CN107754819B - 一种合成具有可见光响应的光催化剂SnS2/Bi2WO6纳米片的制备方法 - Google Patents
一种合成具有可见光响应的光催化剂SnS2/Bi2WO6纳米片的制备方法 Download PDFInfo
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Abstract
一种合成具有可见光响应的光催化剂SnS2/Bi2WO6纳米片的制备方法,先采用水热法制备Bi2WO6,再将SnCl4·5H2O溶解于乙酸与乙醇混合溶液中,然后加入Bi2WO6,进行超声处理,处理结束后再加入硫代乙酰胺获得混合溶液,室温搅拌5小时后将混合溶液放入高温反应釜中,于120℃~220℃的条件下反应8~16小时后自然冷却至室温,反应结束后对产物过滤、洗涤、干燥最终获得SnS2/Bi2WO6。本发明SnS2/Bi2WO6的比表面积大,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SnS2/Bi2WO6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、不易腐蚀的可见光响应的光催化剂 SnS2/Bi2WO6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SnS2/Bi2WO6纳米片的制备方法,包括如下步骤:
先采用水热法制备Bi2WO6,将SnCl4·5H2O溶解于乙酸与乙醇混合溶液中,其中乙酸与乙醇的的体积比为1:19,搅拌溶解后加入Bi2WO6,然后进行超声处理,处理结束后再加入硫代乙酰胺,在磁力搅拌器室温搅拌5小时后将混合溶液放入高温反应釜中,于120℃~220℃的条件下的高温加热8~16小时后自然冷却至室温,反应结束后对产物过滤、洗涤、干燥最终获得SnS2/Bi2WO6。所述的Bi2WO6、SnCl4·5H2O和硫代乙酰胺的摩尔比范围为:1:(1.5~9):(3-18)。
作为优选,水热法制备Bi2WO6的具体方法为:称取1mmolNa2WO4·2H2O, 1.98mmolBi(NO3)·5H2O混合,注入100mL去离子水,并在磁力搅拌器上匀速搅拌30分钟,得混合溶液,搅拌结束后,将混合溶液全部转移注入到100mL高温反应釜中,于高温反应釜中在180℃的条件下加热24小时后自然冷却至室温,高温反应结束后,将样品静置一定时间后倾出上清液,然后对剩下产物进行过滤。将过滤产物用去离子水与乙醇反复洗涤,洗涤后将浊液放入培养箱于60℃干燥 24小时,得到淡黄色粉末状固体即为Bi2WO6。
本发明中通过合成具有可见光响应的光催化剂SnS2/Bi2WO6纳米片,同时通过控制反应时间以及反应温度,形成大比表面积的鳞片状形貌,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SnS2/Bi2WO6纳米片催化降解液相污染物的方法,具体步骤如下:称取0.1g SnS2/Bi2WO6纳米片溶解于10mL的5mg/L苯酚溶液中,先在磁力搅拌器中暗反应搅拌1小时后采用氙灯照射,将氙灯置于一定高度,自上而下的对反应液进行垂直照射,照射的同时将混合溶液置于磁力搅拌器上进行搅拌,进行催化反应1-2小时。
与现有技术相比,本发明具有以下优点:
1、本发明制备的SnS2/Bi2WO6纳米片的比表面积大,吸附能力强;
2、本发明制备的SnS2/Bi2WO6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SnS2/Bi2WO6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SnS2/Bi2WO6纳米片放大倍数4800倍的扫描电镜图。
图2为实施例2中的纯Bi2WO6在4800倍的扫描电镜图。
图3为实施例1中的Sn2S/Bi2WO6纳米片与Bi2WO6光催化降解苯酚中吸光度对比图。
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
称取1mmol的Na2WO4·2H2O和1.98mmol的Bi(NO3)·5H2O,注入100mL 去离子水,并在磁力搅拌器上匀速搅拌30分钟,获得混合溶液。搅拌结束后,将混合溶液全部转移注入到100mL高温反应釜中,于高温反应釜中在180℃的条件下高温加热24小时后自然冷却至室温。高温反应结束后,将产物从反应釜中倒入烧杯,静置一定时间后倾出上清液,然后对剩下产物进行过滤。将过滤产物用去离子水与乙醇反复洗涤,洗涤后将浊液放入培养箱于60℃干燥24小时,得到淡黄色粉末状固体即为Bi2WO6。
采用水热法合成光催化剂SnS2/Bi2WO6:称取5mmol的SnCl4·5H2O溶解于2mL乙酸与38mL乙醇混合溶液中,搅拌溶解后加入0.6g的Bi2WO6。然后进行15分钟的超声处理以完全溶解,再加入10mmol硫代乙酰胺于上述混合物中,在磁力搅拌器上室温搅拌5小时。搅拌完成后将混合物放入50mL高温反应釜中,于180℃的条件下高温加热12小时后自然冷却至室温;高温反应结束后,将产物从反应釜中倒入烧杯,对产物进行过滤。将过滤后的产物用去离子水和乙醇反复洗涤,洗涤后放入培养箱于80℃干燥4小时,得到浅灰的粉末状固体即为SnS2/Bi2WO6。
实施例2
本实施例与实施例1的区别仅在于未加入SnS2,制得纯Bi2WO6纳米片光催化剂。
实施例3
本实施例与实施例1的区别仅在于SnS2占Bi2WO6质量的50wt%,在220℃下反应16h,制得SnS2/Bi2WO6纳米片光催化剂。
实施例4
本实施例与实施例1的区别仅在于SnS2占Bi2WO6质量的30wt%,在120℃下反应8h,制得SnS2/Bi2WO6纳米片光催化剂。
应用例
SnS2/Bi2WO6复合光催化剂的光催化活性通过在可见光的照射下降解苯酚溶液来进行检测。称取0.1g SnS2/Bi2WO6样品溶解于10mL的5mg/L苯酚溶液中,先在磁力搅拌器中暗反应搅拌1小时后采用氙灯照射,为保证照射的均匀程度,保证实验的准确性,将氙灯置于一定高度,自上而下的对实验样品反应液进行垂直照射,照射的同时放置磁力搅拌器,将混合溶液置于其上进行搅拌,使得混合及照射更加均匀。在光照下匀速搅拌1小时后,每隔15分钟吸取3mL悬浊液在离心机中于8000r/min离心3分钟两次后,取上清液在510nm处,用10mm玻璃比色皿,以水为参比测量其吸光度,通过吸光度计算苯酚的去除率。
实验结果见图3所示,在可见光条件下,SnS2/Bi2WO6纳米片作为催化剂时,经过120min降解,效果优于Bi2WO6,因此,在可见光条件下,SnS2/Bi2WO6纳米片对气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 (2)
1.一种合成具有可见光响应的光催化剂SnS2/Bi2WO6纳米片的制备方法,其特征在于,包括如下步骤:
先采用水热法制备Bi2WO6,再将SnCl4·5H2O溶解于乙酸与乙醇混合溶液中,然后加入Bi2WO6进行超声处理,处理结束后再加入硫代乙酰胺获得混合溶液,室温搅拌后将混合溶液放入高温反应釜中,于120℃~220℃的条件下反应8~16小时后自然冷却至室温,反应结束后对产物过滤、洗涤、干燥最终获得鳞片状形貌的SnS2/Bi2WO6;
所述的Bi2WO6、SnCl4·5H2O和硫代乙酰胺的摩尔比范围为:1:(1.5~9):(3-18);所述SnS2占Bi2WO6质量的30wt%~50wt%;
Bi2WO6的制备方法具体为:称取1mmolNa2WO4·2H2O,1.98mmol Bi(NO3)·5H2O混合,注入100mL去离子水,并在磁力搅拌器上匀速搅拌30分钟,得混合溶液,搅拌结束后,将混合溶液全部转移注入到100mL高温反应釜中,在180℃的条件下加热24小时后自然冷却至室温,反应结束后,静置、倾出上清液,对产物进行过滤、洗涤、干燥,得到Bi2WO6。
2.如权利要求1所述的制备方法制备的纳米片SnS2/Bi2WO6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SnS2/Bi2WO6,加入5mg/L 10mL液相污染物中,在暗环境下磁力搅拌,然后放入氙光灯下边搅拌边照射进行催化反应1-2小时;所述的液相污染物为苯酚。
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