CN113368883A - 一种0D/3D Fe2O3 QDs/g-C3N4杂化光芬顿催化剂的制备方法 - Google Patents
一种0D/3D Fe2O3 QDs/g-C3N4杂化光芬顿催化剂的制备方法 Download PDFInfo
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Abstract
本发明公开了一种0D/3D Fe2O3 QDs/g‑C3N4杂化光芬顿催化剂的制备方法，该方法以三聚氰胺和三聚氰酸为原料，采用一步煅烧法制备三维多孔结构的g‑C3N4；通过合适比例的三维g‑C3N4、FeCl3·6H2O和NH4HCO3混合，经简单的自组装合成Fe2O3 QDs/g‑C3N4光芬顿催化剂。该催化剂具有良好的可见光响应、优异的有害污染物降解力和重复利用稳定性，较经典光芬顿催化剂具有更宽的工作范围；该制备方法工艺简单、原料成本低、易于大规模生产。
Description
技术领域
本发明属于降解环境污染物的光芬顿催化剂的制备技术领域，具体涉及一种0D/3D Fe2O3 QDs/g-C3N4杂化光芬顿催化剂的制备方法。
背景技术
铁基催化剂因其毒性小、成本低、富集度高而被广泛应用于非均相芬顿中，但其催化活性通常较低，Fe3+-Fe2+之间的转化较慢，高酸条件下铁浸出，造成催化剂流失，因此，研究人员在增强Fe2+基催化剂的芬顿反应方面做了诸多努力，其中将半导体材料引入Fe2+基催化剂来增强其催化活性。
半导体材料的引入促进了Fe3+-Fe2+转化，提高了降解效率，其中Fe2O3被认为是最有前途的候选材料。但因半导体电荷迁移缓慢、中心缺乏高活性位点等特性，结果并不令人满意。常规Fe2O3纳米粒子因团聚作用，其表面活性位点数量减少，因此，开发具有丰富活性中心位点的高效Fe2O3催化剂具有重要意义。
0D量子点（quantum dots，QDs）的短程有序、大表面积和大量结构缺陷，可以提供大量的活性位点。近来，研究人员采用在2D纳米材料g-C3N4表面负载0D量子点的方法，有效的减少了量子点的自聚现象。但2D材料较薄和较细尺寸，都增加了将其从催化剂悬浮液中分离的难度。理论上，采用在三维纳米材料表面负载量子点的方式，不仅抑制了2D结构层的积累，也促进有机物的吸附和固液分离。
发明内容
本发明解决的技术问题是提供了一种具有良好的可见光响应的0D/3D Fe2O3 QDs/g-C3N4杂化光芬顿催化剂的制备方法，该方法采用一步煅烧法制备具有三维多孔结构的g-C3N4，通过合适比例的三维g-C3N4、FeCl3·6H2O和NH4HCO3混合，经简单的自组装合成Fe2O3QDs/g-C3N4光芬顿催化剂；在可见光下，通过添加H2O2降解有机污染物来评价催化剂的催化性能。该光芬顿催化剂具有良好的可见光响应、优异的有害污染物降解力和重复利用稳定性，较经典光芬顿催化剂具有更宽的光谱工作范围。
本发明为解决上述技术问题采用如下技术方案，一种0D/3D Fe2O3 QDs/g-C3N4杂化光芬顿催化剂的制备方法，其特征在于具体步骤为：
步骤S1：3D多孔g-C3N4的制备
配制三聚氰胺和三聚氰酸混合水溶液，搅拌使其分散均匀后，再转移至培养皿中于60℃进行干燥得到前体物；将干燥后的前驱物研磨，于550℃退火处理2-4h即得到微黄色的3D多孔g-C3N4样品；
步骤S2：0D/3D Fe2O3 QDs/g-C3N4杂化光芬顿催化剂的制备
将步骤S1得到的3D多孔g-C3N4样品分散于乙醇中，磁力搅拌以实现均匀分散得到g-C3N4乙醇分散液，再向上述分散液中添加FeCl3·6H2O和NH4HCO3并搅拌混合均匀，将产物离心、洗涤，并于60℃干燥过夜；然后于350℃退火处理2-4h即得到0D/3D Fe2O3 QDs/ g-C3N4光芬顿催化剂。
进一步限定，步骤S1中所述三聚氰胺与三聚氰酸的投料质量比为1:1，三聚氰胺和三聚氰酸混合水溶液中三聚氰胺和三聚氰酸质量分数均为2%。
进一步限定，步骤S2中所述g-C3N4乙醇分散液中g-C3N4的质量分数为0.9%-2%，FeCl3·6H2O和NH4HCO3与中g-C3N4对应的质量比分别为13.5%-30%和12%-26.5%。
本发明与现有技术相比具有以下有益效果：
1、本发明制得的0D/3D Fe2O3 QDs/g-C3N4杂化光芬顿催化剂具有良好的可见光响应、优异的有害污染物降解力和重复利用稳定性，较经典光芬顿催化剂具有更宽的光谱工作范围，可广泛应用于常见有机污染物的降解；
2、本发明制备0D/3D Fe2O3 QDs/g-C3N4杂化光芬顿催化剂的方法原料成本低廉、制备工艺简单且易于大规模生产；
3、本发明制备的0D/3D Fe2O3 QDs/g-C3N4杂化光芬顿催化剂为一种0D/3D杂化纳米材料，在三维多孔g-C3N4上负载Fe2O3量子点，Fe2O3 QDs为光芬顿反应提供活性位点，三维多孔g-C3N4具有较大的比表面积，具有良好的可见光响应和污染物降解能力。
附图说明
图1是本发明的制备工艺流程图；
图2是本发明制备的0D/3D Fe2O3 QDs/g-C3N4杂化光芬顿催化剂的紫外-可见漫反射吸收光谱图；
图3是本发明制备的0D/3D Fe2O3 QDs/g-C3N4杂化光芬顿催化剂的场发射电子扫描显微镜图；
图4是本发明制备的0D/3D Fe2O3 QDs/g-C3N4杂化光芬顿催化剂的透射电子显微镜图；
图5是本发明制备的0D/3D杂化的Fe2O3 QDs/g-C3N4光芬顿催化剂的罗丹明B（RhB）的去除效果图。
具体实施方式
以下通过实施例对本发明的上述内容做进一步详细说明，但不应该将此理解为本发明上述主题的范围仅限于以下的实施例，凡基于本发明上述内容实现的技术均属于本发明的范围。
实施例1
首先，取2.0g三聚氰胺和2.0g三聚氰酸溶于100mL超纯水中，搅拌12h；然后将上述溶液转移至玻璃皿中，于60℃干燥12h；将所得前体物研磨，于550℃退火处理4h，即得到微黄色的3D多孔g-C3N4样品。取0.9g上述3D多孔g-C3N4样品分散于100mL乙醇中，磁力搅拌2h以实现均匀分散得到g-C3N4乙醇分散液，向上述分散液中添加0.27g FeCl3·6H2O和0.24gNH4HCO3并搅拌12h，将产物离心、洗涤，并于60℃干燥过夜；于350℃退火处理2h，即得到Fe2O3 QDs/g-C3N4光芬顿催化剂。
实施例2
首先，取2.0g三聚氰胺和2.0g三聚氰酸溶于100mL超纯水中，搅拌12h；然后将上述溶液转移至玻璃皿中，于60℃干燥12h；将所得前体物研磨，于550℃退火处理4h，即得到微黄色的3D多孔g-C3N4样品。取1.5g上述3D多孔g-C3N4样品分散于100mL乙醇中，磁力搅拌2h以实现均匀分散得到g-C3N4乙醇分散液，向上述分散液中添加0.27g FeCl3·6H2O和0.24gNH4HCO3并搅拌12h，将产物离心、洗涤，并于60℃干燥过夜；于350℃退火处理2h，即得到Fe2O3 QDs/g-C3N4光芬顿催化剂。
实施例3
取80mL浓度为20mg/L RhB溶液，再加入实施例2中制备的Fe2O3 QDs/g-C3N4光芬顿催化剂，经暗光搅拌10min，取样过滤分析，然后加入1.5mL的双氧水（H2O2，30wt%），开启光源、开始计时，分别在20min，40min，60min，80min时间点取样过滤分析，在可见光下反应60min后，溶液中RhB的去除率大于99%，效果详见图5。
以上实施例描述了本发明的基本原理、主要特征及优点，本行业的技术人员应该了解，本发明不受上述实施例的限制，上述实施例和说明书中描述的只是说明本发明的原理，在不脱离本发明原理的范围下，本发明还会有各种变化和改进，这些变化和改进均落入本发明保护的范围内。
Claims (3)
1.一种0D/3D Fe2O3 QDs/g-C3N4杂化光芬顿催化剂的制备方法，其特征在于具体步骤为：
步骤S1：3D多孔g-C3N4的制备
配制三聚氰胺和三聚氰酸混合水溶液，搅拌使其分散均匀后，再转移至培养皿中于60℃进行干燥得到前体物；将干燥后的前驱物研磨，于550℃退火处理2-4h即得到微黄色的3D多孔g-C3N4样品；
步骤S2：0D/3D Fe2O3 QDs/g-C3N4杂化光芬顿催化剂的制备
将步骤S1得到的3D多孔g-C3N4样品分散于乙醇中，磁力搅拌以实现均匀分散得到g-C3N4乙醇分散液，再向上述分散液中添加FeCl3·6H2O和NH4HCO3并搅拌混合均匀，将产物离心、洗涤，并于60℃干燥过夜；然后于350℃退火处理2-4h即得到0D/3D Fe2O3 QDs/ g-C3N4光芬顿催化剂。
2. 根据权利要求1所述的0D/3D Fe2O3 QDs/g-C3N4杂化光芬顿催化剂的制备方法，其特征在于：步骤S1中所述三聚氰胺与三聚氰酸的投料质量比为1:1，三聚氰胺和三聚氰酸混合水溶液中三聚氰胺和三聚氰酸质量分数均为2%。
3.根据权利要求1所述的0D/3D Fe2O3 QDs/g-C3N4杂化光芬顿催化剂的制备方法，其特征在于：步骤S2中所述g-C3N4乙醇分散液中g-C3N4的质量分数为0.9%-2%，FeCl3·6H2O和NH4HCO3与中g-C3N4对应的质量比分别为13.5%-30%和12%-26.5%。
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