CN108187700B - 碘化银/板状富铋型碘氧铋复合光催化材料的制备方法 - Google Patents
碘化银/板状富铋型碘氧铋复合光催化材料的制备方法 Download PDFInfo
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Abstract
本发明公开了一种碘化银/板状富铋型碘氧铋复合光催化材料的制备方法。所述方法先以Bi(NO3)3·5H2O和KI为原料，通过化学沉淀法制备BiOI，再将BiOI粉末均匀分散在水中，NaOH作为沉淀转化剂，AgNO3作为银源，搅拌条件下，在BiOI悬浊液中依次滴加氢氧化钠溶液和硝酸银溶液，通过原位沉积/沉淀转化法生成AgI/Bi5O7I复合物。本发明方法制备的AgI/Bi5O7I复合物，AgI与Bi5O7I紧密结合，形成异质结，在两者协同作用下产生优异的光催化活性。本发明在常温下进行，条件温和，反应时间较短，操作简便，节能环保，可用于大规模工业生产。
Description
技术领域
本发明涉及一种碘化银/板状富铋型碘氧铋复合光催化材料的制备方法，属于光催化材料制备领域。
背景技术
新型可见光响应的卤氧铋BixOyXz基半导体光催化剂具备独特晶体结构和优异光催化活性，能够有效降解有机污染物和还原二氧化碳。BiOI有着很窄的禁带宽度(1.8eV)，但因其导带位置很正，电子空穴容易重组，导致还原性不足，热稳定性很差。富铋型卤氧铋BixOyXz家族里包括Bi4O5I2、Bi7O9I3、Bi5O7I等。Bi5O7I和BiOI元素相同，有着由[Bi2O2]2+和双I离子层组成的独特的层状晶体结构，由此形成了垂直于片层间的静电场，能促进电子空穴对分离。和BiOI相比较，Bi5O7I有更优异的稳定性且合适的能带位置，固溶体中碘离子的P轨道杂化，使得它有更正的价带位置，且价带顶变得更加离域，能够提供更多活性空穴来氧化有机污染物，如苯酚、MO等，且相比其他卤氧铋其稳定性更高。但是Bi5O7I有较宽的禁带宽度，较低的载流子迁移率，限制了它的光催化活性，需要对其进行修饰改性来提高光催化活性。通过和其它合适的半导体光催化剂复合能够有效提高其光催化活性。如Cui等人构建的Z型光催化剂AgI/Bi5O7I对罗丹明B的光催化活性是Bi5O7I的3.83倍(Cui M,et al.In-situpreparation of Z-scheme AgI/Bi5O7I hybrid and its excellent photocatalyticactivity[J].Applied Surface Science,2016,387:912-920.)。Liu等人通过原位共热解结晶方法得到的g-C3N4/Bi5O7I的光催化活性较Bi5O7I有很大提高(Liu C,et al.In SituCo-Crystallization for Fabrication of g-C3N4/Bi5O7I Heterojunction forEnhanced Visible-Light Photocatalysis[J].Journal of Physical Chemistry C,2015,119(30):17156-17165.)。
AgI是直接带隙半导体，且相比AgCl和AgBr有更小的禁带宽度(约2.77eV)，对可见光吸收范围较大。但是团聚后的微米尺寸和缺乏与基体的紧密连接导致光生载流子容易复合，且性质不稳定，容易转化为金属银。AgI与其他半导体材料复合能够有效克服这一缺点。目前制备银系富铋型碘氧铋复合物时常采用水热法和高温煅烧法，其耗时又耗能。例如Chen等先用水热法制备出BiOI，再用高温煅烧法生成Bi5O7I，最后负载Ag2O制备Ag2O/Bi5O7I(Chen Y,et al.Three-dimensional Ag2O/Bi5O7I p-n heterojunction photocatalystharnessing UV-vis-NIR broad spectrum for photodegradation of organicpollutants.[J].Journal of Hazardous Materials,2017,344:42.)。通常AgI/Bi5O7I都是通过两步法先制备Bi5O7I再制备出AgI/Bi5O7I。如Cui等在Bi5O7I中加入AgNO3溶液，通过水热法制备AgI/Bi5O7I(Cui M,et al.In-situ preparation of Z-scheme AgI/Bi5O7Ihybrid and its excellent photocatalytic activity[J].Applied Surface Science,2016,387:912-920.)。
发明内容
本发明的目的在于提供一种低成本的碘化银/板状富铋型碘氧铋复合光催化材料的制备方法。
本发明的技术方案是：
碘化银/板状富铋型碘氧铋复合光催化材料的制备方法，先通过化学沉淀法生成前驱体BiOI，再采用原位沉积/沉淀转化法得到AgI/Bi5O7I复合物，具体包括如下步骤：
步骤1，将五水合硝酸铋均匀分散在乙二醇中形成硝酸铋悬浊液，搅拌条件下，滴加碘化钾溶液，氨水调节pH至中性，持续搅拌，反应结束后，离心，水洗，醇洗，烘干得到片层物质自组装而成的球状BiOI；
步骤2，将BiOI粉末均匀分散在水中，NaOH作为沉淀转化剂，AgNO3作为银源，搅拌条件下，在BiOI悬浊液中依次滴加氢氧化钠溶液和硝酸银溶液，搅拌，离心，水洗，醇洗，烘干得到碘化银/板状富铋型碘氧铋复合光催化材料。
优选地，步骤1中，所述的五水合硝酸铋和碘化钾的摩尔比为1:1。
优选地，步骤1中，所述的氨水浓度为1.5M。
优选地，步骤1中，所述的碘化钾溶液的滴加速度为1mL/min。
优选地，步骤2中，所述的铋和银的摩尔比为17.8～25.0：100。
优选地，步骤2中，所述的氢氧化钠与铋的摩尔比为5:1。
优选地，步骤2中，所述的氢氧化钠溶液和硝酸银溶液的滴加速度为1mL/min。
与现有技术相比，本发明的优点是：
(1)制备过程在常温下进行，通过原位沉积/沉淀转化法由前驱体BiOI一步得到AgI/Bi5O7I复合物，条件温和，耗时耗能较少，节能环保；
(2)制得的AgI/Bi5O7I复合物，在可见光下，AgI与Bi5O7I具有良好光响应的物质紧密结合，形成异质结，在两者协同作用下，使得AgI/Bi5O7I复合物产生优异的光催化活性，在60min内可以将10mg/L MO降解86.2％，降解速率是纯Bi5O7I的27.7倍，可应用于水中有机污染物及重金属等有害物质的处理。
附图说明
图1为实施例1制备的BA-4复合材料的扫描电镜图。
图2为实施例1中BA-4，实施例2中BA-5复合材料和纯Bi5O7I的紫外可见漫反射图。
图3为对比例1中BA-1，对比例2中BA-2，对比例3中BA-3，实施例1中BA-4，实施例2中BA-5复合材料和纯AgI，Bi5O7I对甲基橙(10mg/L)的降解速率图。
图4为BA-1，BA-2，BA-3，BA-4，BA-5复合材料和纯AgI，Bi5O7I降解甲基橙(10mg/L)的动力性曲线图。
具体实施方式
下面结合实施例和附图对本发明作进一步详述。
实施例1：碘化银/板状富铋型碘氧铋复合光催化材料的制备
①将0.97g Bi(NO3)3·5H2O均匀分散在30mL乙二醇，称量0.332gKI溶于10mL去离子水，逐滴加入硝酸铋悬浊液中，随后用1.5M的氨水来调节pH为7。在室温下搅拌2h，通过离心，三次去离子水洗涤，三次乙醇洗涤，最后70℃干燥8h得到BiOI。
②称取0.5g上述制备好的BiOI，在磁力搅拌的作用下在50mL去离子水中均匀分散，将1M NaOH逐滴加入，最后按照Bi/Ag的摩尔百分比17.8％加入0.1M AgNO3，常温搅拌1h后得到AgI/Bi5O7I复合物，标记为BA-4，样品通过离心，三次去离子水洗涤，三次乙醇洗涤，最后70℃干燥8h得到。
图1为实施例1制备的BA-4复合材料的扫描电镜图。从图中可以看出，纳米级别的AgI负载在微米级板状物Bi5O7I上。
实施例2：碘化银/板状富铋型碘氧铋复合光催化材料的制备
①将0.97g Bi(NO3)3·5H2O均匀分散在30mL乙二醇，称量0.332gKI溶于10mL去离子水，逐滴加入硝酸铋悬浊液中，随后用1.5M的氨水来调节pH为7。在室温下搅拌2h，通过离心，三次去离子水洗涤，三次乙醇洗涤，最后70℃干燥8h得到BiOI。
②称取0.5g上述制备好的BiOI，在磁力搅拌的作用下在50mL去离子水中均匀分散，将1M NaOH逐滴加入，最后按照Bi/Ag的摩尔百分比25.0％加入0.1M AgNO3，常温搅拌1h后得到AgI/Bi5O7I复合物，标记为BA-5，样品通过离心，三次去离子水洗涤，三次乙醇洗涤，最后70℃干燥8h得到。
对比例1：碘化银/板状富铋型碘氧铋复合光催化材料的制备
①将0.97g Bi(NO3)3·5H2O均匀分散在30mL乙二醇，称量0.332gKI溶于10mL去离子水，逐滴加入硝酸铋悬浊液中，随后用1.5M的氨水来调节pH为7。在室温下搅拌2h，通过离心，三次去离子水洗涤，三次乙醇洗涤，最后70℃干燥8h得到BiOI。
②称取0.5g上述制备好的BiOI，在磁力搅拌的作用下在50mL去离子水中均匀分散，将1M NaOH逐滴加入，最后按照Bi/Ag的摩尔百分比3.6％加入0.1M AgNO3，常温搅拌1h后得到AgI/Bi5O7I复合物，标记为BA-1，样品通过离心，三次去离子水洗涤，三次乙醇洗涤，最后70℃干燥8h得到。
对比例2：碘化银/板状富铋型碘氧铋复合光催化材料的制备
①将0.97g Bi(NO3)3·5H2O均匀分散在30mL乙二醇，称量0.332gKI溶于10mL去离子水，逐滴加入硝酸铋悬浊液中，随后用1.5M的氨水来调节pH为7。在室温下搅拌2h，通过离心，三次去离子水洗涤，三次乙醇洗涤，最后70℃干燥8h得到BiOI。
②称取0.5g上述制备好的BiOI，在磁力搅拌的作用下在50mL去离子水中均匀分散，将1M NaOH逐滴加入，最后按照Bi/Ag的摩尔百分比7.2％加入0.1M AgNO3，常温搅拌1h后得到AgI/Bi5O7I复合物，标记为BA-2，样品通过离心，三次去离子水洗涤，三次乙醇洗涤，最后70℃干燥8h得到。
对比例3：碘化银/板状富铋型碘氧铋复合光催化材料的制备
①将0.97g Bi(NO3)3·5H2O均匀分散在30mL乙二醇，称量0.332gKI溶于10mL去离子水，逐滴加入硝酸铋悬浊液中，随后用1.5M的氨水来调节pH为7。在室温下搅拌2h，通过离心，三次去离子水洗涤，三次乙醇洗涤，最后70℃干燥8h得到BiOI。
②称取0.5g上述制备好的BiOI，在磁力搅拌的作用下在50mL去离子水中均匀分散，将1M NaOH逐滴加入，最后按照Bi/Ag的摩尔百分比10.8％加入0.1M AgNO3，常温搅拌1h后得到AgI/Bi5O7I复合物，标记为BA-3，样品通过离心，三次去离子水洗涤，三次乙醇洗涤，最后70℃干燥8h得到。
图2为实施例1中BA-4，实施例2中BA-5复合材料和纯Bi5O7I的紫外可见漫反射图。从图中可以看出，与Bi5O7I相比，BA-4，BA-5复合材料的吸收边缘明显红移，扩大了对可见光的吸收，有助于提高其光催化活性。
图3为对比例1中BA-1，对比例2中BA-2，对比例3中BA-3，实施例1中BA-4，实施例2中BA-5复合材料和纯AgI，Bi5O7I对甲基橙(10mg/L)的降解速率图。从图中可以看出，在60min内BA-4复合材料光催化活性最高，可降解86.2％的10mg/L MO。
图4为BA-1，BA-2，BA-3，BA-4，BA-5复合材料和纯AgI，Bi5O7I降解甲基橙(10mg/L)的动力性曲线图，在60min内对甲基橙(10mg/L)进行降解，BA-4复合材料光催化活性最高，降解速率是Bi5O7I的27.7倍，是纯AgI的66.4倍，是BA-1的9.8倍，是BA-2的4.2倍，是BA-3的3.4倍。
Claims (6)
1.碘化银/板状富铋型碘氧铋复合光催化材料的制备方法，其特征在于，具体包括如下步骤：
步骤1，将五水合硝酸铋均匀分散在乙二醇中形成硝酸铋悬浊液，搅拌条件下，滴加碘化钾溶液，氨水调节pH至中性，持续搅拌，反应结束后，离心，水洗，醇洗，烘干得到片层物质自组装而成的球状BiOI；
步骤2，将BiOI粉末均匀分散在水中，NaOH作为沉淀转化剂，AgNO3作为银源，搅拌条件下，在BiOI悬浊液中依次滴加氢氧化钠溶液和硝酸银溶液，搅拌，离心，水洗，醇洗，烘干得到碘化银/板状富铋型碘氧铋复合光催化材料，所述的铋和银的摩尔比为17.8～25.0：100。
2.根据权利要求1所述的制备方法，其特征在于，步骤1中，所述的五水合硝酸铋和碘化钾的摩尔比为1:1。
3.根据权利要求1所述的制备方法，其特征在于，步骤1中，所述的氨水浓度为1.5M。
4.根据权利要求1所述的制备方法，其特征在于，步骤1中，所述的碘化钾溶液的滴加速度为1mL/min。
5.根据权利要求1所述的制备方法，其特征在于，步骤2中，所述的氢氧化钠与铋的摩尔比为5:1。
6.根据权利要求1所述的制备方法，其特征在于，步骤2中，所述的氢氧化钠溶液和硝酸银溶液的滴加速度为1mL/min。
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