CN109453792B - 一种在光芬顿反应中抗光腐蚀的硫化物异质结材料的制备方法 - Google Patents
一种在光芬顿反应中抗光腐蚀的硫化物异质结材料的制备方法 Download PDFInfo
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Abstract
一种在光芬顿反应中抗光腐蚀的硫化物异质结材料的制备方法，属于光化学能转换、光催化降解领域。本发明要解决在过氧化氢诱导的强氧化性光芬顿反应中，对硫化物的腐蚀可能加剧的技术问题。本发明方法：一、将α‑Fe2O3纳米颗粒加入到去离子水中，搅拌，然后依次加入Na2MoO4·2H2O和CH4N2S，超声震荡，升温后保温，无水乙醇洗涤3次后离子水洗涤3次，干燥，得到Fe2O3/MoS2；二、将步骤一获得的Fe2O3/MoS2分散于混合溶液中，超声震荡，然后在室温下搅拌使TEOS完全水解，取沉淀物，真空干燥，得到硫化物异质结材料。本发明用于光化学能转换、光催化降解领域。
Description
技术领域
本发明属于光化学能转换、光催化降解领域。
背景技术
自Honda-Fujishima效应发现以来，光催化技术受到了科学界的极大关注[1]。以半导体材料为核心的光催化技术可将太阳能作为光源驱动室温化学反应。在水环境中，光诱导产生的电子和空穴分别与吸附的溶解氧和水分子作用产生具有强氧化性的羟基自由基(·OH)和超氧离子自由基(·O2 -)，这类活性基团具有无选择性的氧化降解有机污染物的能力。不同于现有处理污染物和净化空气的方法,光催化降解是热力学自发行为(ΔG<0)，具有成本低、处理彻底、无二次污染的特点，整个过程遵从于地球上的物质能量循环规律，既达到了治理环境污染又实现了资源利用生态化的目的，是有效解决当前环境问题的一种极佳手段。研究表明，d0和d10金属阳离子构成的氧化物半导体具有光催化性质，对于光催化反应机制的研究也多以这类材料建立模型[2-4]。尽管目前针对光催化本质的探索仍在继续，但科学界普遍认为是三个因素制约着催化效率，从而阻碍了这项技术直接进入产业化。其中包括：(1)太阳光谱利用率——常用的金属氧化物通常仅限紫外光激发，太阳光谱利用率尚不足<5％；(2)光生电荷分离转移效率——光生电荷在体相迅速复合，在迁移过程中也易被杂质或缺陷俘获；(3)表面化学反应效率——到达反应活性位点的电子与质子易于表面复合，逆反应的同时发生也大量消耗载流子。最终导致整个反应的光量子效率较低，催化活性受到严重影响。
早期的研究都集中在如TiO2等的氧化物半导体，但这类材料虽然对环境友好且无生物毒害性，但其多为宽禁带半导体，只能利用紫外光部分，制约了其实用性。赤铁矿相三氧化二铁(α-Fe2O3)是最为稳定的铁氧化合物，并且具有n型半导体特性，近年来多应用在催化领域。它具有绝大多数氧化物半导体的优点，如：化学稳定性、储量丰富、成本低廉、无毒害，更为重要的是，其禁带宽度仅为2.2eV可充分利用可见光谱，并且其可参与氧化降解能力更强的芬顿反应。但Fe2O3亦因其较短的空穴扩散长度(2-4nm)、较高的光生电子空穴对复合率、低电导率等因素限制实际利用率。
基于二维片层结构石墨烯材料优异的物化性质启发，一众类石墨烯二维材料引起人们高度关注。其中，二硫化钼(MoS2)纳米材料具有良好的机械性能、电学性能，以及较窄的带隙和较高的空穴迁移率，是理想的构建异质结构催化剂的重要材料，与之相关的诸多报道如Graphene/MoS2,CdS/MoS2,MoS2/WS2,MoO3/MoS2,and TiO2/MoS2等，都表明基于MoS2的异质结构复合材料表现出优异的光催化性质。因此，构建稳定的Fe2O3/MoS2复合材料是提高光化学利用率的有效光催化材料体系。但硫化物本身的光腐蚀性使其在长效使用过程中存在不稳定隐患，特别是在过氧化氢诱导的强氧化性光芬顿反应中，对硫化物的腐蚀可能加剧。
发明内容
本发明要解决在过氧化氢诱导的强氧化性光芬顿反应中，对硫化物的腐蚀可能加剧的技术问题，而提出了一种在光芬顿反应中抗光腐蚀的硫化物异质结材料的制备方法
为解决上述问题；本发明中一种在光芬顿反应中抗光腐蚀的硫化物异质结材料的制备方法是通过下述步骤完成的：
步骤一、将α-Fe2O3纳米颗粒加入到去离子水中，搅拌，然后依次加入Na2MoO4·2H2O和CH4N2S，超声震荡，升温后保温，无水乙醇洗涤3次后离子水洗涤3次，干燥，得到Fe2O3/MoS2；
步骤二、将步骤一获得的Fe2O3/MoS2分散于混合溶液中，超声震荡，然后在室温下搅拌使TEOS完全水解，取沉淀物，真空干燥，得到硫化物异质结材料；
其中，步骤二所述混合溶液是由TEOS、无水乙醇和NaOH配制成。
进一步限定，步骤一所述α-Fe2O3纳米颗粒是按下述步骤进行的：将5mmolFeCl3·6H2O溶于20mL无水乙醇，超声震荡30min后，陆续加入3.4mL去离子水和5mmol醋酸钠，剧烈搅拌1h，然后在200℃条件下水热反应24h，反应完毕后待冷却至室温，取出固体，无水乙醇洗涤3次，去离子水洗涤3次，于60℃真空干燥箱保温10h后取出待用。
进一步限定，步骤一中将0.25mmol～0.75mmolα-Fe2O3纳米颗粒加入到40mL去离子水；Na2MoO4·2H2O用量为1.5mmol，CH4N2S用量为9mmol。
进一步限定，步骤一在180℃～200℃下保温20h～24h。
进一步限定，步骤二步骤二将0.1g～0.3g Fe2O3/MoS2分散在由80μmol～120μmolTEOS、30mL～50mL无水乙醇和180μL～220μL浓度为0.1M NaOH配制的混合溶液中。
进一步限定，步骤一中超声震荡30min。
进一步限定，步骤二中超声震荡30min
进一步限定，步骤二在80℃下真空干燥1h。
本发明方法制备的异质结构Fe2O3/MoS2纳米复合材料呈三维花状，本发明在光催化剂材料表面浸渍沉积一层非晶Si-氢氧化合物(SiOxH)层，以保护MoS2在光芬顿反应中免受光腐蚀，光催化剂可进行稳定循环使用。
附图说明
图1是SiOxH-Fe2O3/MoS2(SiOxH-3MF)的扫描电镜能谱照片及各元素分布照片；
图2是HRTEM照片，(a)3MF试样，(b)SiOxH-3MF试样；
图3是各试样对30mL 20mg/L的亚甲基蓝(MB)溶液的光催化降解情况；
图4是3MF和SiOxH-3MF在光芬顿反应中对MB溶液的降解情况，内插图为SiOxH-3MF试样5次循环使用结果和降解后两催化剂颜色对比。
具体实施方式
实施例1：本实施例使用的α-Fe2O3纳米颗粒是按下述步骤进行的：将5mmolFeCl3·6H2O溶于20mL无水乙醇，超声震荡30min后，陆续加入3.4mL去离子水和5mmol醋酸钠，以300rpm速率剧烈搅拌1h，然后在200℃条件下水热反应24h，反应完毕后待冷却至室温，取出固体，无水乙醇洗涤3次，去离子水洗涤3次，于60℃真空干燥箱保温10h后取出待用。
本实施中一种在光芬顿反应中抗光腐蚀的硫化物异质结材料的制备方法是通过下述步骤完成的：
步骤一、将0.25mmol、0.375mmol、0.5mmol、0.75mmolα-Fe2O3纳米颗粒分别加入到40mL去离子水中，以300rpm速率搅拌，然后依次加入1.5mmolNa2MoO4·2H2O和9mmolCH4N2S，超声震荡30min，在200℃下保温24h，无水乙醇洗涤3次后离子水洗涤3次，在真空条件下60℃干燥10h，得到Fe2O3/MoS2，所得试样按照Mo:Fe原子比，依次为Mo:Fe＝2,3,4和6,分别记作2MF,3MF,4MF和6MF；
步骤二、将0.2g步骤一获得的Fe2O3/MoS2分散于混合溶液(混合溶液是由100μmolTEOS、40mL无水乙醇和200μL浓度为0.1M NaOH配制的)中，超声震荡30min，然后在室温下搅拌使TEOS完全水解(约24h溶液基本挥发)，取沉淀物，在80℃下真空干燥1h，得到硫化物异质结材料，分别记作SiOxH-2MF，SiOxH-3MF，SiOxH-4MF和SiOxH-6MF。
光催化降解采用300W的氙灯作为光源。在100mL的烧杯中放入10mg的待测试样品粉体及30mL20mg/L的亚甲基蓝指示剂溶液。将烧杯置于光源前方搅拌台上，并固定烧杯与光源的距离为5cm，降解反应过程中保持匀速的磁力搅拌。取相同的时间间隔对反应液进行吸光度检测，并计算出反应液浓度，以此做出降解率与光照时间的曲线，由此对样品的光催化活性进行分析对比，见图3和4。
从图3中可以看出，在光催化反应中3MF样品降解速率最快。而在图4的光芬顿测试中，Fe2O3/MoS2(3MF)样品5分钟左右即降解了全部的亚甲基蓝指示剂，但复合材料中的MoS2被消耗殆尽，样品呈红棕色(Fe2O3颜色)。而沉积了非晶层的SiOxH-Fe2O3/MoS2样品则表现出良好的循环使用情况与可观的光芬顿降解性能，说明由SiOxH非晶层进行表面修饰的硫化物光催化剂稳定性得到显著提高。
Claims (9)
1.一种在光芬顿反应中抗光腐蚀的硫化物异质结材料的制备方法，其特征在于所述制备方法是通过下述步骤完成的：
步骤一、将α-Fe2O3纳米颗粒加入到去离子水中，搅拌，然后依次加入Na2MoO4·2H2O和CH4N2S，超声震荡，升温后保温，无水乙醇洗涤3次后去离子水洗涤3次，干燥，得到Fe2O3/MoS2；
步骤二、将0.1g～0.3g步骤一获得的Fe2O3/MoS2分散在由80μmol～120μmolTEOS、30mL～50mL无水乙醇和180μL～220μL浓度为0.1M NaOH配制的混合溶液中，超声震荡，然后在室温下搅拌使TEOS完全水解，取沉淀物，真空干燥，得到硫化物异质结材料。
2.根据权利要求1所述方法，其特征在于步骤一所述α-Fe2O3纳米颗粒是按下述步骤进行的：将5mmol FeCl3˙6H2O溶于20mL无水乙醇，超声震荡30min后，陆续加入3.4mL去离子水和5mmol醋酸钠，剧烈搅拌1h，然后在200℃条件下水热反应24h，反应完毕后待冷却至室温，取出固体，无水乙醇洗涤3次，去离子水洗涤3次，于60℃真空干燥箱保温10h后取出待用。
3.根据权利要求1所述方法，其特征在于步骤一中将0.25mmol～0.75mmolα-Fe2O3纳米颗粒加入到40mL去离子水。
4.根据权利要求3所述方法，其特征在于步骤一中Na2MoO4·2H2O用量为1.5mmol。
5.根据权利要求4所述方法，其特征在于步骤一中CH4N2S用量为9mmol。
6.根据权利要求1所述方法，其特征在于步骤一在180℃～200℃下保温20h～24h。
7.根据权利要求1所述方法，其特征在于步骤二将0.2g Fe2O3/MoS2分散在由100μmolTEOS、40mL无水乙醇和200μL浓度为0.1M NaOH配制的混合溶液中。
8.根据权利要求1所述方法，其特征在于步骤一超声震荡30min，步骤二超声震荡30min。
9.根据权利要求1所述方法，其特征在于步骤二在80℃下真空干燥1h。
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