CN110560096A - 一种负载铋系异质结的氧化石墨烯光催化材料及其制备方法和应用 - Google Patents
一种负载铋系异质结的氧化石墨烯光催化材料及其制备方法和应用 Download PDFInfo
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Abstract
本发明公开了一种负载铋系异质结的氧化石墨烯光催化材料的制备方法,包括以下步骤:首先制备BiOI/BixNbOy光催化剂和氧化石墨烯,将合成的BiOI/BixNbOy异质结催化剂负载于氧化石墨烯纳米片上,以负载后的石墨烯纳米片为前驱体,对预冷冻处理后的化合物进行真空干燥处理,得到具有高强度的负载铋系异质结的氧化石墨烯光催化材料。本发明负载铋系异质结的氧化石墨烯光催化材料具有高强度、高比表面积和强吸附等特点,可以有效解决粉末状光催化剂在使用后难以分离和回收利用的难题,避免了纳米材料对环境造成的二次污染等问题;有利于提高光催化反应速率;提高了催化剂光生载流子的分离率,增加了光催化剂的的稳定性,拓宽了光谱响应范围。
Description
技术领域
本发明涉及一种光催化材料的制备方法,具体为一种负载铋系异质结的氧化石墨烯光催化材料的制备与应用。
背景技术
持久性有机污染物(persistent organic pollutants,简称POPs)是对具有长期残留性和大范围迁移性、生物蓄积性、半挥发性及对生物体有高毒性的一类天然的或人工合成的有机物及其衍生物的统称,POPs污染逐渐成为目前国际上备受关注的新的全球性环境问题。随着国内工农业经济的高速发展,有关水体中POPs经各种途径的排放量不断上升,污染状况呈现恶化趋势,造成的健康问题日趋严重,调查研究表明,地表水环境普遍受到持久性有机物的污染,水源水、地下水水质也面临严峻的考验。
光催化降解是POPs在环境中的重要转化途径,也是最常用的化学降解方法。现有的常规光催化剂、铌系、铋系复合氧化物或异质结,氧化石墨烯基复合催化剂等,但都具有一定的不足。因此,制备具有无毒稳定、催化活性高、绿色能源利用率高及循环利用性能好的新型光催化剂,对于实现水中POPs的高效降解具有重要意义。本发明旨在制备一种具有高效催化性能的负载铋系异质结的氧化石墨烯光催化材料。
发明内容
本发明的目的是为了克服现有光催化材料的光谱响应范围较窄、循环利用性差、产生水体二次污染、载流子分离效率低等不足,提供了一种高效的负载铋系异质结的氧化石墨烯光催化材料的制备方法。
本发明通过以下技术方案实现。
一种负载铋系异质结的氧化石墨烯光催化材料的制备方法,包括以下步骤:
首先制备BiOI/BixNbOy光催化剂和氧化石墨烯,将合成的BiOI/BixNbOy异质结催化剂负载于氧化石墨烯纳米片上,以负载后的石墨烯纳米片为前驱体,借助定向真空冷冻干燥技术,对预冷冻处理后的化合物进行真空干燥处理,即可得到具有高强度的负载铋系异质结的氧化石墨烯光催化材料。
优选地,采用Nb2O5和Bi(NO3)3·5H2O制备BiOI/BixNbOy光催化剂。
优选地,BiOI/BixNbOy光催化剂的制备过程中分别添加不同的表面活性剂或者分别控制不同的反应条件(如反应温度,时间,反应物配比等)合成具有不同晶型的BiOI/BixNbOy异质结光催化剂。
优选地,所述表面活性剂为柠檬酸钠、十二烷基苯磺酸钠或溴化十六烷基三甲胺。
优选地,在真空冷冻干燥的过程中,真空度为3.3~13pa。
一种上述方法制备的负载铋系异质结的氧化石墨烯光催化材料。
上述负载铋系异质结的氧化石墨烯光催化材料主要应用于对水体POPs的降解。
本发明制备方法中BiOI/BixNbOy的负载结合定向真空冷冻干燥技术,可大幅度提高石墨烯基催化剂的机械强度。
上述制备方法中氧化石墨烯基负载可以提高BiOI/BixNbOy催化剂的分散程度和分散均匀性。
与现有技术相比,本发明所提供的技术方案的优点在于:
(1)构筑的负载铋系异质结的氧化石墨烯光催化材料具有高强度、高比表面积和强吸附等特点,可以有效解决粉末状光催化剂在使用后难以分离和回收利用的难题,避免了纳米材料对环境造成的二次污染等问题。
(2)氧化石墨烯负载体比传统光催化剂载体(如活性炭)更易于传质,有利于提高光催化反应速率。
(3)利用高强度的氧化石墨烯作为BiOI/BixNbOy的载体,结合了两者优异的光电性质和结构特质,提高了催化剂光生载流子的分离率,增加了光催化剂的的稳定性,拓宽了光谱响应范围。
附图说明
图1为GO-BiOI/BixNbOy光催化剂的合成及其对POPs的降解机理图。
具体实施方式
实施例1
首先,采用溶剂热法制备BiOI/BixNbOy光催化剂(制备过程中添加表面活性剂柠檬酸钠),然后,采用改进的Hummers法制备氧化石墨烯。将合成的BiOI/BixNbOy异质结催化剂负载于氧化石墨烯纳米片上。再次,以负载后的石墨烯纳米片为前驱体,借助定向真空冷冻干燥技术,在真空度为3.3Pa下,进行真空干燥,即可得到高强度的负载铋系异质结的石墨烯光催化材料。
以氙灯为模拟太阳光源,构建负载BiOI/BixNbOy异质结的氧化石墨烯连续流反应器。分别以含POPs的模型污水和实际污水为处理对象,在污染物和光催化达到吸附平衡后,每隔一定时间取样测定POPs浓度和COD、TOC的含量,分析POPs的降解率和矿化度。
本发明公开了一种负载铋系异质结的氧化石墨烯光催化材料的制备与应用。通过在氧化石墨烯上负载BiOI/BixNbOy异质结,再进行真空冷冻干燥,即得到高强度的负载铋系异质结的氧化石墨烯光催化材料。
实施例2
首先,采用溶剂热法制备BiOI/BixNbOy光催化剂(制备过程中添加表面活性剂十二烷基苯磺酸钠),然后,采用改进的Hummers法制备氧化石墨烯。将合成的BiOI/BixNbOy异质结催化剂负载于氧化石墨烯纳米片上。再次,以负载后的石墨烯纳米片为前驱体,借助定向真空冷冻干燥技术,在真空度为5.0Pa下,进行真空干燥,即可得到高强度的负载铋系异质结的石墨烯光催化材料。
实施例3
首先,采用溶剂热法制备BiOI/BixNbOy光催化剂(制备过程中添加表面活性剂溴化十六烷基三甲铵),然后,采用改进的Hummers法制备氧化石墨烯。将合成的BiOI/BixNbOy异质结催化剂负载于氧化石墨烯纳米片上。再次,以负载后的石墨烯纳米片为前驱体,借助定向真空冷冻干燥技术,在真空度为6.0Pa下,进行真空干燥,即可得到高强度的负载铋系异质结的石墨烯光催化材料。
最后应说明的是:以上所述仅为本发明的优选实施例而已,并不用于限制本发明,尽管参照前述实施例对本发明进行了详细的说明,对于本领域的技术人员来说,其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换。凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (7)
1.一种负载铋系异质结的氧化石墨烯光催化材料的制备方法,其特征在于,包括以下步骤:
首先制备BiOI/BixNbOy光催化剂和氧化石墨烯,将合成的BiOI/BixNbOy异质结催化剂负载于氧化石墨烯纳米片上,以负载后的石墨烯纳米片为前驱体,采用定向真空冷冻干燥技术,对预冷冻处理后的化合物进行真空干燥处理,得到具有高强度的负载铋系异质结的氧化石墨烯光催化材料。
2.根据权利要求1所述负载铋系异质结的氧化石墨烯光催化材料的制备方法,其特征在于,采用Nb2O5和Bi5(NO3)3·5H2O制备BiOI/BixNbOy光催化剂。
3.根据权利要求1所述负载铋系异质结的氧化石墨烯光催化材料的制备方法,其特征在于,BiOI/BixNbOy光催化剂的制备过程中添加表面活性剂,合成BiOI/BixNbOy异质结光催化剂。
4.根据权利要求1所述负载铋系异质结的氧化石墨烯光催化材料的制备方法,其特征在于,所述表面活性剂为柠檬酸钠、十二烷基苯磺酸钠或溴化十六烷基三甲胺。
5.根据权利要求1所述负载铋系异质结的氧化石墨烯光催化材料的制备方法,其特征在于,在真空冷冻干燥的过程中,真空度为3.3~13pa。
6.一种权利要求1-5中任一项所述的方法制备的负载铋系异质结的氧化石墨烯光催化材料。
7.权利要求6所述负载铋系异质结的氧化石墨烯光催化材料应用于对水体POPs的降解。
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CN104069844A (zh) * | 2014-07-23 | 2014-10-01 | 武汉理工大学 | 一种分级三维多孔石墨烯/二氧化钛光催化剂及其制备方法 |
CN106732681A (zh) * | 2016-12-07 | 2017-05-31 | 湖北工业大学 | 三维泡沫状还原石墨烯碘氧化铋复合光催化剂的制备方法 |
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CN113522321B (zh) * | 2021-07-07 | 2022-07-01 | 浙江大学 | 一种表面/体相结可见光催化剂及其制备方法 |
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