CN109999787A - 一种零维/一维异质结构钒酸铋/氧化锆纳米带光催化剂及制备方法 - Google Patents
一种零维/一维异质结构钒酸铋/氧化锆纳米带光催化剂及制备方法 Download PDFInfo
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Abstract
本发明公开了一种零维/一维异质结构钒酸铋/氧化锆纳米带光催化剂及制备方法,具体是首先使用水热法制备出钒酸铋量子点,后将氧氯化锆与钒酸铋量子点加入到PVP的DMF与水溶液中进行超声与搅拌处理,使其混合均匀生成电纺溶胶并使用静电纺丝法得到BiVO4/ZrO2的纤维膜,后经过煅烧处理得到BiVO4/ZrO2纳米带光催化剂。本发明的特点是使用水热法与静电纺丝法两步结合,后结合煅烧工艺制备出BiVO4/ZrO2纳米带光催化剂,这可以使BiVO4量子点均匀的负载到ZrO2纳米带上,极大的增加了催化剂的比表面积,使其具有更多的活性位点,并且通过异质结构的形成有效的促进了电子的传输效率并降低电子空穴的复合率,使制备的催化剂具有很高的光催化活性。
Description
技术领域
本发明属于光催化技术领域,具体为钒酸铋量子点以及氧化锆纳米带材料的制备方法。
背景技术
在科技迅速发展,工业经济发达的当今社会,环境污染的治理成为人们面临的首要问题之一。由于具有环境友好的特点,光催化在治理环境污染中的应用越来越引起人们的关注。它可用于各种方面,如净水、杀菌、自洁、空气净化、防雾和散热等,并且由于其具有较低的成本、高成效等优点,半导体光催化剂逐渐成为处理水污染领域的研究热点。
传统光催化剂TiO2自1972年Fujishima和Honda(Nature 1972, 238, 37-8)用其做为电极将水电解成H2和O2以来,由于其具有成本低、效率高、稳定性好等诸多优点引起人们广泛的关注。但是由于其较大的禁带宽度(~3.2eV)决定其不能吸收可见光,严重限制了其应用。为了克服这个缺点,人们对新型光催化剂给予了极大的关注,其中最让人感到兴奋是可见光活性铋基光催化剂,而钒酸铋又以其较小的带隙(~2.4eV)从中脱颖而出。但是经过人们长期研究发现,虽然其吸光范围更大,但单一钒酸铋半导体光催化剂由于其较高的电子空穴复合率导致其光催化活性并不理想,而通过与其他物质构建异质结构可以有效的减小电子空穴的复合。目前已经有许多课题组对钒酸铋异质结构光催化进行了研究,例如Meryam Zalfani(J.Mater.Chem.A, 2014, 00,1-3)等人使用水热法制备了BiVO4/TiO2异质结构纳米复合材料,发现其对罗丹明B的降解效率相对单纯的BiVO4纳米颗粒提升了大约四倍。而相对TiO2,ZrO2具有相对其更加稳定的性质,且静电纺丝得到的ZrO2纳米带以及BiVO4量子点具有更大的比表面积,通过两步法将钒酸铋量子点负载到氧化锆纳米带上会使其吸光度大大增强,且在其表面形成更多的活性位点,这些优势都非常有利于其对污染物的降解及光催化效率的提升。
发明内容
本发明目的是利用构建钒酸铋量子点和氧化锆纳米带的异质结构获得具有高光催化活性的催化剂。
为实现本发明的目的,提供以下技术方案:
一种零维/一维异质结构钒酸铋/氧化锆纳米带光催化剂及制备方法,包括步骤如下:
(1)将油酸钠置于去离子水中,并在室温下搅拌30min获得质量浓度0.1%的油酸钠溶液A;
(2)将硝酸铋以及偏钒酸铵加入溶液A中,室温下搅拌10~10min;
(3)将溶液A加入到反应釜中并且在90℃的烘箱中加热反应6~10h;
(4)将反应完成后的溶液进行多次离心并将所得物质使用乙醇及去离子水多次洗涤以获得钒酸铋量子点;
(5)将聚乙烯吡咯烷酮(PVP)溶于N,N-二甲基甲酰胺和少量去离子水的混合溶剂中并搅拌均匀获得溶液B;
(6)将氧氯化锆以及钒酸铋量子点加入到PVP质量浓度约为10~20%的溶液B中,超声20~40min后室温搅拌2h获得可纺溶胶;
(7)将制得的可纺溶胶加入到注射器针管中,进行静电纺丝;
(8)将静电纺丝制得的纤维膜进行煅烧,得到钒酸铋量子点负载的氧化锆纳米带。
根据本发明,优选的,步骤(1)中,油酸钠的质量浓度为0.09%。
根据本发明,优选的,步骤(2)中,硝酸铋的质量浓度为0.12%,偏钒酸铵的质量浓度为0.1%。
根据本发明,优选的,步骤(3)中,加热时间为8h。
根据本发明,优选的,步骤(5)中,PVP质量浓度为 10%。
根据本发明,优选的,步骤(6)中,氧氯化锆和钒酸铋量子点摩尔比为1:1。
根据本发明,优选的,步骤(8)中,煅烧的温度为500℃,煅烧速率为1℃/min,保温时间为60min。
本发明是采用钒酸铋量子点与氧化锆纳米带构建异质结构纳米级别光催化剂,将钒酸铋量子点负载到氧化锆纳米带上,使氧化锆纳米带的比表面积大大增加,增强了催化剂对太阳光的吸收能力,进一步提高了光催化活性。利用水热与静电纺丝两步法相结合制备出异质结构光催化剂,有效的促进了电子转移并且大大降低了光生电子空穴的复合率,明显提高了光催化剂的光催化效率。
附图说明
图1为本发明实例1的实验流程图。
图2为本发明实例1的XRD图。
图3为本发明实例1的扫描电镜图。
图4为本发明实例1的透射电镜图。
图5为本发明实例1的污染降解性能对比曲线图。
图6为本发明实例1的罗丹明B降解紫外曲线。
图7为本发明实例1的氮气吸脱附及孔径分布曲线。
具体实施方式
以下实施例旨在说明本发明而不是对本发明的进一步限定。
实施例1:
(1)将0.730g油酸钠置于80mL去离子水中,并在室温下搅拌30min获得质量浓度约为0.1%的油酸钠溶液A;
(2)将0.097g硝酸铋以及0.080g偏钒酸铵加入溶液A中,室温下搅拌10~10min;
(3)将溶液A加入到反应釜中并且在90℃的烘箱中加热反应8h;
(4)将反应完成后的溶液进行多次离心并将所得物质使用乙醇及去离子水多次洗涤以获得钒酸铋量子点;
(5)将1.0g聚乙烯吡咯烷酮(PVP)溶于10mL N,N-二甲基甲酰胺和1mL去离子水的混合溶剂中并搅拌均匀获得溶液B;
(6)将0.064g氧氯化锆以及0.065g钒酸铋量子点加入到溶液B中,超声20~40min后室温搅拌2h获得可纺溶胶;
(7)将制得的可纺溶胶加入到注射器针管中,进行静电纺丝;
(8)将静电纺丝制得的纤维膜进行煅烧,得到钒酸铋量子点负载的氧化锆纳米带;
对本实例制得的产物进行电镜扫描,如图所示,制备的纳米带尺寸在100~150nm左右。
实施例2:
(1)将0.730g油酸钠置于80mL去离子水中,并在室温下搅拌30min获得质量浓度约为0.1%的油酸钠溶液A;
(2)将0.097g硝酸铋以及0.080g偏钒酸铵加入溶液A中,室温下搅拌10~10min;
(3)将溶液A加入到反应釜中并且在90℃的烘箱中加热反应6h;
(4)将反应完成后的溶液进行多次离心并将所得物质使用乙醇及去离子水多次洗涤以获得钒酸铋量子点。
实施例3:
(1)将1.0g聚乙烯吡咯烷酮(PVP)溶于10mL N,N-二甲基甲酰胺和1mL去离子水的混合溶剂中并搅拌均匀获得溶液A;
(2)将0.064g氧氯化锆加入到溶液A中,超声20~40min后室温搅拌2h获得可纺溶胶;
(3)将制得的可纺溶胶加入到注射器针管中,进行静电纺丝;
(4)将静电纺丝制得的纤维膜进行煅烧,得到氧化锆纳米带。
实验例
通过硝基苯(NB)以及罗丹明B(RhB)的吸附及光催化降解实验,测试BiVO4/ZrO2异质结构纳米带的光催化性能。
光催化反应在圆柱形玻璃容器内常温下进行,采用光源浸没式进行反应,光源为800W氙灯,以NB及RhB作为模拟污染物来评价异质结构纳米带的污染物清除性能。实验过程中,分别将60mg BiVO4量子点、ZrO2纳米带以及BiVO4/ZrO2异质结构纳米带样品置于NB(RhB)溶液(50mg/L),在黑暗条件下磁力搅拌并暗反应60min,当NB(RhB)溶液与样品达到吸附平衡以后打开氙灯进行光照。每隔30min取样4mL,经针头过滤器过滤后使用紫外可见光光度计测定滤液的吸光度并计算残余的NB(RhB)浓度。图5为实施例1所制备的BiVO4/ZrO2异质结构纳米带与BiVO4量子点及ZrO2纳米带的降解效率对比,可以看出实施例1制备的BiVO4/ZrO2异质结构纳米带降解效率最高。
Claims (7)
1.一种零维/一维异质结构钒酸铋/氧化锆纳米带光催化剂,其特征在于,该催化剂由钒酸铋量子点、氧化锆纳米带组成。
2.根据权利要求1所述的零维/一维异质结构钒酸铋/氧化锆纳米带光催化剂,其特征在于,所述的催化剂钒酸铋为单斜相,氧化锆为四方相。
3.根据权利要求1所述的零维/一维异质结构钒酸铋/氧化锆纳米带光催化剂,其特征在于,按物质的量百分比计:钒酸铋含量50%,氧化锆含量50%。
4.根据权利要求1所述的零维/一维异质结构钒酸铋/氧化锆纳米带光催化剂,其特征在于,所述的催化剂的比表面积为44.45m2/g。
5.根据权利要求1所述的零维/一维异质结构钒酸铋/氧化锆纳米带光催化剂,其特征在于,所述的催化剂在可见光下对50mg/L硝基苯210分钟的降解率达到95.1%。
6.根据权利要求1所述一种零维/一维异质结构钒酸铋/氧化锆纳米带光催化剂及制备方法,其特征在于溶剂为去离子水、N,N-二甲基甲酰胺的至少一种。
7.一种权利要求1所述的零维/一维异质结构钒酸铋/氧化锆纳米带光催化剂的制备方法,包括步骤如下:
(1)将油酸钠置于去离子水中,并在室温下搅拌30min获得质量浓度0.1%的油酸钠溶液A;
(2)将硝酸铋以及偏钒酸铵加入溶液A中,室温下搅拌10~20min;
(3)将溶液A加入到反应釜中并且在90℃的烘箱中加热反应8~12h;
(4)将反应完成后的溶液进行多次离心并将所得物质使用乙醇及去离子水多次洗涤以获得钒酸铋量子点;
(5)将聚乙烯吡咯烷酮(PVP)溶于N,N-二甲基甲酰胺和少量去离子水的混合中并搅拌均匀获得溶液B;
(6)将氧氯化锆以及钒酸铋量子点加入到PVP质量浓度约为10~20%的溶液B中,超声20~40min后室温搅拌2 h获得可纺溶胶;
(7)将制得的可纺溶胶加入到注射器针管中,进行静电纺丝;
(8)将静电纺丝制得的纤维膜进行煅烧,得到钒酸铋量子点负载的氧化锆纳米带。
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