CN109012752A - 一种磁性ZnFe2O4/PANI/Au复合光催化剂的制备方法 - Google Patents
一种磁性ZnFe2O4/PANI/Au复合光催化剂的制备方法 Download PDFInfo
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Abstract
本发明公开了一种磁性ZnFe2O4/PANI/Au复合光催化剂的制备方法,具体包含以下步骤:(1).取0.219g(CH3COO)2Zn·2H2O,0.808gFe(NO3)3·9H2O,溶解在16mL甘油,60mL异丙醇混合溶液中;(2).将步骤(1)制备的溶液放置在反应釜中,温度控制在180℃,反应时间为12h;(3)将步骤(2)制备的溶液取出,用水和乙醇各洗三遍,烘干,在马弗炉中温度控制在400℃反应2h,制得ZnFe2O4粉末备用;(4).在ZnFe2O4存在下加入氯金酸和苯胺原位氧化还原制备磁性ZnFe2O4/PANI/Au纳米复合物。本发明合成纳米ZnFe2O4/PANI/Au复合物,通过使ZnFe2O4,聚苯胺和Au的复合使得ZnFe2O4光生电子-空穴有效分离,提升光生载流子的迁移速率,从而改善ZnFe2O4光催化剂性能。由于ZnFe2O4、PANI、Au三者的协同作用使得该纳米复合物在可见光下具有较高的光催化效果。
Description
技术领域
本发明涉及一种磁性ZnFe2O4/PANI/Au复合光催化剂的制备方法。
背景技术
随着人类文明的不断发展进步,有机废水的排放量也日益增大。由于各类化工生产所使用的化工原料种类很多,因此废水中的成分很复杂,可生化性差,色度很高,COD居高不下。各种苯类、卤代烃等大分子物质及各种显色集团均溶解于水中,有的甚至和水形成氢键。燃料废水中的毒性可直接影响人体健康,破坏生态环境。每年有大于5.5万亿立方米的水的淡水受到污染,这样的形势非常严峻。因此,有机废水的处理一直受到国内外的广泛关注。但由于成分复杂,使废水的处理难度很大。
特别是进入20世纪以来,有毒,难降解有机污染物(如农药,染料等)导致了水体污染,现在环境水体的污染已经成为影响人类的生命健康的重大问题。然而传统的水处理方法,例如:混凝法、吸附法、膜过滤分离、化学沉淀法等方法在实际处理中还是存在一定的困难,且处理效果不是很理想。但通过光催化的方法利用太阳能,可以将对环境中有毒、难降解解有机污染物实现完全降解。这一方法被认为是解决人类环境问题最行之有效的技术方案之一。
近年来,在光催化制氢、光敏化太阳能电池、治理有机污染物等方面的研究半导体材料的应用极其广泛。在众多的半导体中,纳米级半导体材料更是倍受青睐。铁酸锌作为一种稳定的材料,在磁性材料、传感器、光催化降解有机物等方面被得到了广泛应用。由于其具有很小的带隙(约为1.9eV)和优质的光化学稳定性,这使得铁酸锌在光催化方面表现出很大的优越性,大量的研究表明,纳米铁酸锌材料具有良好的光催化特性。与普通的纳米材料相比,中空结构纳米微球具有比表面积大,表面渗透性强,密度低,光学性能优,稳定性强等优点,表现出更加优异的性能。迄今为止,许多学者成功地合成了SiO2,TiO2,Sb2S3,SnO2,MnO2,Fe3O4等中空微球,在这些中空结构中,磁性材料中空微球在许多领域中具有潜在的应用;
以TiO2为基础的的半导体光催化剂是目前最被广泛应用和接受的光催化剂,但有很多关键性的技术性难题有待解决,(1)量子效率低(~4%);难以处理量大且浓度高的废气和废水,难以实现光催化分解水制氢产业化;(2)太阳能利用率低;由于TiO2半导体的能带结构(Eg=3.2eV)决定了其只能吸收利用紫外光或太阳光中的紫外线部分(太阳光中紫外辐射仅占~5%);(3)多相光催化反应机理尚不十分明确;以半导体能带理论为基础的光催化理论难以解释许多实验现象,使得改进和开发新型高效光催化剂的研究工作盲目性大;(4)光催化应用中的技术难题;如在液相反应体系中光催化剂的负载技术和分离回收技术,在气相反应体系中光催化剂的成膜技术及光催化剂活性稳定性问题;上述关键问题也是目前国内外光催化领域的研究焦点,围绕这些问题开展进一步研究不仅可望在光催化基础理论方面获得较大的突破,而且有利于促进光催化技术真正能在上述众多领域得到大规模广泛工业应用。
发明内容
本发明目的是提供一种磁性ZnFe2O4/PANI/Au复合光催化剂的制备方法,它能有效地解决背景技术中所存在的问题。
一种磁性ZnFe2O4/PANI/Au复合光催化剂的制备方法,具体包含以下步骤:
(1).准备16mL的甘油,60mL的异丙醇,搅拌溶解备用;
(2).取0.219g(CH3COO)2Zn·2H2O,0.808gFe(NO3)3·9H2O,溶解在步骤(1)制备的溶液中;
(3).将步骤(2)制备的溶液放置在反应釜中,温度控制在180℃,反应时间为12h;
(4).将步骤(3)制备的溶液取出,实用离心机用水和乙醇各洗三遍,烘干,在马弗炉中温度控制在400℃反应2h,然后进行冷却研磨,即可制得ZnFe2O4粉末备用;
(5).取0.1928g步骤(4)制备的ZnFe2O4粉末放入到装有100ml的烧杯中,再将100ml的水倒入烧杯中,再加入4mL的苯胺,搅拌2h;
(6).在步骤(5)制备的溶液中加入1.2mLHAuCl4,继续搅拌4h;
(7)将步骤(6)制得的产物使用水和乙醇再各洗三遍,放在温度为60℃的烘箱中烘干,时间24h取出。
由于采用了以上技术方案,本发明具有以下有益效果:本发明合成纳米ZnFe2O4/PANI/Au复合物,通过使ZnFe2O4,聚苯胺和Au的复合使得ZnFe2O4光生电子-空穴的有效分离,提升光生载流子的迁移速率,并使其吸收波长范围得到扩展,从而改善ZnFe2O4光催化剂性能,研究了该复合物对有机污染物甲基橙的降解作用,结果表明由于ZnFe2O4、PANI、Au三者的协同作用使得该纳米复合物在可见光下具有较高的光催化效果。
附图说明
为了更清楚地说明本发明,下面将结合附图对实施例作简单的介绍。
图1是实施例2中ZnFe2O4的扫描电镜图(左低倍镜图,右高倍镜图);
图2是实施例3中ZnFe2O4/PANI/Au的扫描电镜图(左低倍镜图,右高倍镜图);
图3是实施例4中ZnFe2O4和ZnFe2O4/PANI/Au复合物的紫外光谱图;
图4是实施例5中ZnFe2O4和ZnFe2O4/PANI/Au红外谱图;
图5是实施例6中ZnFe2O4和ZnFe2O4/PANI/Au复合物XRD图;
图6是实施例7中磁铁吸附下和常态下的ZnFe2O4/PANI/Au溶液的对比图;
图7是实施例8中可见光照射下ZnFe2O4/PANI/Au样品光催化降解甲基橙(1×10- 5mol/L,50mL)过程的紫外—可见光谱图;
图8是实施例9中ZnFe2O4/PANI/Au复合光催化剂的可循环性检测图。
具体实施方式
为了使本发明实现的技术手段、创作特征、达成目的与功效易于明白了解,下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述。
实施例
实验药品
硝酸铁(Ⅲ)九水合物(上海麦克林生物化学公司)
Zn(Ac)2·9H2O(烧杯盛放)
甘油(aladdin公司生产)
苯胺(国药集团化学试剂有限公司)
异丙醇(天津博迪化工股份有限公司)
实验仪器
陶瓷坩埚
马弗炉
SHA-B水浴恒温振荡器
KQ-250DB型数控超声波清洗器
BS224S电子天平
TGL16M离心机
DHG-9101A电热恒温鼓风干燥箱
量筒(10ml,100ml)、容量瓶、玻璃棒、磁力搅拌器、磁力搅拌子、一次性手套、标签、100ml烧杯、100ml高温加热反应釜。
实施例1
一种磁性ZnFe2O4/PANI/Au复合光催化剂的制备方法,具体包含以下步骤:
(1).准备16mL的甘油,60mL的异丙醇,搅拌溶解备用;
(2).取0.219g(CH3COO)2Zn·2H2O,0.808gFe(NO3)3·9H2O,溶解在步骤(1)制备的溶液中;
(3).将步骤(2)制备的溶液放置在反应釜中,温度控制在180℃,反应时间为12h;
(4).将步骤(3)制备的溶液取出,实用离心机用水和乙醇各洗三遍,烘干,在马弗炉中温度控制在400℃反应2h,然后进行冷却研磨,即可制得ZnFe2O4粉末备用;
(5).取0.1928g步骤(4)制备的ZnFe2O4粉末放入到装有100ml的烧杯中,再将100ml的水倒入烧杯中,再加入4mL的苯胺,搅拌2h;
(6).在步骤(5)制备的溶液中加入1.2mLHAuCl4,继续搅拌4h;
(7)将步骤(6)制得的产物使用水和乙醇再各洗三遍,放在温度为60℃的烘箱中烘干,时间24h取出。
实施例2
参看图1,ZnFe2O4的扫描电镜图,左图的倍数较低,从整体上看分布较为均匀,密集。球形大小在150nm左右,表面不光滑。右图是ZnFe2O4的高倍镜图,可以看到ZnFe2O4的较直观具体的形貌。与左图相比,球形的表面粗糙,可见ZnFe2O4纳米球是由更小的颗粒组装而成的。
实施例3
参看图2,ZnFe2O4/PANI/Au的扫描电镜图,从左图可以看出复合物的形貌跟ZnFe2O4相比变化很大,球的尺寸变大,这是因为复合上了Au和聚苯胺的缘故。右图是左图的放大图,在大颗粒的表面分布有一些小颗粒,应该是Au的纳米颗粒。聚苯胺和Au包裹在ZnFe2O4外面形成品相较好的复合光催化剂,可见前期的制备工作还是有成果的。
实施例4
参看图3,跟ZnFe2O4的紫外光谱图相比,ZnFe2O4/PANI/Au纳米复合物在可见光强的吸收明显增强,这是因为复合上了Au和聚苯胺的缘故,一方面表明成功制备了三者的复合物,另一面说明复合物可以做可见光催化剂。
实施例5
参看图4,ZnFe2O4/PANI/Au复合物的红外光谱图中出现了聚苯胺的特征峰,在1577cm-1和1494cm-1分别对应醌式结构和苯式结构的特征峰。3500cm-1左右的是氨基的特征峰。进一步证明了复合物中聚苯胺的存在。
实施例6
参看图5,ZnFe2O4的XRD图中出现了ZnFe2O4的特征峰,无杂质峰存在,表明了得到了纯的ZnFe2O4纳米晶体。而复合物ZnFe2O4/PANI/Au ZnFe2O4的特征峰外,出现了Au的几个特征峰,表明了Au的存在,但强度相对较弱,这可能与Au在复合物中的含量较少有关。另外在2θ为15°出现的峰是苯胺的特征峰。XRD图进一步证明了成功制备了ZnFe2O4/PANI/Au三者的纳米复合物。
实施例7
参看图6,对于这种催化剂,它的磁性是目前存在的很多光催化剂所不具备的。因此我们专门设计了实验来验证ZnFe2O4/PANI/Au具有磁性。实验如图,从实验的对比图可以看出ZnFe2O4/PANI/Au复合光催化剂具有很好的磁性。在右侧的磁铁吸附下,ZnFe2O4/PANI/Au几乎全部被吸附在试管右侧。
实施例8
参看图7,为了证明所制得的ZnFe2O4/PANI/Au纳米复合物在光催化降解有机污染物有潜在的应用,我们研究了室温下在水溶液中光催化降解甲基橙的实验。甲基橙分子在可见光下(无复合物样品)是稳定的。另外,在暗反应时ZnFe2O4/PANI/Au复合光催化剂对甲基橙几乎无催化降解活性。因此,为了有效地催化降解甲基橙,光照是必须的,甲基橙的降解是在复合物样品存在下由光反应引起的。甲基橙的特征吸收峰被用来监控光催化降解情况。图8为所合成的ZnFe2O4/PANI/Au样品纳米复合物在可见光照射下光催化降解甲基橙的活性。从图中可以看出,随时间的延长,特征吸收峰峰强度明显降低,100分钟后,几乎完全消失,这表明甲基橙彻底被降解。光催化结果表明,样品ZnFe2O4/PANI/Au纳米复合物显示出较好的光催化活性。
实施例9
参看图8,图8是检测ZnFe2O4/PANI/Au复合光催化剂能否被循环利用的检测图。一共做了五次对相同浓度1×10-3mol/L的甲基橙的降解实验。从图中看每次都可以将甲基橙基本全部降解,说明ZnFe2O4/PANI/Au复合光催化剂具有很好的催化性能且可循环性很好。
最后应说明的是:以上实施例仅用以说明本发明的技术方案,而非对其限制;尽管参照前述实施例对本发明进行了详细的说明,本领域的普通技术人员应当理解,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;而这些修改或者替换,并不使相应技术方案的本质脱离本发明各实施例技术方案的精神和范围。
Claims (1)
1.一种磁性ZnFe2O4/PANI/Au复合光催化剂的制备方法,其特征在于具体包含以下步骤:
(1).准备16mL的甘油,60mL的异丙醇,搅拌溶解备用;
(2).取0.219g(CH3COO)2Zn·2H2O,0.808gFe(NO3)3·9H2O,溶解在步骤(1)制备的溶液中;
(3).将步骤(2)制备的溶液放置在反应釜中,温度控制在180℃,反应时间为12h;
(4).将步骤(3)制备的溶液取出,实用离心机用水和乙醇各洗三遍,烘干,在马弗炉中温度控制在400℃反应2h,然后进行冷却研磨,即可制得ZnFe2O4粉末备用;
(5).取0.1928g步骤(4)制备的ZnFe2O4粉末放入到装有100ml的烧杯中,再将100ml的水倒入烧杯中,再加入4mL的苯胺,搅拌2h;
(6).在步骤(5)制备的溶液中加入1.2mLHAuCl4,继续搅拌4h;
(7)将步骤(6)制得的产物使用水和乙醇再各洗三遍,放在温度为60℃的烘箱中烘干,时间24h取出。
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