CN106391089B - 一种高效降解对硝基苯酚的氮化碳负载氧化铁光催化剂 - Google Patents
一种高效降解对硝基苯酚的氮化碳负载氧化铁光催化剂 Download PDFInfo
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Abstract
一种高效降解对硝基苯酚的氮化碳负载氧化铁光催化剂，属于纳米材料制备领域。制备方法为：采用热聚合法制备得到载体g‑C3N4，将所得的样品研磨成粉末备用。采用等体积浸渍法制备Fe2O3/g‑C3N4，称取一定量的硝酸铁，以异丙醇作为溶剂，利用等体积浸渍法将硝酸铁溶液浸渍至载体中，将所得混合物转移管式炉中，以1℃/min的速率从室温升至350℃，保温3h,得到Fe2O3/g‑C3N4。本发明所制备的本发明制备得到的Fe2O3/g‑C3N4催化剂对对硝基苯酚表现出优异的光催化性能。本发明具有原料廉价易得，制备过程简单，产量高，在光催化领域具有良好的应用前景。
Description
技术领域
本发明涉及一种Fe2O3/g-C3N4:高效降解对硝基苯酚的光催化剂、其制备方法及其对对硝基苯酚的光催化氧化，具体的涉及采用热聚合法以盐酸胍作为前驱体制备二维g-C3N4纳米片，采用等体积浸渍法制备g-C3N4负载Fe2O3的光催化剂，得到对对硝基苯酚具有高光催化氧化活性的复合半导体纳米催化剂，属于纳米材料制备领域。
背景技术
随着工业的迅猛发展，全国各地出现严重的水体污染问题。水体污染治理成为环境治理工作的重中之重。含酚废水由于成分复杂、在环境中停留时间长、高毒性和难降解性，是造成水体污染的主要来源。以对硝基苯酚为例，传统的废水处理方法主要有物理方法、化学方法以及生物降解法。但是，传统处理方法存在成本高、工艺复杂，以及二次污染等问题。光催化是一种新型的废水处理技术，具有处理效率高、反应条件温和、无二次污染等优点。半导体在光催化过程中产生的空穴有很强的氧化性，可以氧化分解绝大部分的有机物，在室温下可实现对有机污染物的深度矿化。因此，利用光催化氧化方法实现废水中对硝基苯酚的高效氧化具有重要的发展前景，而光催化剂的性能是决定能否有效消除对硝基苯酚的关键。
氮化碳作为一种富电子有机半导体，禁带宽度约为2.7eV,由于其独特的电子能带结构和优异的物理化学性质,使得在光催化方面有巨大的应用前景。查阅文献得知，不同半导体之间进行复合可以提高体系的电荷分离效率，扩展光谱响应范围，提高催化剂活性。例如，朱永法等人将C3N4和有机超导体TCNQ进行复合，得到层层结构；TCNQ与C3N4通过π-π作用降低价带位置0.3eV，增强光催化剂的氧化能力；光催化降解苯酚活性提高了6倍；可见光活性拓展至600nm(Y.F.Zhu et al.J.Mater.Chem.A 2014,2(29),11432–11438)。王心晨等人选择半导体MoS2与g-C3N4复合形成超薄异质结，MoS2/g-C3N4体系的光生电荷分离以及传输效率提高；在可见光下光解水产氢、产氧量子效率分别达到2.1％和1.1％(X.C.Wang etal.Angew.Chem.Int.Ed.2013，52(13),3621–3625)。据我们所知，目前没有报道将Fe2O3/g-C3N4复合型催化剂应用于对硝基苯酚的光催化氧化。
发明内容
本发明的目的在于提供一种高效光催化氧化对硝基苯酚的Fe2O3/g-C3N4纳米催化剂及其制备方法，具体涉及采用热聚合法制备载体g-C3N4，采用等体积浸渍法制备Fe2O3/g-C3N4，应用于对硝基苯酚的光催化氧化。
Fe2O3/g-C3N4:高效降解对硝基苯酚的光催化剂，其制备主要包括以下步骤：将一定量的盐酸胍称量至坩埚中，加盖密封，转移至马弗炉内，以2.3℃/min的速率从室温升至550℃，保温4h，自然冷却至室温，研磨成粉末备用；
采用等体积浸渍法制备Fe2O3/g-C3N4纳米催化剂，催化剂具体制备如下：称取一定量的Fe(NO3)3·9H2O，溶解于异丙醇中，搅拌30min得到均匀溶液，取适量上述溶液滴加至g-C3N4中，静置，干燥，将得到的混合物转移至管式炉中，通入N2(优选200mL/min),以1℃/min的速率从室温升至350℃，保温3h，自然冷却至室温得到Fe2O3/g-C3N4催化剂。
上述Fe2O3/g-C3N4催化剂中Fe2O3的负载量为0.1wt％-0.8wt％，优选0.5wt％。
在可见光照射下，将Fe2O3/g-C3N4催化剂加入到初始浓度为0.2mmol/L对硝基苯酚溶液中，加入30wt％的H2O2溶液,加入HCl调节pH至3.5。每0.1g催化剂对应0.6mL H2O2溶液，对应100mL对硝基苯酚溶液；负载0.5wt％Fe2O3/g-C3N4的光催化活性最好，光照射40min后，对硝基苯酚转化率达95％，比g-C3N4纳米片的提高了约6倍。
本发明具有原料廉价易得，制备过程简单，产量较高等特征。本发明制备得到的Fe2O3/g-C3N4催化剂对对硝基苯酚表现出优异的光催化性能。
附图说明
图1为所制得Fe2O3/g-C3N4样品的XRD谱图。其中曲线(a)、(b)、(c)、(d)、(e)、(f)分别为实施例1、实施例2、实施例3、实施例4、实施例5、实施例6催化剂样品的XRD谱图。
图2为所制得Fe2O3/g-C3N4样品的SEM和TEM照片。其中图(a)和(b)分别为g-C3N4的SEM和TEM照片，(c-e)0.5wt％Fe2O3/g-C3N4和(f)0.8wt％Fe2O3/g-C3N4样品的TEM照片。
图3为所制得Fe2O3/g-C3N4样品可见光下对对硝基苯酚的光催化氧化活性。图中曲线分别为实施例1、实施例2、实施例3、实施例4、实施例5、实施例6催化剂可见光照射下在对硝基苯酚初始浓度为0.2mmol/L(0.6mL H2O2)、初始pH为3.5条件下的对硝基苯酚光降解活性曲线。
具体实施方式
为了进一步了解本发明，下面以实施例作详细说明，并给出附图描述本发明得到的对对硝基苯酚具有优异催化活性的Fe2O3/g-C3N4催化剂。
实施例1：称取5g盐酸胍，转移至坩埚中，加盖密封，转移至马弗炉内，以2.3℃/min的速率从室温升至550℃，保温4h，自然冷却至室温，研磨成粉末，得到g-C3N4纳米催化剂。
实施例2：称取5g盐酸胍，转移至坩埚中，加盖密封，转移至马弗炉内，以2.3℃/min的速率从室温升至550℃，保温4h，自然冷却至室温，研磨成粉末，得到g-C3N4纳米催化剂。称取0.097g的Fe(NO3)3·9H2O，溶解于50mL异丙醇中，搅拌30min得到均匀溶液，取1.3mL上述溶液滴加至0.5g g-C3N4中，静置，60℃干燥，将得到的混合物转移至管式炉中，通入N2(200mL/min),以1℃/min的速率从室温升至350℃，保温3h，自然冷却至室温得到0.1wt％Fe2O3/g-C3N4催化剂。
实施例3-6
制备方法同实施例2，不同的是Fe2O3/g-C3N4催化剂的负载量依次为0.3wt％、0.5wt％、0.7wt％、0.8wt％。
本发明制备方法新颖，原料廉价，制备过程简单，且产量较高，所得Fe2O3/g-C3N4纳米材料对对硝基苯酚有良好的光催化氧化性能。
上述实施例所制得Fe2O3/g-C3N4样品的XRD谱图见图1，其中曲线(a)、(b)、(c)、(d)、(e)、(f)分别为g-C3N4，0.1wt％Fe2O3/g-C3N4，0.3wt％Fe2O3/g-C3N4，0.5wt％Fe2O3/g-C3N4，0.7wt％Fe2O3/g-C3N4和0.8wt％Fe2O3/g-C3N4的XRD谱图；所制得的Fe2O3/g-C3N4样品的TEM照片见图2，其中图(a)和(b)分别为g-C3N4的SEM和TEM照片，(c-e)、(f)分别为0.5wt％Fe2O3/g-C3N4和0.8wt％Fe2O3/g-C3N4样品的TEM照片；所制得Fe2O3/g-C3N4样品可见光下对对硝基苯酚的光催化氧化活性见图3。
Claims (5)
1.一种高效降解对硝基苯酚的光催化剂Fe2O3/g-C3N4的制备方法，其特征在于，Fe2O3/g-C3N4催化剂中Fe2O3的负载量为0.1wt％-0.8wt％，包括以下步骤：g-C3N4的制备：将一定量的盐酸胍称量至坩埚中，加盖密封，转移至马弗炉内，以2.3℃/min的速率从室温升至550℃，保温4h，自然冷却至室温，研磨成粉末备用；采用等体积浸渍法制备Fe2O3/g-C3N4纳米催化剂：称取一定量的Fe(NO3)3·9H2O，溶解于异丙醇中，搅拌30min得到均匀溶液，取适量上述溶液滴加至g-C3N4中，静置，干燥，将得到的混合物转移至管式炉中，通入N2，以1℃/min的速率从室温升至350℃，保温3h，自然冷却至室温得到Fe2O3/g-C3N4催化剂。
2.按照权利要求1所述的制备方法，其特征在于，光催化剂Fe2O3/g-C3N4中Fe2O3的负载量为0.5wt％。
3.按照权利要求1或2所述的制备方法制备得到的催化剂Fe2O3/g-C3N4。
4.按照权利要求1或2所述的制备方法制备得到的催化剂Fe2O3/g-C3N4的应用，用于降解对硝基苯酚。
5.按照权利要求4的应用，其特征在于，在可见光照射下，将Fe2O3/g-C3N4催化剂加入到初始浓度为0.2mmol/L对硝基苯酚溶液中，加入30wt％的H2O2溶液,加入HCl调节pH至3.5；每0.1g催化剂对应0.6mL H2O2溶液，对应100ml对硝基苯酚溶液；光照射40min。
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