CN107597101A - 简易水热法合成具有可见光响应的光催化剂Bi2WO6/SnO2纳米片的制备方法 - Google Patents
简易水热法合成具有可见光响应的光催化剂Bi2WO6/SnO2纳米片的制备方法 Download PDFInfo
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Abstract
简易水热法合成具有可见光响应的光催化剂Bi2WO6/SnO2纳米片的制备方法,将采用水热法合成的Bi2WO6加入乙二醇中,搅拌获得Bi2WO6悬浊液。向Bi2WO6悬浊液中加入SnCl4·5H2O获得混合悬浮液。同时向去离子水中加入尿素,所获得的溶液迅速加入混合悬浮液,并在室温下搅拌。然后,混合溶液转移到反应釜中加热反应,最后得到的Bi2WO6/SnO2纳米片。本发明制备的Bi2WO6/SnO2纳米片比表面积大,吸附能力强;具有更好的可见光吸收性能,对光催化氧化降解有机污染物有很大的提高;而且本发明Bi2WO6/SnO2纳米片的制备方法比较简单,易于操作。
Description
技术领域
本发明涉及一种用于治理环境污染的半导体光催化剂及制备方法。
背景技术
能源危机和环境问题已是人类必须要面临的两个严峻问题,如何有效的控制和治理各种化学污染物对环境的污染是环境综合治理中的重点。近些年,作为高级氧化技术之一的半导体光催化氧化技术,正受到国内外学者的广泛研究,这种技术可以以太阳能作为能源来降解环境中的污染物,有效地利用太阳能,降低人们的能源消耗。
半导体光催化氧化技术始于日本科学家Fujishima和Honda发现受光辐照的TiO2单晶电极可以将H2O分解,利用TiO2半导体光催化剂将光能转化为电能和化学能就成为半导体光催化领域的研究热点。然而,锐钛矿型TiO2的禁带宽度为3.2eV,其激发波长为387.5nm,属于太阳光中的紫外光范围。而对于太阳能,其主要能量集中于400~600nm的可见光范围,这大大减少了TiO2半导体光催化剂的效率,因此,开发出对可见光响应的新型的半导体材料是半导体光催化剂研究的重点内容之一。
目前,在众多的新开发的半导体光催化剂中,研究者开发了钨酸盐化合物,发现该类催化剂具有较小的禁带宽度,能充分的利用太阳光,是一类有前景的光催化剂。但是随着研究的深入,研究者发现大多数的钨酸盐化合物出现稳定性差,易光腐蚀等缺陷,限制了其发展。
发明内容
为弥补现有技术的不足,本发明提供一种不仅具有可见光响应的、对有机污染物具有降解能力而且稳定性好、不易腐蚀的光催化剂Bi2WO6/SnO2纳米片及制备方法。
本发明是这样实现的,水热法合成具有可见光响应的光催化剂Bi2WO6/SnO2纳米片的制备方法,包括如下步骤:
S1.纯Bi2WO6和混合Bi2WO6样品均采用水热法合成。
将1mmol Na2WO4·2H2O,1.98mmol Bi(NO3)3·5H2O溶于100mL蒸馏水,搅拌30min,得到的淡黄色的悬浮液。将悬浮液转移到100mL高压反应釜中90℃-220℃反应12-36小时,反应结束后,自然冷却、过滤、洗涤,于60℃干燥24小时,得到产品纯Bi2WO6。
S2.Bi2WO6/SnO2纳米片的合成:
向乙二醇中加入Bi2WO6,搅拌获得Bi2WO6悬浊液;将Bi2WO6悬浊液加入到SnCl4·5H2O中制备混合悬浮液,配制尿素水溶液,将尿素水溶液迅速加入混合悬浮液中,并在室温下搅拌1小时,然后转移到反应釜中加热150-210℃12-24小时,经洗涤、80℃干燥24小时;最后制得Bi2WO6/SnO2纳米片,其中Bi2WO6占SnO2质量的24.47%-88.13%。
本发明通过一锅法合成具有可见光响应的光催化剂Bi2WO6/SnO2纳米片,同时通过控制反应时间以及反应温度,形成大比表面积的球状形貌,使得制备的材料具有较大的比表面积,有利于污染物的吸附降解。
本发明另一个目的是请求保护采用本发明方法制备的Bi2WO6/SnO2纳米片催化降解液相污染物的方法,具体步骤如下:称取100mgBi2WO6/SnO2纳米片,加入5mg/L 100mL苯酚溶液中,在暗环境下磁力搅拌30min,然后放入氙光灯下边搅拌边照射,进行催化反应。
本发明的通过合理的调控Bi2WO6和SnO2配比,调节工艺参数,将纳米片经溶剂热反应获得微观结构为片状纳米级复合物Bi2WO6/SnO2。与现有技术相比,本发明具有以下优点:
1、本发明制备的Bi2WO6/SnO2纳米片的比表面积大,吸附能力强;
2、本发明制备的Bi2WO6/SnO2纳米片与传统光催化剂二氧化钛相比,具有更好的可见光吸收性能,对光催化氧化降解有机污染物有很大的提高;
3、本发明提供的Bi2WO6/SnO2纳米片的制备方法比较简单,易于操作,适于工业生产。
附图说明
图1为实施例1中的Bi2WO6/SnO2纳米片放大倍数8000倍的扫描电镜图。
图2为实施例1和实施例2中的Bi2WO6/SnO2纳米片XRD衍射图谱。
图3为实施例1中的Bi2WO6/SnO2纳米片UR-Vis DRS光谱分析图。
图4为实施例1中的不同含量的Bi2WO6/SnO2异质结构光降解数据图。
具体实施方式
下面通过附图和具体实施例详述本发明,但不限制本发明的保护范围。如无特殊说明,本发明所采用的实验方法均为常规方法,所用实验器材、材料、试剂等均可从化学公司购买。应用例中涉及到光催化TiO2,型号P25,购买于赢创工业集团。
实施例1
(1)将1mmol Na2WO4·2H2O,1.98mmol Bi(NO3)3·5H2O溶于100mL蒸馏水,搅拌30min,得到的淡黄色的悬浮液,将悬浮液转移到100mL不锈钢高压反应釜中保持在180℃24小时。自然冷却后,产物过滤,用去离子水和乙醇反复洗涤,然后在60℃干燥24小时制得纯Bi2WO6。
(2)50mL乙二醇中加入0.7g Bi2WO6,搅拌3小时获得Bi2WO6悬浊液。向Bi2WO6悬浊液中加入0.7g SnCl4·5H2O获得混合悬浮液。向30mL去离子水中加入0.4g尿素,获得尿素水溶液。将尿素水溶液迅速加入混合悬浮液中,在室温下搅拌1小时,然后转移到聚四氟乙烯内衬钢反应釜,于180℃加热16小时,收集,用去离子水多次洗涤,于80℃干燥24小时,最后得到72.12wt%-Bi2WO6/SnO2纳米片。
实施例2
(1)将1mmol Na2WO4·2H2O,1.98mmol Bi(NO3)3·5H2O溶于100mL蒸馏水,搅拌30min,得到的淡黄色的悬浮液,将悬浮液转移到100mL不锈钢高压反应釜中保持在90℃36小时。自然冷却后,产物过滤,用去离子水和乙醇反复洗涤,然后在60℃干燥24小时制得纯Bi2WO6。
(2)50mL乙二醇中加入0.7g Bi2WO6,搅拌3小时获得Bi2WO6悬浊液。向Bi2WO6悬浊液中加入0.86g SnCl4·5H2O获得混合悬浮液。同时,30mL去离子水中加入0.4g尿素,获得尿素水溶液。将尿素水溶液迅速加入混合悬浮液中,在室温下搅拌1小时,然后转移到聚四氟乙烯内衬钢反应釜,于150℃加热24小时,收集和去离子水多次洗涤,于80℃干燥24小时,最后得到88.13wt%-Bi2WO6/SnO2纳米片。
实施例3
(1)将1mmol Na2WO4·2H2O,1.98mmol Bi(NO3)3·5H2O溶于100mL蒸馏水,搅拌30min,得到的淡黄色的悬浮液,将悬浮液转移到100mL不锈钢高压反应釜中保持在220℃12小时。自然冷却后,产物过滤,用去离子水和乙醇反复洗涤,然后在60℃干燥24小时制得纯Bi2WO6。
(2)50mL乙二醇中加入0.7g Bi2WO6,搅拌3小时获得Bi2WO6悬浊液。向Bi2WO6悬浊液中加入0.86g SnCl4·5H2O获得混合悬浮液。同时,30mL去离子水中加入0.4g尿素,获得尿素水溶液。将尿素水溶液迅速加入混合悬浮液中,在室温下搅拌1小时,然后转移到聚四氟乙烯内衬钢反应釜,于150℃加热24小时,收集和去离子水多次洗涤,于80℃干燥24小时,最后得到88.13wt%-Bi2WO6/SnO2纳米片。
实施例4
(1)将1mmol Na2WO4·2H2O,1.98mmol Bi(NO3)3·5H2O溶于100mL蒸馏水,搅拌30min,得到的淡黄色的悬浮液,将悬浮液转移到100mL不锈钢高压反应釜中保持在90℃36小时。自然冷却后,产物过滤,用去离子水和乙醇反复洗涤,然后在60℃干燥24小时制得纯Bi2WO6。
(2)50mL乙二醇中加入0.7g Bi2WO6,搅拌3小时获得Bi2WO6悬浊液。向Bi2WO6悬浊液中加入0.23g SnCl4·5H2O获得混合悬浮液。同时,30mL去离子水中加入0.4g尿素,获得尿素水溶液。将尿素水溶液迅速加入混合悬浮液中,在室温下搅拌1小时,然后转移到聚四氟乙烯内衬钢反应釜,于150℃加热24小时,收集和去离子水多次洗涤,于80℃干燥24小时,最后得到24.47wt%-Bi2WO6/SnO2纳米片。
应用例1
购买商业光催化TiO2,未经过任何处理,直接用于光催化反应作为对比。
按实施例1中的方法制备Bi2WO6/SnO2纳米片,取100mg纯Bi2WO6,加入5mg/L 100mL苯酚溶液中,在暗环境下磁力搅拌30min,之后放入氙光灯下边搅拌边照射,每15min取一次样品,取出的样品在2000r/min下离心20min,再用移液枪取出上清液,然后在510nm出测其吸光度,并记录数据。
实验结果如图4所示,在可见光条件下,纯Bi2WO6纳米片作为催化剂时对苯酚具有一般的催化氧化活性。
应用例2
购买商业光催化TiO2,未经过任何处理,直接用于光催化反应作为对比。
按实施例1中的方法制备72.12%Bi2WO6/SnO2纳米片,取100mg72.12%Bi2WO6/SnO2纳米片,加入5mg/L 100mL苯酚溶液中,在暗环境下磁力搅拌30min,之后放入氙光灯下边搅拌边照射,每15min取一次样品,取出的样品在2000r/min下离心20min,再用移液枪取出上清液,然后在510nm出测其吸光度,并记录数据。
实验结果如图4所示,在可见光条件下,72.12%Bi2WO6/SnO2纳米片作为催化剂时,在可见光条件下,对液相污染物具有较强的催化氧化活性。
以上所述,仅为本发明创造较佳的具体实施方式,但本发明创造的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明创造披露的技术范围内,根据本发明创造的技术方案及其发明构思加以等同替换或改变,都应涵盖在本发明创造的保护范围之内。
Claims (4)
1.简易水热法合成具有可见光响应的光催化剂Bi2WO6/SnO2纳米片的制备方法,其特征在于,包括如下步骤:
向乙二醇中加入Bi2WO6,搅拌获得Bi2WO6悬浊液;将Bi2WO6悬浊液加入到SnCl4·5H2O中制备混合悬浮液,配制尿素水溶液,将尿素水溶液迅速加入混合悬浮液中,并在室温下搅拌1小时,然后转移到反应釜中加热150-210℃12-24小时,经洗涤、80℃干燥24小时;最后制得Bi2WO6/SnO2纳米片,其中Bi2WO6占SnO2质量的24.47%-88.13%。
2.根据权利要求1所述的方法,其特征在于,Bi2WO6的制备方法具体为:将1mmolNa2WO4·2H2O,1.98mmol Bi(NO3)3·5H2O溶于100mL蒸馏水,搅拌30min,得到悬浮液,将悬浮液转移到100mL高压反应釜中90℃-220℃反应12-36小时,反应结束后,自然冷却、过滤、洗涤,于60℃干燥24小时,得到Bi2WO6。
3.如权利要求1所述的纳米片Bi2WO6/SnO2催化降解液相污染物的方法,其特征在于,具体步骤如下:取100mg样品Bi2WO6/SnO2,加入5mg/L 100mL液相污染物中,在暗环境下磁力搅拌30min,然后放入氙光灯下边搅拌边照射,进行催化反应。
4.根据权利要求3所述的方法,其特征在于,所述液相污染物为苯酚。
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