CN114669308A - 一种借助电化学法原位反应制备BiOCl/Bi24O31Cl10复合粉体的方法 - Google Patents
一种借助电化学法原位反应制备BiOCl/Bi24O31Cl10复合粉体的方法 Download PDFInfo
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- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 239000000843 powder Substances 0.000 title claims abstract description 43
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 19
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- 239000003365 glass fiber Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 229910052797 bismuth Inorganic materials 0.000 claims description 4
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 4
- 238000003487 electrochemical reaction Methods 0.000 claims 7
- 230000001699 photocatalysis Effects 0.000 abstract description 6
- 230000003197 catalytic effect Effects 0.000 abstract description 5
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- 239000003054 catalyst Substances 0.000 abstract 1
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- 238000005516 engineering process Methods 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
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- 238000004458 analytical method Methods 0.000 description 1
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Abstract
一种借助电化学法原位反应制备BiOCl/Bi24O31Cl10复合粉体的方法。本发明采用电化学辅助的方法对BiOCl催化剂进行处理制备BiOCl/Bi24O31Cl10复合粉体,从而大幅度提高降解有机污染物的光催化性。本方法如下:一、将BiOCl放入含有水的电解池中,电解池以隔膜分开;二、在搅拌的状态下,通过酸(或碱)调节电解液的pH值;三、将电极插入电解池中,在恒压(或恒流)模式下维持一定时间,通电过程中控制电解池中液体的温度;四、将步骤三得到的粉体过滤后清洗至中性,烘干既得具有高催化活性的BiOCl/Bi24O31Cl10复合粉体。本发明具有制备方法简单,价格低廉且样品中两相的含量可调控等优点。
Description
技术领域
本发明涉及一种借助电化学法原位反应制备BiOCl/Bi24O31Cl10复合粉体的方法。
背景技术
随着科技和工业的快速发展,许多新兴产业的出现导致了大量的工业废弃物被排入到地下水中,严重危害了人类健康和赖以生存的水资源生态环境。以太阳能作为主要能量来源的半导体光催化技术由于其具有节能、高效以及不会产生二次污染等特点,被认为是处理目前水污染问题最为理想的技术手段之一。然而,以二氧化钛(TiO2)为代表的传统光催化剂由于其光谱响应范围有限且光生载流子分离效率不高,限制了光催化技术在环境修复领域中的应用。卤氧化铋因其独特的开放式层状结构和适当的能带结构,被认为是最具发展潜力的新型半导体光催化剂之一。然而较大的禁带宽度使BiOCl在可见光下的催化降解效率并不理想,其光催化性能还有待提高。以往的研究结果表明:通过在BiOCl材料中引入助催化剂构建异质结是改善其光催化活性的有效方法。
发明内容
本发明为了寻找一种BiOCl/Bi24O31Cl10复合粉体的原位反应制备方法,以满足提升光催化性能的需要,提供了一种电化学辅助条件下的制备方法。
1、一种借助电化学法原位反应制备BiOCl/Bi24O31Cl10复合粉体的方法,其特征在于采用电化学辅助进行原位反应的方法按照以下步骤进行:
一、将BiOCl放入含有水的电解池中的正极一侧,电解池以隔膜分开;BiOCl与水的质量比为1:1~10000,其中电解池隔膜的孔径为3~1000000nm,隔膜的材质可为PE、PVDF、玻璃纤维等;
二、在搅拌的状态下,通过酸(或碱)调节电解液的pH值,pH值范围在1~14;
三、将电极插入电解池中,在恒压模式下电压的范围为1~10000V,恒流模式下电流的范围为0.01~10000mA,通电时间为1~100000000s,通电过程中控制电解池中液体的温度在0~100℃;
四、通电结束后将步骤三得到的粉体过滤后使用蒸馏水洗涤1-8次至中性,在30~150℃下烘干既得BiOCl/Bi24O31Cl10复合粉体。
本发明调控的卤氧化铋复合粉体具有制备方法简单,成本低,高催化活性等优点。
附图说明
图1是实验一制备的BiOCl/Bi24O31Cl10复合粉体扫描电镜照片;
图2实验一制备的BiOCl/Bi24O31Cl10复合粉体物相分析图;
图3实验一制备实验一制备BiOCl/Bi24O31Cl10光催化降解罗丹明B和CIP的曲线;
具体实施方式
本发明技术方案不局限于以下所列举具体实施方式,还包括各具体实施方式间的任意组合。
具体实施方式一:本实施方式一种借助电化学法原位反应制备BiOCl/Bi24O31Cl10复合粉体的方法按照以下步骤进行:
一、将BiOCl放入含有水的电解池中的正极一侧,电解池以隔膜分开;BiOCl与水的质量比为1:1~10000,其中电解池隔膜的孔径为3~1000000nm,隔膜的材质可为PE、PVDF、玻璃纤维等;
二、在搅拌的状态下,通过酸(或碱)调节电解液的pH值,pH值范围在1~14;
三、将电极插入电解池中,在恒压模式下电压的范围为1~10000V,恒流模式下电流的范围为0.01~10000mA,通电时间为1~100000000s,通电过程中控制电解池中液体的温度在0~100℃;
四、通电结束后将步骤三得到的粉体过滤后使用蒸馏水洗涤1-8次至中性,在30~150℃下烘干既得BiOCl/Bi24O31Cl10复合粉体。
具体实施方式二:本实施方式与具体实施方式一不同的是步骤一中BiOCl与水的质量比为1:10~8000,其中电解池隔膜的孔径为3~1000000nm,隔膜的材质可为PE、PVDF、玻璃纤维等。
具体实施方式三:本实施方式与具体实施方式一至二不同的是步骤二中通过酸(或碱)调节电解液的pH值,pH值范围在5~8。
具体实施方式四:本实施方式与具体实施方式一至三不同的是步骤三中在恒压模式下电压的范围为0.1~8000V。
具体实施方式五:本实施方式与具体实施方式一至四不同的是步骤三中,恒流模式下电流的范围为0.001~9000mA。
具体实施方式六:本实施方式与具体实施方式一至五不同的是步骤三中,通电时间为10~80000000s,通电过程中控制电解池中液体的温度在0~100℃。
具体实施方式七:本实施方式与具体实施方式一至六不同的是步骤三中通电过程中控制电解池中液体的温度在0~90℃。
采用下述实验验证本发明效果:
实验一:
一种借助电化学法原位反应制备BiOCl/Bi24O31Cl10复合粉体的方法,按照以下步骤进行:
一、将BiOCl放入含有水的电解池中的正极一侧,电解池以隔膜分开;BiOCl与水的质量比为1:100,其中电解池隔膜的孔径为200nm,隔膜的材质可为PE;
二、在搅拌的状态下,通过酸(或碱)调节电解液的pH值,pH值范围在7;
三、将电极插入电解池中,在恒压模式下电压的范围为300V,通电时间为20000s,通电过程中控制电解池中液体的温度在25℃;
四、通电结束后将步骤三得到的粉体过滤后使用蒸馏水洗涤3次至中性,在50℃下烘干既得具有高催化活性的BiOCl/Bi24O31Cl10复合粉体。
实验二:
一种借助电化学法原位反应制备BiOCl/Bi24O31Cl10复合粉体的方法,按照以下步骤进行:
一、将BiOCl放入含有水的电解池中的正极一侧,电解池以隔膜分开;BiOCl与水的质量比为1:500,其中电解池隔膜的孔径为500nm,隔膜的材质可为PVDF;
二、在搅拌的状态下,通过酸(或碱)调节电解液的pH值,pH值范围在6;
三、将电极插入电解池中,在恒流模式下电压的范围为0.02A,通电时间为28800s,通电过程中控制电解池中液体的温度在20℃;
四、通电结束后将步骤三得到的粉体过滤后使用蒸馏水洗涤5次至中性,在50℃下烘干既得具有高催化活性的BiOCl/Bi24O31Cl10复合粉体。
Claims (8)
1.一种借助电化学法原位反应制备BiOCl/Bi24O31Cl10复合粉体的方法,其特征在于采用电化学辅助进行原位反应的方法按照以下步骤进行:
一、将BiOCl放入含有水的电解池中的正极一侧,电解池以隔膜分开;BiOCl与水的质量比为1:1~10000,其中电解池隔膜的孔径为3~1000000nm,隔膜的材质可为PE、PVDF、玻璃纤维等;
二、在搅拌的状态下,通过酸(或碱)调节电解液的pH值,pH值范围在1~14;
三、将电极插入电解池中,在恒压模式下电压的范围为1~10000V,恒流模式下电流的范围为0.01~10000mA,通电时间为1~100000000s,通电过程中控制电解池中液体的温度在0~100℃;
四、通电结束后将步骤三得到的粉体过滤后使用蒸馏水洗涤1-8次至中性,在30~150℃下烘干既得BiOCl/Bi24O31Cl10复合粉体。
2.根据权利要求1所述一种借助电化学法原位反应制备BiOCl/Bi24O31Cl10复合粉体的方法,其特征在于步骤一中将卤氧化铋放入含有水的电解池中的正极一侧,电解池以隔膜分开。
3.根据权利要求1所述一种借助电化学法原位反应制备BiOCl/Bi24O31Cl10复合粉体的方法,其特征在于步骤一中卤氧化铋与水的质量比为1:1~10000。
4.根据权利要求1所述一种借助电化学法原位反应制备BiOCl/Bi24O31Cl10复合粉体的方法,其特征在于步骤一中,电解池两极之间以隔膜分开,隔膜的孔径为3~1000000nm,隔膜的材质可为PE、PVDF、玻璃纤维等。
5.根据权利要求1所述一种借助电化学法原位反应制备BiOCl/Bi24O31Cl10复合粉体的方法,其特征在于步骤二中,通过酸(或碱)调节电解液的pH值,pH值范围在1~14。
6.根据权利要求1所述一种借助电化学法原位反应制备BiOCl/Bi24O31Cl10复合粉体的方法,其特征在于步骤三中,在恒压模式下电压的范围为1~10000V。
7.根据权利要求1所述一种借助电化学法原位反应制备BiOCl/Bi24O31Cl10复合粉体的方法,其特征在于步骤三中,恒流模式下电流的范围为0.01~10000mA。
8.根据权利要求1所述一种借助电化学法原位反应制备BiOCl/Bi24O31Cl10复合粉体的方法,其特征在于步骤三中,通电时间为1~100000000s,通电过程中控制电解池中液体的温度在0~100℃。
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