具体步骤为：
步骤S1：将HF加入到钛酸四丁酯液体中，搅拌，转移至反应釜中，于180oC反应36h，分别用无水乙醇和蒸馏水洗涤，得到的沉淀转移至NaOH溶液中搅拌，随后水洗至中性，烘干，得到TiO2纳米片；
步骤S2：将步骤S1得到的TiO2纳米片加入到蒸馏水中，搅拌，加入硝酸银溶液，避光搅拌，再加入硝酸铁溶液，调节混合体系的pH值为12，继续搅拌2h，用蒸馏水和无水乙醇分别洗涤三次，离心，于80oC烘干，得到AgFeO2/TiO2异质结光催化剂。
2.根据权利要求1所述的AgFeO2/TiO2异质结光催化剂的制备方法，其特征在于：步骤S1中所述NaOH溶液的浓度为0.1M。
3.根据权利要求1所述的AgFeO2/TiO2异质结光催化剂的制备方法，其特征在于：步骤S2中所述硝酸银溶液的浓度为0.4337g/mL；所述硝酸铁溶液的浓度为0.4121g/mL。
4.根据权利要求1-3中任意一项所述的方法制得的AgFeO2/TiO2异质结光催化剂在光催化降解去除水体中污染物中的应用。
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