CN109012705A - 制备Bi5O7I纳米棒的方法 - Google Patents
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- 229910052797 bismuth Inorganic materials 0.000 description 2
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Abstract
本发明公开了一种制备Bi5O7I纳米棒的方法。采用尿素溶液为溶剂溶解Bi(NO3)3·5H2O和KI，滴加NaOH溶液调节pH值，在室温下通过均相反应制备了高度晶化的棒状Bi5O7I。本发明制备的Bi5O7I纳米棒表现出了优异的光催化降解染料分解的活性，表明其在去除工业废水中染料等污染物方面具有较好的应用前景。
Description
技术领域
本发明涉及一种室温下制备Bi5O7I纳米棒的方法，属于无机纳米材料制备领域。
背景技术
光催化技术能将多种有机污染物彻底矿化去除，特别是对一些生物难以有效降解的有毒有害物质的去除提供了一种极具前途的环境污染深度净化方法。其中铋系光催化剂以其合适禁带宽度、稳定、降解效果好、合成条件可控等优点被广泛关注，在光催化降解领域有良好的应用前景。
卤氧铋系列光催化剂，由于具有[Bi2O2]与双卤离子层交错排列的层状结构，故存在内建电场，能有效分离光生电子与空穴，从而提高光催化性能。其中BiOI的禁带宽度最小（1.7-1.9 eV)，故对可见光的吸收能力最强，但由于光生电子与空穴易复合而导致光催化效率降低。通过改变Bi/O比，如Bi4O5I2、Bi7O9I3、Bi5O7I等富铋或富氧型碘氧铋系列化合物，可调节其禁带宽度，特别是提高其价带电位，从而增加其价带空穴的氧化能力，达到改善其光催化性能的目的。已有关于Bi4O5I2、Bi7O9I3、Bi5O7I等富铋型碘氧铋光催化剂的制备及性能研究报道，但制备大多采用水热法或溶剂热法。Chao Liu等在室温下在乙二醇-水体系中通过调节pH制备得到Bi4O5I2和Bi5O7I超薄纳米片，但结晶度较低，使其光催化性能受到不良影响。
发明内容
本发明的目的在于提供一种Bi5O7I纳米棒的制备方法。
实现本发明目的的技术解决方案为：一种室温下制备Bi5O7I纳米棒的方法，包括以下步骤：
步骤一：将Bi(NO3)3·5H2O溶于尿素水溶液中得到澄清溶液，加入KI并搅拌均匀；
步骤二：调节步骤一所述溶液的pH值至12.5~13.0，并于室温下反应12 h；
步骤三：反应结束后离心洗涤即得Bi5O7I纳米棒。
进一步地，步骤一所得溶液中Bi(NO3)3·5H2O摩尔浓度为0.1 mol/L，尿素的摩尔浓度为5.9 mol/L，KI的摩尔浓度为0.1 mol/L。
进一步地，步骤一中，Bi(NO3)3·5H2O与KI的摩尔比为1:1。
进一步地，步骤二中，采用2mol/L的NaOH溶液调节溶液的pH值。
与现有技术相比，本发明具有以下显著优点：
1、本发明所述方法简单，无需加入模板剂，室温条件下反应得到了高度晶化的Bi5O7I纳米棒光催化剂。
2、本发明制备的Bi5O7I纳米棒催化剂在可见光激发下对罗丹明B降解表现出优异的催化性能，有望在工业废水治理领域具有良好的应用。
附图说明
图1为本发明制备Bi5O7I纳米棒光催化剂的流程示意图。
图2为实施例1及对比例1 - 4所制得的Bi5O7I纳米棒光催化剂的TEM图（其中，(a)和(b)实施例1；(c)对比例1； (d)对比例2；(e) 对比例3；(f) 对比例4）。
图3为不同pH值条件下制备的Bi5O7I纳米棒光催化剂对罗丹明B的降解率图。
图4为对比例不同尿素量对所制备Bi5O7I纳米棒催化罗丹明B降解的影响图。
图5为对比例所制备的BiOI纳米片催化罗丹明B的降解率图。
具体实施方式
下面结合附图和具体实施方式对本发明作进一步详细说明。
结合图1，本发明利用尿素溶液为溶剂，制备光催化性能优异的Bi5O7I纳米棒状光催化剂的方法，其特征包括以下步骤：
步骤一：将Bi(NO3)3·5H2O溶于尿素水溶液中得到澄清溶液，加入KI并搅拌均匀，尿素的摩尔浓度为5.9 mol/L，Bi(NO3)3·5H2O摩尔浓度为0.1 mol/L， KI的摩尔浓度为0.1mol/L，Bi(NO3)3·5H2O与KI的摩尔比为1:1；
步骤二：滴加NaOH溶液至步骤二溶液中，调节pH值至12.5~13.0，室温下反应12 h；
步骤三：反应结束后离心洗涤即得Bi5O7I纳米棒。
下面结合实施例、对比例和附图对本发明做进一步详细的说明：
实施例1：
步骤一：将2 mmol Bi(NO3)3·5H2O溶于20 ml含有117 mmol尿素的水溶液中得到澄清溶液，加入2 mmol KI并搅拌均匀；
步骤二：滴加4 mL 2 mol/L NaOH溶液至步骤二溶液中，调节pH值至12.5~13.0，室温下反应12 h；
步骤三：反应结束后离心洗涤即得Bi5O7I纳米棒。
所得产物的透射电镜图如图2(a)、(b)，产物为纳米棒。所得产物的光催化性能如图3所示，在可见光激发下，60 min内其降解率达到90.2 %。
改变步骤二中pH值为11.0~11.5，13.5~14.0，大于14.0（分别滴加3mL、5mL、6mL 2mol/L NaOH溶液）后，其产物在可见光激发下，60 min内降解率分别达到86.3 %、73.4 %、68.9 %，均低于实施例1所制备的Bi5O7I纳米棒。
对比例1：
步骤一：将2 mmol Bi(NO3)3·5H2O溶于20 ml含有250 mmol尿素的水溶液中得到澄清溶液，加入2 mmol KI并搅拌均匀；
步骤二：滴加4 mL 2 mol/L NaOH溶液至步骤一溶液中，调节pH值至12.5~13.0，室温下反应12 h；
步骤三：反应结束后离心洗涤即得Bi5O7I纳米棒。
所得产物的透射电镜图片如图2(c)，产物为纳米棒。所得产物的光催化性能如图4所示，在可见光激发下，60 min内其降解率达到69.4 %。
对比例2：
步骤一：将2 mmol Bi(NO3)3·5H2O溶于20 ml含有83 mmol尿素的水溶液中得到浅乳白色溶液，加入2 mmol KI并搅拌均匀；
步骤二：滴加4 mL 2 mol/L NaOH溶液至步骤一溶液中，调节pH值至12.5~13.0，室温下反应12 h；
步骤三：反应结束后离心洗涤即得Bi5O7I纳米棒。
所得产物的透射电镜图片如图2(d)，产物为纳米棒。所得产物的光催化性能如图4所示，在可见光激发下，60 min内其降解率达到60.8 %。
对比例3：
步骤一：将2 mmol Bi(NO3)3·5H2O溶于20 ml去离子水中得到浅乳白色溶液，加入2mmol KI并搅拌均匀；
步骤二：滴加4 mL 2 mol/L NaOH溶液至步骤一溶液中，调节pH值至12.5~13.0，室温下反应12 h；
步骤三：反应结束后离心洗涤即得Bi5O7I纳米棒。
所得产物的透射电镜图片如图2(e)，产物为纳米棒。所得产物的光催化性能如图4所示，在可见光激发下，60 min内其降解率达到82.4 %。
对比例4：
步骤一：将2 mmol Bi(NO3)3·5H2O溶于20 ml含有117 mmol尿素的水溶液中得到澄清溶液，加入2 mmol KI并搅拌均匀，所得溶液pH值为2；
步骤二：室温下反应12 h；
步骤三：反应结束后离心洗涤即得BiOI纳米晶。
所得产物的透射电镜图片如图2(f)，产物为纳米片。所得产物的光催化性能如图5所示，在可见光激发下，60 min内其降解率达到60.6 %。
Claims (4)
1.制备Bi5O7I纳米棒的方法，其特征在于，包括如下步骤：
（1）将Bi(NO3)3·5H2O溶于尿素水溶液中得到澄清溶液，加入KI并搅拌均匀；
（2）调节步骤（1）所述溶液的pH值至12.5~13.0，并于室温下反应12 h；
（3）反应结束后离心洗涤即得Bi5O7I纳米棒。
2.如权利要求1所述的方法，其特征在于，步骤（1）中，所得溶液中Bi(NO3)3·5H2O摩尔浓度为0.1 mol/L，尿素的摩尔浓度为5.9 mol/L，KI的摩尔浓度为0.1 mol/L。
3.如权利要求1所述的方法，其特征在于，步骤（1）中，Bi(NO3)3·5H2O与KI的摩尔比为1:1。
4.如权利要求1所述的方法，其特征在于，步骤（2）中，采用2mol/L的NaOH溶液调节溶液的pH值。
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| CN105597793A (zh) * | 2015-11-17 | 2016-05-25 | 中国科学院海洋研究所 | 一种光催化剂及其制备方法和应用 |
| CN105800686A (zh) * | 2016-03-11 | 2016-07-27 | 石家庄经济学院 | 一种制备Bi5O7I的方法 |
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| CN105597793A (zh) * | 2015-11-17 | 2016-05-25 | 中国科学院海洋研究所 | 一种光催化剂及其制备方法和应用 |
| CN105800686A (zh) * | 2016-03-11 | 2016-07-27 | 石家庄经济学院 | 一种制备Bi5O7I的方法 |
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| JING CAO ET AL.: "Low temperature synthesis of novel rodlike Bi5O7I with visible light photocatalytic performance", 《MATERIALS LETTERS》 * |
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