CN108325518A - 一种花球形碳负载钨酸锑复合光催化剂的制备 - Google Patents
一种花球形碳负载钨酸锑复合光催化剂的制备 Download PDFInfo
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Abstract
本发明公开了一种花球形碳负载钨酸锑复合光催化剂的制备方法及其在光催化降解污染物上的应用，属于材料制备及光催化的技术领域。该催化剂的特点有：具有3维的花球形貌特征，由3维结构的C微球与钨酸锑纳米片复合而成。在制备光催化剂过程中，采用工艺简单的水热法，合成出花球形碳负载钨酸锑复合光催化剂。在碳和钨酸锑的共同作用下，花球形碳负载钨酸锑复合光催化剂表现出良好的吸附性能和光催化性能，促进了新型半导体钨酸锑光催化剂的研究。
Description
技术领域
本发明涉及一种花球形碳负载钨酸锑的复合光催化剂的制备。通过一步水热法制备出花球形碳负载钨酸锑复合光催化剂，制备工艺简单安全、节能环保。该材料在可见光照射的条件下表现出良好的光催化活性，因此在环境污染处理领域具有广泛的应用前景。
背景技术
随着工业化程度的推进，环境污染的问题已受到越来越多的关注。传统的污染物处理方法已经满足不了人们的要求。寻找出一种清洁，高效，节能环保的污水处理方法，成了人们研究的热点方向。
自1972年首次发现TiO2具有光催化活性以来，光催化技术的研究一直是材料领域的热点方向。光催化技术凭借其节能环保、无二次污染等优点为污水的处理提供了一个非常好的解决途径。半导体光催化材料可以利用取之不尽、用之不竭的太阳能处理空气中或者水中有毒有害物质,改善环境,达到资源利用生态化的目的。目前，各种不同的半导体光光催化剂材料被广泛研究，如钨酸铋，钨酸铯等。但是钨酸锑凭借其材料来源广泛，价格低廉，无生物毒性等优点成为光催化研究的热点材料之一。
但是, 钨酸锑光催化剂也存在着一些缺陷，例如，其量子效率偏低,并且高得光生电子-空穴复合速率，这些都阻碍了其进一步的发展与应用。在这种背景下,如何提高钨酸锑的光催化效率和拓宽其光相应范围，成了钨酸锑光催化剂的研究重点。至今为止,各种方法已经被用来提高其量子效率和扩展其光相应范围,如:形貌控制、半导体复合等。但是,上述方法改性后钨酸锑的光催化效率、稳定性以及在实际应用中的反复使用性受到了一定的限制。
近年来，利用其他材料与钨酸锑催化剂进行复合，制备复合光催化剂的研究取得了一定的进展，得到的钨酸锑基复合光催化剂在太阳光的照射下表现出良好的光催化活性。本发明利用碳材料高的吸附性与钨酸锑进行复合，形成3维的花球形微观结构，有效地提高了钨酸锑的可见光利用率和光催化活性。
发明内容
本发明的目的是制备出具有高的可见光利用率和高催化活性的钨酸锑基复合光催化剂，并且其催化循环稳定性高，推进钨酸锑的实际应用。
为实现本发明目的采用如下技术方案：
利用葡萄糖的水解性，通过水热反应，在钨酸锑的结晶过程在制备出花球形碳负载钨酸锑复合光催化剂。在碳的吸附性作用下提高钨酸锑的可见光催化活性。
一种花球形碳负载钨酸锑复合光催化剂的制备，其特征步骤如下：
（1）称取一定量葡萄糖溶解在50ml去离子水中，搅拌均匀；
（2）加入适量SbCl3于上述溶液中，磁力搅拌均匀；
（3）向步骤（2）溶液中适量Na2WO4﹒2H2O，继续搅拌均匀；
（4）向步骤（3）溶液中加入0.08g NaOH，搅拌均匀；
（5）将搅拌好的溶液转移到高压反应釜中反应；
（6）将反应完全的样品离心洗涤，干燥后研磨即得到样品。
步骤(1)中葡萄糖的质量为0.3g。
步骤(2)中SbCl3的质量为0.228g。
步骤(3)中Na2WO4﹒2H2O的质量为0.165g。
步骤(5)中反应温度为180℃，反应时间为12h。
步骤(5)中的离心清洗过程为先用乙醇清洗4次，再用去离子水清洗2次，离心速率8000rpm，时间6min。
所述花球形碳负载钨酸锑复合光催化剂用于水溶液中有机污染物的可见光催化降解。
目标污染物为罗丹明B。
本发明具有如下优点：本发明制备方法采用的是水热法，实验条件安全、操作步骤简单、绿色环保。本发明制备的是一种花球形碳负载钨酸锑复合光催化剂，经扫描电镜可发现该材料是由碳球负载钨酸锑纳米片复合而成(图1)。
本发明中的花球形碳负载钨酸锑复合光催化剂具有良好的光催化活性，其催化活性在钨酸锑单体的基础上有了显著的提升。在暗反应过程中，花球形碳负载钨酸锑复合光催化剂表现出高的吸附性；在70min人造可见光源的照射下降解罗丹明B染料花球形碳负载钨酸锑复合光催化剂表现出良好的光催化活性(图2)。
附图说明
图1为花球形碳负载钨酸锑复合材料的扫描电镜图。
图2为花球形碳负载钨酸锑复合材料的光催化降解图。
具体实施方式
一种花球形碳负载钨酸锑复合光催化剂的制备，其特征步骤如下：
（1）称取一定量葡萄糖溶解在50ml去离子水中，搅拌均匀；
（2）加入适量SbCl3于上述溶液中，磁力搅拌均匀；
（3）向步骤（2）溶液中适量Na2WO4﹒2H2O，继续搅拌均匀；
（4）向步骤（3）溶液中加入0.08g NaOH，搅拌均匀；
（5）将搅拌好的溶液转移到高压反应釜中反应；
（6）将反应完全的样品离心洗涤，干燥后研磨即得到样品。
步骤(1)中葡萄糖的质量为0.3g。
步骤(2)中SbCl3的质量为0.228g。
步骤(3)中Na2WO4﹒2H2O的质量为0.165g。
步骤(5)中反应温度为180℃，反应时间为12h。
步骤(5)中的离心清洗过程为先用乙醇清洗4次，再用去离子水清洗2次，离心速率8000rpm，时间6min。
所述花球形碳负载钨酸锑复合光催化剂用于水溶液中有机污染物的可见光催化降解。
下面例举实施例子制备花球形碳负载钨酸锑复合光催化剂。
实施例1：花球形碳负载钨酸锑复合光催化剂的制备
量取50ml去离子水，称量0.3g 葡萄糖加入到水中，搅拌均匀，然后称量0.228g SbCl3于溶液中，搅拌均匀；接着加入0.165g Na2WO4﹒2H2O，继续磁力搅拌；再称量氢氧化钠0.08g，加入到上述溶液中，磁力搅拌；接着将溶液倒入反应釜中，加热，加热温度为180℃，时间为12h。反应完成后，离心洗涤，先用乙醇清洗4次，在用水洗2次，离心速度为8000rpm，时间为6min。最后烘箱中60℃干燥，研磨即得到样品。
实施例2：花球形碳负载钨酸锑复合光催化剂在可见光照射下降解罗丹明B
按实施例1方法制得的花球形碳负载钨酸锑复合光催化剂进行降解罗丹明B实验。罗丹明B溶液的浓度是1×10-5mol L-1；取复合材料粉体50mg，置于100mL上述罗丹明B溶液中，在暗室中搅拌60分钟，然后将溶液置于紫外光被过滤掉的可见光源中，每10分钟取5mL罗丹明B溶液，用紫外-可见分光光度计测出溶液中罗丹明B的特征峰值。
按实施例2得到花球形碳负载钨酸锑复合光催化剂可见光降解罗丹明B的降解曲线，见图2。从图2可以看出施例1制备的复合材料粉体粉体在光照70min后催化降解达到90%以上，表现出高的催化活性。
Claims (6)
1.一种花球形碳负载钨酸锑复合光催化剂的制备，其特征包括以下步骤：
称取一定量葡萄糖溶解在50ml去离子水中，搅拌均匀；
加入适量SbCl3于上述溶液中，磁力搅拌均匀；
向步骤（2）溶液中适量Na2WO4﹒2H2O，继续搅拌均匀；
向步骤（3）溶液中加入0.08gNaOH，搅拌均匀；
将搅拌好的溶液转移到高压反应釜中反应；
将反应完全的样品离心洗涤，干燥后研磨即得到样品。
2.根据权利要求1一种花球形碳负载钨酸锑复合光催化剂的制备，其特征在于葡萄糖的质量为0.3g。
3.根据权利要求1一种花球形碳负载钨酸锑复合光催化剂的制备，其特征在于SbCl3的质量为0.228g。
4.根据权利要求1一种花球形碳负载钨酸锑复合光催化剂的制备，其特征在于Na2WO4﹒2H2O的质量为0.165g。
5.根据权利要求1一种花球形碳负载钨酸锑复合光催化剂的制备，其特征在于反应温度为180℃，反应时间为12h。
6.根据权利要求1一种花球形碳负载钨酸锑复合光催化剂的制备，其特征在于具有三维花球状形貌。
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