CN110180565B - 一种光催化剂Bi5O7Br的合成方法及其应用 - Google Patents
一种光催化剂Bi5O7Br的合成方法及其应用 Download PDFInfo
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Abstract
一种光催化剂Bi5O7Br的合成方法及其应用,属于纳米材料技术领域,可解决现有Bi5O7Br催化剂的制备需要高温高压,长时间反应和有机溶剂溶解等条件的问题,本发明以五水硝酸铋和溴酸钠为原料,以氨水为pH值调节剂,利用简单经济环保的常温水解法制得带隙较窄、可见光响应能力较强、组成单一的Bi5O7Br光催化剂,本发明所用原料廉价易得,不使用有机溶剂,所用方法简单易行、经济环保,不产生有毒有害副产物,所用条件常温常压、简单安全,易于实现工业化生产。
Description
技术领域
本发明属于纳米材料技术领域,具体涉及一种光催化剂Bi5O7Br的合成方法及其应用,可以用于降解环境中的药物。
背景技术
近年来,药物制剂被频频的在饮用水中检测到,严重威胁到了生态环境和人体健康,此类新型的药物污染问题已成为了全球和我国所面临的重大环境问题之一。多相光催化氧化技术由于高效节能、低成本,操作简单和可持续应用,而在药物去除技术中表现出了良好的应用前景。
在众多的光催化剂中,BiOBr半导体光催化剂由于其独特的开放式层状结构、间接跃迁模式以及优良的光催化活性,在其被发现之时就受到了各国科研工作者们的青睐和关注。但其活性仍受到一系列诸如太阳光响应能力低、光生电子-空穴对复合率高以及氧化还原能力弱等因素的制约。从物质本质属性出发,上述制约因素均与催化剂的价带和导带位置有关,而对于Bi-O-Br三元化合物来说其价带主要由Br 4p和O 2p轨道组成,导带主要由Bi 6p轨道组成,通过调控BiOBr催化剂中Br、O、Bi三种元素的比值可以有效地改变催化剂的带隙结构,使其具有更强的可见光响应能力和光生电子-空穴氧化还原能力(Journal ofmaterials chemistry 2012, 45 (5), 2688-2697、RSC advances 2016, 6 (53), 47545-47551、Journal of the Taiwan Institute of Chemical Engineers 2014, 45 (4),1892-1909),进而改善催化剂的性能。因此,寻找一种简单有效的调控方法制备高活性的非化学计量比BiOBr光催化剂成为了该领域的研究重点。
在目前所制的非化学计量比BiOBr催化剂中,Bi5O7Br由于其导带电子的还原能力更强,电子空穴对的分离效率更好而表现出了优异的有机污染物降解活性。如叶立群等人首次利用水热法合成了Bi5O7Br,且可以有效地降解罗丹明B(LiQun Ye et al. AppliedSurface Science. 2015, 346, 311–316);中国专利申请“一种带状结构的Bi5O7Br纳米光催化材料的制备方法”(专利申请号201710184498.5)成功制备出带状催化剂,且在50分钟内可以降解甲基橙93.4%;中国专利申请“可见光催化剂Bi5O7Br及其制备方法”(专利申请号201410029932.9)采用改进低温水热法,首次制备出十字星型的Bi5O7Br,且可以有效地降解罗丹明B和甲基橙。然而,目前报道的此类催化剂的制备均需要高温高压,长时间反应和有机溶剂溶解等条件,因此寻找出一种简单经济环保的制备方法,可以有效响应可见光且对难降解药物有较好催化活性的Bi5O7Br催化剂,具有重大的意义,同时也是光催化技术领域一项长期而艰巨的任务。
发明内容
本发明针对现有Bi5O7Br催化剂的制备需要高温高压,长时间反应和有机溶剂溶解等条件的问题,提供一种光催化剂Bi5O7Br的合成方法及其应用,本发明的目的是提供一种简单经济环保的常温水解法,以制备出一种带隙较窄、可见光响应能力较强、组成单一的新型光催化剂,从而达到对太阳能的充分有效利用以及降解水体中残留药物之功效。
本发明采用如下技术方案:
一种光催化剂Bi5O7Br的合成方法,包括如下步骤:
第一步,称取0.485~7.275 g的五水硝酸铋,将其放置于20~60 mL的蒸馏水中,在室温下搅拌1~3 h,直至完全溶解,记为溶液A;
第二步,称取0.151~2.265 g的溴酸钠,将其放置于15~50 mL蒸馏水中,在室温下搅拌1~3 h,直至溶液变为澄清,记为溶液B;
第三步,将溶液B加入溶液A中,搅拌使其混合均匀,加入1~3 mL氨水调节pH为7~10,并在室温下继续搅拌反应1~6 h,即可得到沉淀;
第四步,将沉淀抽滤分离,用蒸馏水和无水乙醇分别洗涤2-3次,在50~70 ℃下烘干,即得到可见光响应较强、带隙为2.52-2.92 eV可用于降解水中微量难降解药物的光催化剂Bi5O7Br。
一种光催化剂Bi5O7Br应用于水中微量难降解的卡马西平或盐酸四环素的降解。
一种光催化剂Bi5O7Br应用于水中微量难降解的卡马西平或盐酸四环素的降解,反应条件为:常温常压,光催化剂用量为0.05g,卡马西平或盐酸四环素的处理量为50~100mL、10 mg·L-1,所用光源为氙灯,功率为500 W,照度为120 klx,距离反应界面20 cm, 所发光为波长大于420 nm的可见光。
本发明的有益效果如下:
1. 本发明所用原料廉价易得,不使用有机溶剂,所用方法简单易行、经济环保,不产生有毒有害副产物,所用条件常温常压、简单安全,易于实现工业化生产;
2. 本发明所制催化剂组成单一,带隙较窄、可见光响应能力较强,且价带上空穴的氧化能力较强;
3. 相比较于传统的TiO2(P25)和BiOBr光催化剂,本发明所制Bi5O7Br催化剂在可见光下表现出了良好的光催化活性,且性能稳定,可重复使用,对环境治理和绿色能源利用具有重要意义。
附图说明
图1为实施例1所制备的Bi5O7Br光催化剂的XRD图谱;
图2为实施例1所制备的Bi5O7Br光催化剂的DRS图谱。
具体实施方式
实施例1
将4.85 g Bi(NO3)3·5H2O加入到50 mL蒸馏水中在室温下搅拌1.5 h,将1.51 gNaBrO3加入到40 mL蒸馏水中在室温下搅拌1.5 h,将两种溶液混合,加入2.5 mL氨水调节溶液pH,并在此条件下连续反应3 h,直至沉淀生成,最后对所得沉淀进行分离、洗涤烘干,即可得到Bi5O7Br催化剂,记为Bi5O7Br-A。
所得Bi5O7Br-A光催化剂用于光催化降解卡马西平和盐酸四环素溶液。其反应条件为:常温常压,催化剂用量为0.05 g,水中微量药物污染物卡马西平或者盐酸四环素的处理量为100 mL、10 mg·L-1,所用光源为氙灯,功率为500 W,照度为120 klx,距离反应界面20cm, 所发光为波长大于420 nm的可见光,首先在避光条件下吸附0.5 h,以期达到吸附平衡;然后打开光源,对卡马西平或者盐酸四环素溶液进行光催化降解实验,每隔30 min取样一次,利用紫外-可见分光光度法对溶液中剩余待降解物的浓度进行分析并计算其降解率,结果如表1和表2所示。实施例1所制备样品的XRD图见图1,其谱图与Bi5O7Br标准卡(PDF#97-024-1125)相一致,基本没有杂峰的存在。所制备样品的紫外漫反射光谱(DRS)图见图2,由图可知,本发明的Bi5O7Br从紫外光区到可见光区都有一定的吸收,最大吸收波长达到410nm,其禁带宽度为2.802eV。
实施例2
将0.485 g Bi(NO3)3·5H2O加入到20 mL蒸馏水中在室温下搅拌1.5 h,将0.151gNaBrO3加入到15 mL蒸馏水中在室温下搅拌1.5 h,将两种溶液混合,加入1 mL氨水调节溶液pH,并在此条件下连续反应3 h,直至沉淀生成,最后对所得沉淀进行分离、洗涤烘干,即可得到Bi5O7Br催化剂,记为Bi5O7Br-B。
所得Bi5O7Br-B光催化剂用于光催化降解卡马西平和盐酸四环素溶液。其反应条件为:常温常压,催化剂用量为0.05 g,水中微量药物污染物卡马西平或者盐酸四环素的处理量为100 mL、10 mg·L-1,所用光源为氙灯,功率为500 W,照度为120 klx,距离反应界面20cm, 所发光为波长大于420 nm的可见光,首先在避光条件下吸附0.5 h,以期达到吸附平衡;然后打开光源,对卡马西平或者盐酸四环素溶液进行光催化降解实验,每隔30 min取样一次,利用紫外-可见分光光度法对溶液中剩余待降解物的浓度进行分析并计算其降解率,结果如表1和表2所示。
实施例3
将4.85 g Bi(NO3)3·5H2O加入到50 mL蒸馏水中在室温下搅拌1.5 h,将1.51 gNaBrO3加入到40 mL蒸馏水中在室温下搅拌1.5 h,将两种溶液混合,加入3 mL氨水调节溶液pH,并在此条件下连续反应3 h,直至沉淀生成,最后对所得沉淀进行分离、洗涤烘干,即可得到Bi5O7Br催化剂,记为Bi5O7Br-C。
所得Bi5O7Br-C光催化剂用于光催化降解卡马西平和盐酸四环素溶液。其反应条件为:常温常压,催化剂用量为0.05 g,水中微量药物污染物卡马西平或者盐酸四环素的处理量为100 mL、10 mg·L-1,所用光源为氙灯,功率为500 W,照度为120 klx,距离反应界面20cm, 所发光为波长大于420 nm的可见光,首先在避光条件下吸附0.5 h,以期达到吸附平衡;然后打开光源,对卡马西平或者盐酸四环素溶液进行光催化降解实验,每隔30 min取样一次,利用紫外-可见分光光度法对溶液中剩余待降解物的浓度进行分析并计算其降解率,结果如表1和表2所示。
表1 不同Bi5O7Br催化剂在可见光下对于卡马西平降解活性
表2 不同Bi5O7Br催化剂在可见光下对于盐酸四环素降解活性
Claims (3)
1.一种光催化剂Bi5O7Br的合成方法,其特征在于:包括如下步骤:
第一步,称取0.485~7.275 g的五水硝酸铋,将其放置于20~60 mL的蒸馏水中,在室温下搅拌1~3 h,直至完全溶解,记为溶液A;
第二步,称取0.151~2.265 g的溴酸钠,将其放置于15~50 mL蒸馏水中,在室温下搅拌1~3 h,直至溶液变为澄清,记为溶液B;
第三步,将溶液B加入溶液A中,搅拌使其混合均匀,加入1~3 mL氨水调节pH为7~10,并在室温下继续搅拌反应1~6 h,即可得到沉淀;
第四步,将沉淀抽滤分离,用蒸馏水和无水乙醇分别洗涤2-3次,在50~70 ℃下烘干,即得到具有可见光响应、带隙为2.52-2.92 eV可用于降解水中微量难降解药物的光催化剂Bi5O7Br。
2.一种如权利要求1所述的光催化剂Bi5O7Br应用于水中微量难降解的卡马西平或盐酸四环素的降解。
3.根据权利要求2所述的一种光催化剂Bi5O7Br应用于水中微量难降解的卡马西平或盐酸四环素的降解,其特征在于:反应条件为:常温常压,光催化剂用量为0.05g,卡马西平或盐酸四环素的处理量为50~100 mL、10 mg·L-1,所用光源为氙灯,功率为500 W,照度为120klx,距离反应界面20 cm, 所发光为波长大于420 nm的可见光。
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