CN114904534B - 钼酸铋/钒酸铁复合纳米材料及其制备方法和在声光催化降解水中污染物的应用 - Google Patents
钼酸铋/钒酸铁复合纳米材料及其制备方法和在声光催化降解水中污染物的应用 Download PDFInfo
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Abstract
本发明公开了一种钼酸铋/钒酸铁复合纳米材料及其制备方法和在声光催化降解水中污染物的应用，将Bi(NO3)3·5H2O和Na2MoO4·2H2O分别溶于乙二醇中；然后在Bi(NO3)3·5H2O中加入FeVO4，超声搅拌直到溶解，再与Na2MoO4·2H2O混合，并在磁力搅拌下持续30min；最后，转移至高压釜中，加热至160℃下保持24h，冷却至室温后，经离子水和乙醇漂洗、干燥得到Bi2MoO6/FeVO4复合纳米材料。本发明采用简单的一步溶剂热法制备出Bi2MoO6/FeVO4异质结构。该材料可通过添加不同质量的Bi2MoO6/FeVO4来控制其摩尔比，可制得不同处理效率的Bi2MoO6/FeVO4复合材料。
Description
技术领域
本发明属于声光催化材料技术领域，具体涉及一种钼酸铋/钒酸铁复合纳米材料及其制备方法和在声光催化降解水中污染物的应用。
背景技术
目前现有的水处理工艺对抗生素的去除效果相当有限，无法进行有效去除，致使水中大部分抗生素进入到生态环境中，对自然界与人体都造成重大危害。现在常用光催化技术进行水中抗生素的去除，该技术对光催化剂的依赖程度较高，而大部分光催化材料都存在材料的载流子扩散缓慢、电子-空穴对复合率较快、太阳能利用率低的量子产率差以及回收率低等问题，大大限制了其光催化性能。相比之下，掺杂其他金属化合物所制备的复合材料，具有较好的光催化性能。掺杂金属化合物后的光催化剂由于具有强烈的局域表面等离子体共振效应，可促进电子扩散、电荷载流子的快速再生和提高光催化活性，从而显示出有效的光催化性能。同时，该复合材料的稳定性以及回收率较之于传统光催化剂也大大提高了。
发明内容
针对目前的问题，本发明采用简单的一步溶剂热法制备出Bi2MoO6/FeVO4异质结构。该材料可通过添加不同质量的Bi2MoO6/FeVO4来控制其摩尔比，可制得不同处理效率的Bi2MoO6/FeVO4复合材料。
为实现上述目的，本发明采用如下技术方案：
一种Bi2MoO6/FeVO4复合纳米材料的制备方法包括以下步骤：将Bi(NO3)3·5H2O(2mmol)和Na2MoO4·2H2O(1 mmol)分别溶于乙二醇中；然后在Bi(NO3)3·5H2O中加入FeVO4(2mmol)，超声搅拌直到溶解，再与Na2MoO4·2H2O混合，并在磁力搅拌下持续30min；最后，转移至高压釜中，加热至160℃下保持24h，冷却至室温后，经离子水和乙醇漂洗、干燥得到Bi2MoO6/FeVO4复合纳米材料。
进一步地，所述超声搅拌具体为超声0.5h后再搅拌1h。
进一步地，所述干燥是在80℃下干燥12h。
本发明制得的Bi2MoO6/FeVO4复合纳米材料中Bi2MoO6和FeVO4的摩尔比最优为1:2，可用于声光催化降解水中的环丙沙星。
本发明制得的Bi2MoO6/FeVO4复合纳米材料声光催化降解环丙沙星的机理为：声光可共同激发Bi2MoO6价带中的电子向导带中跃迁，并产生h+跟e-，h+与H2O反应生成·OH，而FeVO4价带中电子也可通过光芬顿反应跃迁至其导带中并产生h+跟e-，e-与O2反应撤生成·O2 -，然后通过生成的·O2和·OH将环丙沙星分解成水、二氧化碳以及其他小分子物质。纯FeVO4或纯Bi2MoO6的降解机理与上述结果一致，但纯FeVO4或纯Bi2MoO6导带与价带中的h+跟e-容易复合，从而没有足够多的h+跟e-来将O2与H2O氧化成·O2 -和·OH等活性物质，会使环丙沙星的降解能力下降。与纯FeVO4或纯Bi2MoO6不同的是，本发明制得的Bi2MoO6/FeVO4复合纳米材料可以避免这种情况，从而大大提高声光催化降解性能。
附图说明
图1为纯FeVO4和纯Bi2MoO6的扫描电镜图，其中a和b为纯FeVO4；c和d为纯Bi2MoO6；
图2为本发明制得的Bi2MoO6/FeVO4复合纳米材料的扫描电镜图，其中e和f为BF-1；g和h为BF-0.75；i和j为BF-0.5；k和l为BF-0.25（其中BF为材料中Bi2MoO6和FeVO4的摩尔比，如BF-1便为Bi2MoO6和FeVO4的摩尔比值为1：1）；
图3为Bi2MoO6/FeVO4复合纳米材料对CIP的降解效果曲线图。
具体实施方式
为了使本发明所述的内容更加便于理解，下面结合具体实施方式对本发明所述的技术方案做进一步的说明，但是本发明不仅限于此。
实施例1
首先，将称取的Bi(NO3)3·5H2O(2 mmol)和Na2MoO4·2H2O(1mmol)分别倒入到装有15mL乙二醇的烧杯中，并在Bi(NO3)3·5H2O溶液中加入制备好的FeVO4(2mmol)。将上述溶液超声0.5h后在搅拌1h直到溶液溶解，然后将两种溶液混合，并在磁力搅拌下持续30min。最后，将上述混合物转移到50mL内衬聚四氟乙烯的不锈钢高压釜中，加热至160℃下保持24h。冷却至室温后，所得样品用去离子水和乙醇漂洗3次，最后在烘箱中80℃干燥12h，得到Bi2MoO6/FeVO4复合纳米材料。
图1是纯FeVO4和纯Bi2MoO6的扫描电镜图，如图1(a-b)所示，合成的FeVO4纳米棒所具有的直径为约3微米，宽度在300纳米左右，从而能为Bi2MoO6/FeVO4异质结的形成提供适宜的环境。制备的几颗直径为1-2微米的微球状Bi2MoO6纳米材料可以在图1(c-d)观察到，值得注意的是，花状微球是由Bi2MoO6纳米片组装而成的。两种材料结合后，如图2(i, j)所示，在Bi2MoO6和FeVO4制备摩尔比1:2时，大量的Bi2MoO6纳米薄片沉积在FeVO4纳米棒表面形成3D分层结构，表明在以添加FeVO4为前驱体的溶剂热制备法中，FeVO4可以作为基底并极大抑制Bi2MoO6纳米片在其生长过程中的聚集。此外，这种混合结构可以增加比表面积并暴露更多的表面活性位点参与声光催化反应。其他不同配比制备材料的SEM图像如图2(e-h, k-l)所示，由于Bi2MoO6具有独立成核的性质，当FeVO4的含量较少时会导致Bi2MoO6的聚集体（图2e-h）。随着FeVO4含量的增加（Bi2MoO6含量降低），覆盖在FeVO4纳米棒上的Bi2MoO6纳米片越来越少，复合光催化剂的表面变得光滑，这意味着BF-0.25形成的异质结在减少。当摩尔配比大于0.25时，从图中可以看出FeVO4纳米棒被Bi2MoO6纳米片包裹得很好。
图3是Bi2MoO6/FeVO4复合纳米材料对CIP的降解效果曲线图，可以看出经过3h的反应后，Bi2MoO6与FeVO4的比值为1：2的Bi2MoO6/FeVO4复合纳米材料对CIP的去除效果最好去，除率可达到90.3%，没有加入该材料，对CIP的去除率仅为1.7%。由此可知，所制备的光催化材料Bi2MoO6/FeVO4具有优异的降解CIP的性能，且所制备的Bi2MoO6/FeVO4摩尔比为1：2的复合材料具有更加优异的去除CIP的性能。
以上所述仅为本发明的较佳实施例，凡依本发明申请专利范围所做的均等变化与修饰，皆应属本发明的涵盖范围。
Claims (3)
1.一种Bi2MoO6/FeVO4复合纳米材料在声光催化降解水中污染物环丙沙星的应用，其特征在于：所述复合纳米材料的制备方法包括以下步骤：将Bi(NO3)3·5H2O和Na2MoO4·2H2O分别溶于乙二醇中；然后在Bi(NO3)3·5H2O中加入FeVO4，超声搅拌直到溶解，再与Na2MoO4·2H2O混合，并在磁力搅拌下持续30min；最后，转移至高压釜中，加热至160℃下保持24h，冷却至室温后，经离子水和乙醇漂洗、干燥得到Bi2MoO6/FeVO4复合纳米材料；Bi2MoO6和FeVO4的摩尔比为1:2。
2.根据权利要求1所述的应用，其特征在于：所述超声搅拌具体为超声0.5h后再搅拌1h。
3.根据权利要求1所述的应用，其特征在于：所述干燥是在80℃下干燥12h。
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