CN106513021A - 层状氢氧化物/BiOCl光催化材料及其制备方法 - Google Patents
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Abstract
本发明涉及层状氢氧化物/BiOCl光催化材料及其制备方法。用水热法制备BiOCl，共沉淀法制备LDH；将LDH用甲酰胺剥离得带正电LDH，再将剥离的LDH与带负电BiOCl溶液混合，密封搅拌一天，两种材料通过自组装得到BiOCl/LDH层层复合材料。通过BiOCl、LDH形貌、剥离LDH与层状BiOCl表面电荷性质控制复合材料形貌，制备LDH/BiOCl层层自组装复合的异质结复合材料，从而提供一种制备可见光光催化性能优良BiOCl/LDH层层复合材料的方法，可高效催化去除TOC。本发明涉及的这种层层BiOCl/LDH复合可见光光催化材料具有良好的可见光光催化降解有机物性能，能耗低。
Description
技术领域
本发明涉及一种层状氢氧化物/BiOCl光催化材料及其制备方法，该材料用于可见光光催化降解罗丹明B等有机污染物。
背景技术
生活工业废水中存在大量有机物，其对经济发展和人们健康造成极大的危害。目前关于污水治理方法的研究引起了人们的广泛重视，开发高效、低能耗、适用范围广和有深度氧化能力的化学污染物清除技术一直是此领域的研究热点。
光催化技术是指在含有污染物的水溶液中加入一定量的半导体光催化剂,在光照射的条件下,半导体材料被光激发出具有强氧化能力的电子一空穴对,从而发生一系列的氧化还原反应,使有毒的污染物得以降解的一种水处理方法。此技术在环境和能源开发领域具有广泛前景。它最大的优势在于降解反应一般在常温常压下进行,在催化剂存在的条件下能将水体中的有机污染物彻底分解,使其矿化为一些无机小分子物质、CO2和H2O。此外，光催化技术是利用光能,与其它传统污染治理技术相比,可节省其它能源的使用,缓解日益严重的能源危机。
BiOCl作为一种新型光催化剂，具有独特的电子结构、适合的禁带宽度以及优异的催化性能。而且，其具有开放层状结构有利于电子－空穴的有效分离及电荷转移，具有很高的催化活性。但由于BiOCl的禁带带宽较宽(Eg=3.3eV)无可见光响应，只能被太阳光中的紫外光激发，且重复性较差，对其应用领域和实际应用有限制。层状双氢氧化物(LDHs)因其特殊的层状结构及物理化学性质,可用来制备兼具吸附和光催化能力的复合催化剂(其中ZnCr、NiCr、ZnAl-LDHs在降解污染物方面有很好的催化活性)。但由于光生电子空穴复合速率较快，限制了实用效果。
复合半导体可以实现不同半导体性质上的互补，拓展对光的吸收范围，促进光生电子与空穴的分离，从而有效改善单一半导体的光催化性能。2D纳米片具有大比表面积、大自由度、多晶体取向的优点。
通过文献检索，未发现花状BiOCl/ LDH层层自组装复合的可见光催化材料的制备方法的专利申请和文献报道。
发明内容
本发明的目的之一在于提供一种本发明的目的层状氢氧化物/BiOCl光催化材料。
本发明的目的之二在于提供该光催化材料的制备方法。
本发明的技术构思是：通过BiOCl、LDH形貌、剥离LDH与层状BiOCl表面电荷性质控制复合材料形貌，制备LDH/BiOCl层层自组装复合的异质结复合材料，从而提供一种制备可见光光催化性能优良BiOCl/LDH层层复合材料的方法。
根据上述构思，本发明采用下述技术的方案：
一种层状双氢氧化物/BiOCl光催化材料，其特征在于所述的光催化材料是由带正电的层状双氢氧化物LDH纳米片与带负电BiOCl纳米片通过静电作用自组装形成层层交替堆叠的层状结构，每层的厚度在0.5~5nm，总层数为：6~20层 。
上述的层状双氢氧化物为：二价、三价过渡金属组成层板，水分子、阴离子在层间共同组成的具有层状结构的氧化物。
上述的层状双氢氧化物为：ZnCrLDH、NiCrLDH或ZnFeLDH。
一种制备上述的层状双氢氧化物/BiOCl光催化材料的方法，其特征在于该方法的具体步骤为：
a. 将BiOCl溶于二次水中配制成浓度为1~2g/L，分散均匀得到分散液A；
b. 将层状双氢氧化物LDH溶于甲酰胺中配制成浓度为1~2g/L的溶液，在惰性气氛保护下，搅拌12~24h，离心去除的未剥离LDH，制得带正电LDH 纳米片溶液，即溶液B；
c. 将步骤a所得溶液A缓慢加入步骤b所得溶液B中，密封下搅拌12~24h，经离心分离，水洗，取固相烘干得层状双氢氧化物/BiOCl光催化材料；所述的溶液A与溶液B的体积比为：1:（1~2）。
本发明BiOCl/LDH层层复合可见光催化剂能够高效催化去除罗丹明B染料废水，所制备的复合催化剂以带正电LDH纳米片与带负电BiOCl纳米片自组装形成，两种纳米片复合形成多孔堆叠结构,增强光催化性能，拓展对光的吸收范围，实现不同半导体性质上的互补，有效改善单一半导体的光催化性能，形成光催化性能增强、稳定性、重复性良好的复合材料。通过BiOCl、LDH形貌特征、两种材料表面电荷特性，形成异质结，增强光催化活性。
本发明BiOCl/LDH复合可见光催化剂催化降解罗丹明B染料废水的机理如下：光激发下，半导体价带上的e-跃迁至导带，从而在价带上产生光生空穴，导带上产生光生电子。因两者的禁带宽度不同,价带、导带位置有偏差,光生电子从导带位置较负的半导体的导带流向导带位置较正的半导体的导带，而空穴则由价带位置较正的半导体移向价带位置较负的半导体的价带，实现光生电子、空穴有效分离;光生电子被O2捕获，光生空穴与OH-反应生成·OH，与反应物反应，使其矿化为一些无机小分子物质、CO2和H2O。
具体实施方式
实施例一 ：在本实施例中，以处理浓度为2000mg/L TOC为例，BiOCl/ZnCrLDH层层自组装复合可见光光催化材料的制备方法,步骤如下：
(1)用水热法制备BiOCl，共沉淀法制备ZnCrLDH；
(2)将步骤（1）制得BiOCl以1g/L溶于二次水中，超声6h；
(3)将步骤（1）制得LDH以1g/L溶于甲酰胺中，在氮气下搅拌24h，以3000 rpm离心10分钟去除部分未剥离LDH，制得带正电LDH 纳米片；
(4)将按步骤(2)溶液缓慢加入步骤(3)中，两种溶液混合，再在密封胶密封下搅拌24h；
(5)将按步骤(4)溶液用二次水离心洗涤，取固相在60℃烘箱干燥10h，得ZnCrLDH/BiOCl自组装产物。
在本实施例中，对于2000mg/L TOC进行可见光催化，所制备的催化剂能够达到90%的去除率。
实施例二：在本实施例中，以处理浓度为2000mg/L TOC为例，BiOCl/NiCrLDH层层自组装复合可见光光催化材料的制备方法,步骤如下：
(1)用水热法制备BiOCl，共沉淀法制备NiCrLDH；
(2)将步骤（1）制得BiOCl以1g/L溶于二次水中，超声6h；
(3)将步骤（1）制得NiCrLDH以1g/L溶于甲酰胺中，在氮气下搅拌24h，以3000 rpm离心10分钟去除部分未剥离LDH，制得带正电LDH 纳米片；
(4)将按步骤(2)溶液缓慢加入步骤(3)中，两种溶液混合，再在密封胶密封下搅拌24h；
(5)将按步骤(4)溶液用二次水离心洗涤，取固相在60℃烘箱干燥10h，得NiCrLDH/BiOCl自组装产物。
在本实施例中，对于2000mg/L TOC进行可见光催化，所制备的催化剂能够达到85%的去除率。
实施例三：在本实施例中，以处理浓度为2000mg/L TOC为例，BiOCl/ZnFeLDH层层自组装复合可见光光催化材料的制备方法,步骤如下：
(1)用水热法制备BiOCl，共沉淀法制备ZnFeLDH；
(2)将步骤（1）制得BiOCl以1g/L溶于二次水中，超声6h；
(3)将步骤（1）制得ZnFeLDH以1g/L溶于甲酰胺中，在氮气下搅拌24h，以3000 rpm离心10分钟去除部分未剥离LDH，制得带正电LDH 纳米片；
(4)将按步骤(2)溶液缓慢加入步骤(3)中，两种溶液混合，再在密封胶密封下搅拌24h；
(5)将按步骤(4)溶液用二次水离心洗涤，取固相在60℃烘箱干燥10h，得ZnFeLDH/BiOCl自组装产物。
在本实施例中，对于2000mg/L TOC进行可见光催化，所制备的催化剂能够达到82%的去除率。
上面对本发明实施例进行了说明，但本发明不限于上述实施例。只要符合本发明的发明目的，只要不背离本发明层层BiOCl/LDH材料的制备方法及处理废水中有机污染物的方法的技术原理和发明构思，应用于环境污染治理和光催化材料制备等领域，都属于本发明的保护范围。
Claims (4)
1.一种层状双氢氧化物/BiOCl光催化材料，其特征在于所述的光催化材料是由带正电的层状双氢氧化物LDH纳米片与带负电BiOCl纳米片通过静电作用自组装形成层层交替堆叠的层状结构，每层的厚度在0.5~5nm，总层数为：6~20层 。
2.根据权利要求1所述的层状双氢氧化物/BiOCl光催化材料，其特征在于所述的层状双氢氧化物为：二价、三价过渡金属组成层板，水分子、阴离子在层间共同组成的具有层状结构的氧化物。
3.根据权利要求2所述的层状双氢氧化物/BiOCl光催化材料，其特征在于所述的层状双氢氧化物为：ZnCrLDH、NiCrLDH或ZnFeLDH。
4.一种制备根据权利要求1、2或3所述的层状双氢氧化物/BiOCl光催化材料的方法，其特征在于该方法的具体步骤为：
a. 将BiOCl溶于二次水中配制成浓度为1~2g/L，分散均匀得到分散液A；
b. 将层状双氢氧化物LDH溶于甲酰胺中配制成浓度为1~2g/L的溶液，在惰性气氛保护下，搅拌12~24h，离心去除的未剥离LDH，制得带正电LDH 纳米片溶液，即溶液B；
c. 将步骤a所得溶液A缓慢加入步骤b所得溶液B中，密封下搅拌12~24h，经离心分离，水洗，取固相烘干得层状双氢氧化物/BiOCl光催化材料；所述的溶液A与溶液B的体积比为：1:（1~2）。
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| CN112337424A (zh) * | 2020-09-30 | 2021-02-09 | 成都理工大学 | 一种Bi5O7I/煅烧水滑石复合材料及其制备方法 |
| CN113976149A (zh) * | 2021-11-05 | 2022-01-28 | 湖南大学 | 钴铝水滑石/富铋氯氧化铋复合光催化剂及其制备方法和应用 |
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| CN112337424A (zh) * | 2020-09-30 | 2021-02-09 | 成都理工大学 | 一种Bi5O7I/煅烧水滑石复合材料及其制备方法 |
| CN112337424B (zh) * | 2020-09-30 | 2022-04-22 | 成都理工大学 | 一种Bi5O7I/煅烧水滑石复合材料及其制备方法 |
| CN113976149A (zh) * | 2021-11-05 | 2022-01-28 | 湖南大学 | 钴铝水滑石/富铋氯氧化铋复合光催化剂及其制备方法和应用 |
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