CN114471536A - 一种氧空位浓度可调的MnCr2O4光催化剂及其制备方法与应用 - Google Patents
一种氧空位浓度可调的MnCr2O4光催化剂及其制备方法与应用 Download PDFInfo
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Abstract
本发明涉及一种氧空位浓度可调的MnCr2O4光催化剂及其制备方法与应用。将纯MnCr2O4放入管式炉中,将管式炉在未加热情况下通氢气0.5h,然后将样品在管式炉烧制2小时,并持续向管式炉内通入氢气,并在500℃下焙烧。本发明通过退火在纯MnCr2O4内引入氧空位来提高MnCr2O4的光催化活性,适当地改变退火温度引入氧空位降解异丙醇,与纯MnCr2O4比较,在120分钟时,活性比纯MnCr2O4提高了约11.4倍,因此适当引入氧空位,这样有利于提高电荷空穴的分离效率,提高可见光吸收与光催化活性。
Description
技术领域
本发明属于光催化材料技术领域,具体涉及一种氧空位浓度可调的MnCr2O4光催化剂及其制备方法与应用。
背景技术
随着社会的进步与经济的高速发展,能源危机与环境污染的问题日渐突出。环境污染不但严重影响人类的身体健康,也给社会带来了难以估量的经济损失,环境污染的控制与治理是人类二十一世纪面临和等待解决的重大课题。催化技术在环境净化中具有广阔的发展前景,有害物质通过光催化,热催化,电催化等技术有效的降解。由于光催化技术在解决环境污染与有机物降解中具有突出有效作用,因此这项技术引起了科研人员广泛的兴趣。
发明内容
本发明提供一种氧空位浓度可调的MnCr2O4光催化剂及其制备方法,该方法简单,成本低,易操作,并且在解决环境污染与有机物降解中具有突出有效作用。
一种氧空位浓度可调的MnCr2O4光催化剂,制备方法包括如下步骤,将纯MnCr2O4放入管式炉中,将管式炉在未加热情况下通氢气0.5h,然后将样品在管式炉烧制2小时,并持续向管式炉内通入氢气。
上述的一种氧空位浓度可调的MnCr2O4光催化剂,烧制的温度为500℃。
上述的一种氧空位浓度可调的MnCr2O4光催化剂,管式炉升温速率为3℃/min;氢气流速为50sccm。
上述的一种氧空位浓度可调的MnCr2O4光催化剂,所述纯MnCr2O4的制备方法包括如下步骤:将铬盐与锰盐分别加入去离子水中,充分搅拌溶解,混合均匀后加入柠檬酸,继续搅拌,得溶胶体;将溶胶体置于烘箱中烘干,得前驱体;将所得前驱体研磨,在管式炉中空气环境下进行煅烧,得目标产物。
上述的一种氧空位浓度可调的MnCr2O4光催化剂,所述铬盐为九水硝酸铬;所述锰盐为六水合硝酸锰;按摩尔比,Cr(NO3)3·9H2O:Mn(NO3)2·6H2O=2:1。
上述的一种氧空位浓度可调的MnCr2O4光催化剂,所述柠檬酸为一水合柠檬酸,加入量为铬盐与锰盐总摩尔的1.2倍;搅拌时间为2小时。
上述的一种氧空位浓度可调的MnCr2O4光催化剂,步骤4)中,所述煅烧,煅烧温度为600℃,煅烧时间为4小时。
上述的一种氧空位浓度可调的MnCr2O4光催化剂在光催化降解气体污染物中的应用。
上述的应用,所述的气体污染物为异丙醇。
上述的应用,方法如下:在光催化反应器中加入上述任意一项一种氧空位浓度可调的MnCr2O4光催化剂,再加入气体异丙醇,在氙灯下光催化降解。
本发明的有益效果是:
1、本发明所需材料成本较低,环境友好,由钼盐与锌盐合成的一种氧空位浓度可调的MnCr2O4光催化剂,结构稳定,具有较高的光催化活性。
2、本发明提供的一种氧空位浓度可调的MnCr2O4光催化剂,通过引入氧缺陷,禁带变窄,显著提高了光催化活性。
3、本发明提供的一种氧空位浓度可调的MnCr2O4光催化剂,窄的禁带宽度有利于提高电荷空穴的分离效率,延长光生载流子的复合时间,从而提高光催化活性。
4、本发明通过退火在纯MnCr2O4内引入氧空位来提高MnCr2O4的光催化活性,适当地改变退火温度引入氧空位降解异丙醇,与纯MnCr2O4比较,在120分钟时,活性比纯MnCr2O4提高了约11.4倍,因此适当引入氧空位,这样有利于提高电荷空穴的分离效率,提高可见光吸收与光催化活性。
附图说明
图1为纯MnCr2O4、MnCr2O4-500-120的XRD对比图。
图2为本发明制备的一种氧空位浓度可调亚铬酸锰降解异丙醇后生成丙酮量图。
图3为本发明的氧空位浓度可调的MnCr2O4光催化剂降解异丙醇光催化机理图。
具体实施方式
实施例1
(一)亚铬酸锰(MnCr2O4)粉末,制备方法包括以下步骤:
1)将0.4g(2mmol)九水硝酸铬和0.287g(1mmol)六水合硝酸锰分别溶于50ml去离子水中,搅拌0.5h,混合均匀。
2)将步骤1)所得混合溶液中加入0.757g一水合柠檬酸,室温搅拌2h,搅拌均匀,得溶胶体。
3)将步骤2)所得溶胶体置于120℃鼓风干燥箱中,烘干10-12h,得前驱体。
4)将步骤3)所得前驱体研磨后,置于管式炉中,600℃下焙烧4小时,得亚铬酸锰。
5)将纯MnCr2O4放入管式炉中,将管式炉在未加热情况下通氢气0.5h,保证管式炉内部是无氧环境,然后将样品在管式炉烧制2小时,并持续向管式炉内通入氢气(氢气流速为50sccm),并在500℃下焙烧。(管式炉升温速率为3℃/min),得到氧空位浓度可调的MnCr2O4光催化剂,记为MnCr2O4-500-2h。
(二)检测
图1为纯MnCr2O4和MnCr2O4-500-2h的XRD对比图,由JADE的标准卡片可见,样品MnCr2O4-500-2h多出一个峰,此峰为Mn3O4的一个峰,MnCr2O4-500-2h的其他峰与MnCr2O4标准卡基本一致,证明成功合成氧空位浓度可调的亚铬酸锰纳米材料。
实施例2
氧空位浓度可调的MnCr2O4光催化剂在光催化降解气体污染物中的应用
方法:分别称取0.1g实施例1制备的纯MnCr2O4、和MnCr2O4-500-2h放于光催化反应器内,抽取5μL异丙醇,打入反应器内。反应两小时。用氙灯照射两小时,用气相色谱仪器分析。
图2为本发明制备的一种氧空位浓度可调亚铬酸锰降解异丙醇后生成丙酮量图。通过适当地改变退火温度引入氧空位降解异丙醇,与纯MnCr2O4比较,2小时内异丙醇持续降解,在120分钟时,活性比纯MnCr2O4提高了约11.4倍。这是由于适当引入氧空位,会在MnCr2O4的导带下方引入一个施主能级,减小其禁带宽度,进而拓展其光吸收范围,提升其光吸收能力。其次,表面氧空位形成的施主能级能吸引且束缚光生电子,提升载流子的分离效率,延长光生载流子的复合时间,从而提升其光催化活性。此外,氧空位的存在将提升MnCr2O4对O2分子的吸附能力,有利于后续催化反应的进行,从而提高氧空位浓度可调亚铬酸锰光催化降解异丙醇的活性。
实施例3
氧空位浓度可调的MnCr2O4光催化剂在光催化降解异丙醇的原理
氧空位浓度可调的MnCr2O4纳米材料在氙灯的光照下产生大量的光生电子与空穴,氧空位的存在会产生施主能级,施主能级能够吸引且束缚光生电子,提升载流子分离效率。材料表面吸附的O2可以与光生电子反应产生超氧化物·O2 -和过氧化物·O2 2-,吸附在表面的OH-可以与空穴反应生成羟基自由基·OH,如图3所示。当异丙醇吸附在含氧空位浓度可调的MnCr2O4纳米材料表面,·O2 -、·O2 2-和·OH将吸附的异丙醇氧化成丙酮,最后丙酮氧化成水和CO2。
Claims (10)
1.一种氧空位浓度可调的MnCr2O4光催化剂,其特征在于,制备方法包括如下步骤,将纯MnCr2O4放入管式炉中,将管式炉在未加热情况下通氢气0.5h,然后将样品在管式炉烧制2小时,并持续向管式炉内通入氢气。
2.根据权利要求1所述的一种氧空位浓度可调的MnCr2O4光催化剂,其特征在于,烧制的温度为500℃。
3.根据权利要求1所述的一种氧空位浓度可调的MnCr2O4光催化剂,其特征在于,管式炉升温速率为3℃/min;氢气流速为50sccm。
4.根据权利要求1或2或3所述的一种氧空位浓度可调的MnCr2O4光催化剂,其特征在于,所述纯MnCr2O4的制备方法包括如下步骤:
1)将铬盐与锰盐分别加入去离子水中,充分搅拌溶解,混合均匀后加入柠檬酸,继续搅拌,得溶胶体;将溶胶体置于烘箱中烘干,得前驱体;将所得前驱体研磨,在管式炉中空气环境下进行煅烧,得目标产物。
5.根据权利要求4所述的一种氧空位浓度可调的MnCr2O4光催化剂,其特征在于,所述铬盐为九水硝酸铬;所述锰盐为六水合硝酸锰;按摩尔比,Cr(NO3)3·9H2O:Mn(NO3)2·6H2O=2:1。
6.根据权利要求5所述的一种氧空位浓度可调的MnCr2O4光催化剂,其特征在于,所述柠檬酸为一水合柠檬酸,加入量为铬盐与锰盐总摩尔的1.2倍;搅拌时间为2小时。
7.根据权利要求6所述的一种氧空位浓度可调的MnCr2O4光催化剂,其特征在于,步骤4)中,所述煅烧,煅烧温度为600℃,煅烧时间为4小时。
8.权利要求1-7任意一项所述的一种氧空位浓度可调的MnCr2O4光催化剂在光催化降解气体污染物中的应用。
9.根据权利要求8所述的应用,其特征在于,所述的气体污染物为异丙醇。
10.根据权利要求9所述的应用,其特征在于,方法如下:在光催化反应器中加入权利要求1-7任意一项所述的一种氧空位浓度可调的MnCr2O4光催化剂,再加入气体异丙醇,在氙灯下光催化降解。
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