CN110694650B - 一种Bi负载的Bi4NbO8Cl复合可见光催化剂的制备方法 - Google Patents
一种Bi负载的Bi4NbO8Cl复合可见光催化剂的制备方法 Download PDFInfo
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Abstract
本发明提供了一种Bi负载Bi4NbO8Cl复合可见光催化剂的制备方法，属于纳米材料的制备领域。本发明使用NaCl/KCl混合熔盐法制备的Bi4NbO8Cl片状结构为原料，采用乙二醇溶剂热法成功原位制备了零维Bi颗粒负载的Bi4NbO8Br二维结构；由于乙二醇的还原性，二维Bi4NbO8Br同时富含大量氧空位，零维铋金属作为电子陷阱和氧空位的协同作用，提高了Bi负载Bi4NbO8Cl复合可见光催化剂降解罗丹明B的性能。
Description
技术领域：
本发明涉及Bi负载Bi4NbO8Cl复合可见光催化剂的制备方法，具体地说，利用熔盐法制备Bi4NbO8Cl 片层结构为前驱体，以乙二醇为还原剂，采用原位生长法，通过控制不同的溶剂热反应温度和时间，一步制备出具有优良光催化性能的复合可见光催化剂，本技术属于光催化材料制备领域。
背景技术：
随着世界人口、工业和经济的快速增长，水环境污染已经成为一个严重的问题。近几十年来，光催化技术已被用作一种经济有效且环保的氧化过程，以去除有害的环境污染物，而传统的半导体催化剂如TiO2、 ZnO等，只能对紫外光进行响应，而紫外光只占太阳光的4％-6％，因此，开发一种新型的可见光响应的光催化剂成为一个具有挑战性的课题。
近年来的研究发现，很多铋基氧化物(BiVO4、Bi2WO6、BiOX等)具有较高的光催化性能，因其具有合适的禁带宽度、较高的电子迁移率和较大的可见光吸收系数。其中，Bi4NbO8Cl作为一种新型的铋基氯氧化物受到了广泛的关注，其属于Aurivilius-Sillén结构，是由[Bi2O2]2+层、[NbO4]3-层和[Cl]-层组成，这种独特的层状分子结构有利于光生载流子的分离，从而提高催化剂的光催化性能。由于Bi4NbO8Cl在价带和导带都具有很强的Bi 6s轨道和O 2p轨道杂化，这种特性可以缩小带隙，提供可见光吸收和较高的光稳定性。引入氧空位缺陷或沉积非贵金属可提高光催化性能，一方面，氧空位可以扩大光的响应范围，捕获电子或空穴，降低复合速率，提供催化过程中的活性位点，另一方面，金属铋可以作为贵金属的理想替代品，它具有有效质量低、电子捕获性能优异、高活性载流子、价格低廉、易获得等优点。
关于Bi4NbO8Cl的改性报道中，多数使用贵金属沉积或者半导体复合方式提高Bi4NbO8Cl的催化性能。到目前为止，还没有关于铋金属代替贵金属沉积到Bi4NbO8Cl纳米片上，同时在Bi4NbO8Cl中引入氧空位的相关报道。因此，我们设计了一种Bi原位负载Bi4NbO8Cl复合光催化材料的制备方法，不仅保持 Bi4NbO8Cl的原有二维形貌，形成的零维铋金属和氧空位的协同作用，提高了光催化效率。
发明内容：
本发明采用乙二醇热法，制备出一种性能优异的Bi负载Bi4NbO8Cl复合可见光催化剂。
本发明是通过如下技术方案实现的：
一种Bi负载Bi4NbO8Cl复合可见光催化剂的制备方法，按以下步骤进行：
(1)室温下，分别称取一定量的NaCl和KCl，放入玛瑙研钵中；再依次称取一定量的BiOCl、Nb2O5、 Bi2O3，相继加入到玛瑙研钵中；将上述混合物于玛瑙研钵中研磨15min，直至无明显颗粒感；将上述混合物转移到刚玉坩埚中，在马弗炉中煅烧，并保持升温速率；将煅烧后的产物取出，不经研磨使用300mL 的80℃热水分5次洗涤，期间注意超声；用0.1M的AgNO3检验残余Cl-浓度；将上述产物在60℃烘箱中干燥12h，并研磨，获得Bi4NbO8Cl粉体。
(2)室温下，分别称取预先制备的一定量的Bi4NbO8Cl粉体，放入装有80mL乙二醇的烧杯中，磁力充分搅拌，取出上述混合物中磁子，将悬浮液转移到100mL聚四氟乙烯内衬高压釜中，于鼓风干燥箱中 160℃反应不同时长，反应结束后，过滤收集沉淀，用去离子水和乙醇洗涤几次，以去除残留的杂质。最后，在空气中60℃干燥24h，得到Bi负载Bi4NbO8Cl样品。
优选的，步骤(1)中所述的NaCl和KCl的物质的量比为1:1，BiOCl、Nb2O5、Bi2O3的物质的量比为2:1:3，并且其与混合熔盐NaCl/KCl的质量比为82.1:100。
优选的，步骤(1)中所述的煅烧温度为600-800℃，煅烧时间为0.5-5h，升温速率为2-5℃/min。
优选的，步骤(2)中所述的Bi4NbO8Cl粉体量为0.5mmol(546mg)。
优选的，步骤(2)中所述的溶剂热反应温度为120-180℃，时间2-48h。
与现有技术相比，本发明的有益效果：
本发明中使用熔盐法制备的Bi4NbO8Cl片状结构为前驱体，采用乙二醇热法，成功制备出Bi负载 Bi4NbO8Cl纳米复合物，并保持了Bi4NbO8Cl的二维形貌；使用乙二醇为还原剂，在高温条件下，同时形成了铋金属和氧空位，通过氧空位和铋金属的协同作用，提高催化剂的性能。本发明以Bi4NbO8Cl可见光响应的催化剂为基础，通过不断的调节溶剂热反应温度和时间，得到了0D/2D复合结构Bi负载富氧空位的Bi4NbO8Cl可见光催化剂，并用于光催化降解污染物的领域，取得了良好的效果，当溶剂热反应温度为 160℃，反应时间为10h时，光催化性能最优。
附图说明
图1为本发明制备的不同溶剂热时间的Bi负载Bi4NbO8Cl复合材料的XRD图。
图2为实施例1制备的样品的SEM图。
图3为实施例1制备的样品的ESR图。
图4为本发明制备的溶剂热时间的Bi负载Bi4NbO8Cl复合材料对于罗丹明B的降解曲线图。
具体实施方式：
实施例1：
室温下，分别称取292mg的NaCl和372mg的KCl，放入玛瑙研钵中；再依次称取130mg的BiOCl、 66mg的Nb2O5和349mg的Bi2O3，相继加入到玛瑙研钵中；将上述混合物于玛瑙研钵中研磨15min，直至无明显颗粒感；将上述混合物转移到刚玉坩埚中，在马弗炉中750℃煅烧60min，并保持升温速率为 3℃/min；将煅烧后的产物取出，不经研磨使用300mL的80℃热水分5次洗涤，期间注意超声；用0.1M 的AgNO3检验残余Cl-浓度；将上述产物在60℃烘箱中干燥12h，并研磨，获得Bi4NbO8Cl粉体。
分别称取预先制备的546mg的Bi4NbO8Cl粉体，放入装有80mL乙二醇的烧杯中，磁力充分搅拌，取出上述混合物中磁子，将悬浮液转移到100mL聚四氟乙烯内衬高压釜中，于鼓风干燥箱中160℃反应 10h，反应结束后，过滤收集沉淀，用去离子水和乙醇洗涤几次，以去除残留的杂质。最后，在空气中60℃干燥24h，得到Bi负载Bi4NbO8Cl样品。
实施例2：
室温下，分别称取292mg的NaCl和372mg的KCl，放入玛瑙研钵中；再依次称取130mg的BiOCl、 66mg的Nb2O5和349mg的Bi2O3，相继加入到玛瑙研钵中；将上述混合物于玛瑙研钵中研磨15min，直至无明显颗粒感；将上述混合物转移到刚玉坩埚中，在马弗炉中750℃煅烧60min，并保持升温速率为 3℃/min；将煅烧后的产物取出，不经研磨使用300mL的80℃热水分5次洗涤，期间注意超声；用0.1M 的AgNO3检验残余Cl-浓度；将上述产物在60℃烘箱中干燥12h，并研磨，获得Bi4NbO8Cl粉体。
分别称取预先制备的546mg的Bi4NbO8Cl粉体，放入装有80mL乙二醇的烧杯中，磁力充分搅拌，取出上述混合物中磁子，将悬浮液转移到100mL聚四氟乙烯内衬高压釜中，于鼓风干燥箱中180℃反应10h，反应结束后，过滤收集沉淀，用去离子水和乙醇洗涤几次，以去除残留的杂质。最后，在空气中60℃干燥24h，得到Bi负载Bi4NbO8Cl样品。
实施例3：
室温下，分别称取292mg的NaCl和372mg的KCl，放入玛瑙研钵中；再依次称取130mg的BiOCl、 66mg的Nb2O5和349mg的Bi2O3，相继加入到玛瑙研钵中；将上述混合物于玛瑙研钵中研磨15min，直至无明显颗粒感；将上述混合物转移到刚玉坩埚中，在马弗炉中750℃煅烧60min，并保持升温速率为 3℃/min；将煅烧后的产物取出，不经研磨使用300mL的80℃热水分5次洗涤，期间注意超声；用0.1M 的AgNO3检验残余Cl-浓度；将上述产物在60℃烘箱中干燥12h，并研磨，获得Bi4NbO8Cl粉体。
分别称取预先制备的546mg的Bi4NbO8Cl粉体，放入装有80mL乙二醇的烧杯中，磁力充分搅拌，取出上述混合物中磁子，将悬浮液转移到100mL聚四氟乙烯内衬高压釜中，于鼓风干燥箱中160℃反应 48h，反应结束后，过滤收集沉淀，用去离子水和乙醇洗涤几次，以去除残留的杂质。最后，在空气中60℃干燥24h，得到Bi负载Bi4NbO8Cl样品。
Claims (3)
1.一种Bi负载Bi4NbO8Cl复合可见光催化剂的制备方法，其特征在于，所述的复合光催化剂中Bi以零维金属颗粒的形式负载于二维的Bi4NbO8Cl片状结构上；该复合光催化剂的制备过程按以下步骤进行：
(1)室温下，分别称取292mg的NaCl和372mg的KCl，放入玛瑙研钵中；再依次称取的130mg的BiOCl、66mg的Nb2O5、349mg的Bi2O3，相继加入到玛瑙研钵中；将上述混合物于玛瑙研钵中研磨15min，直至无明显颗粒感；将上述混合物转移到刚玉坩埚中，在马弗炉中750℃煅烧，并保持升温速率为3℃/min，保温60min；将煅烧后的产物取出，不经研磨使用300mL的80℃热水分5次洗涤产物，期间注意超声；用0.1M的AgNO3检验残余Cl-浓度；将上述产物在60℃烘箱中干燥12h，并研磨，获得Bi4NbO8Cl粉体；
(2)室温下，分别称取546mg预先制备的Bi4NbO8Cl粉体，放入装有80mL乙二醇的烧杯中，磁力充分搅拌，取出上述混合物中磁子，将悬浮液转移到100mL聚四氟乙烯内衬高压釜中，于鼓风干燥箱中加热并反应一段时间，反应结束后，过滤收集沉淀，用去离子水和乙醇洗涤几次，以去除残留的杂质；最后，在空气中60℃干燥24h，得到Bi负载的Bi4NbO8Cl样品。
2.根据权利要求1所述一种Bi负载Bi4NbO8Cl复合可见光催化剂的制备方法，其特征在于，所述的Bi负载Bi4NbO8Cl复合可见光催化剂含有大量的氧空位。
3.根据权利要求1所述的一种Bi负载Bi4NbO8Cl复合可见光催化剂的制备方法，其特征在于，步骤(2)中所述的溶剂热温度为120-180℃，反应时间为2-48h。
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