CN109225309A - 一种基于石墨相氮化碳的复合光催化剂的制备方法及应用 - Google Patents
一种基于石墨相氮化碳的复合光催化剂的制备方法及应用 Download PDFInfo
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Abstract
本发明公开了一种基于石墨相氮化碳的复合光催化剂的制备方法及应用,其化学式为Pt/MoS2/g‑C3N4。其制备方法为:首先通过光化学法将具有层状结构的MoS2沉积到片状g‑C3N4的表面,然后再通过光化学法将具有纳米颗粒结构的Pt沉积到片状g‑C3N4的表面,最后再通过在低温下进行退火得到Pt/MoS2/g‑C3N4复合光催化剂。本发明所提供的制备方法,工艺简单,反应条件温和,产率高。Pt和MoS2双助催化剂的协同沉积可以大幅增强g‑C3N4在可见光下的性能,所制备的复合光催化剂Pt/MoS2/g‑C3N4在可见光下表现出良好的光催化性能,在可见光下的产氢速率达到911.5μmol/h,4小时内可以将220ppmV的甲苯降解93%,可用于能源与环境等领域。
Description
技术领域
本发明属于光催化技术领域,尤其涉及一种基于石墨相氮化碳的复合光催化剂的制备方法及应用。
背景技术
随着全球经济的高速发展,日益严重的全球能源短缺和环境污染问题已经受到国际社会和各国政府的高度关注。作为最大的发展中国家,中国面临着前所未有的能源与环境双重考验。自从Fujishima和Honda在n-型半导体二氧化钛单晶电极上发现水的光解现象以来,半导体光催化技术因其有望成为利用太阳能缓解污染和能源问题的绿色手段而得到越来越多的关注。
光催化剂的物理与化学性质对光催化反应有决定性的影响,现在常用的TiO2光催化剂由于光谱响应范围窄、只能吸收紫外光的不足影响了其光催化的实际应用。为了充分利用太阳能,研究者们开发出了一系列具有可见光响应的新型光催化材料体系,如金属硫化物、g-C3N4、金属有机框架(MOF)材料等。其中,聚合物半导体石墨相氮化碳(g-C3N4)因其独特的半导体能带结构和优异的化学稳定性,作为一种不含金属组分的可见光光催化剂被引入到光催化领域,用于光解水产氢产氧、光催化有机选择性合成、光催化降解有机污染物等,引起人们的广泛关注。
对于单组分g-C3N4光催化剂而言,虽然可以通过调控其尺寸、维度、晶化度、和缺陷浓度等方面来促进光生电荷的分离,但是其调控程度仍受限于单组分本身的限制,即光生电子和光生空穴在迁移至g-C3N4表面发生光催化反应前仍处于同一局域范围内,二者存在着较大的复合几率,导致光催化效率偏低。如果能从空间上将光生电子和光生空穴分离,就可以有效抑制光生载流子的复合,从而提高g-C3N4的光催化性能。在这样的指导思想下,基于g-C3N4的复合型光催化材料应运而生,如MoS2/g-C3N4、Bi2MoO6/g-C3N4、Pt/g-C3N4、ZnO/g-C3N4、Bi/g-C3N4等。
现代科学技术的发展对材料的性能提出了更高的要求,而简单地将两种或多种材料复合常常已难以胜任。对于复合型光催化剂的有效构建,不仅仅局限于两种或多种组分的简单复合,而是在此基础上,如何更加有效地发挥各个组分的作用、优势及组分间的协同效应。g-C3N4虽然是一种低成本、可量产的可见光催化剂,但其价带位置高,氧化能力不足,难以破坏苯环结构实现彻底降解,对含苯环的有机污染物降解能力有限;同时,g-C3N4催化剂介于有机和无机材料之间,电荷的平均自由程短,结构缺陷多,光催化性能相对较低。因此,针对单一光催化剂g-C3N4光催化性能低的不足,设计合成基于g-C3N4的高性能复合型光催化剂已成为当前g-C3N4研究方向的热点之一。
发明内容
本发明目的是针对g-C3N4光催化性能低的问题,提供一种基于石墨相氮化碳的复合光催化剂的制备方法及其在光催化领域中的应用。该复合光催化剂可以有效分离光生载流子,充分发挥每个组分的优势,利用组分之间的协同作用,可以有效增强g-C3N4的光催化性能,包括分解水制氢和降解有机污染物。
本发明是通过以下技术方案实现的:
一种基于石墨相氮化碳的复合光催化剂,其化学式为Pt/MoS2/g-C3N4,首先通过光化学法将具有层状结构的石墨相硫化钼沉积到g-C3N4表面,然后再利用光化学法将小尺寸的纳米颗粒Pt沉积到MoS2/g-C3N4表面,最后将样品进行退火,得到Pt/MoS2/g-C3N4复合光催化剂。作为助催化剂,Pt和MoS2具有较低的还原电势,能降低光催化还原反应的活化能。同时,通过光化学法将Pt和MoS2沉积到g-C3N4表面,不仅可以有效地抑制Pt和MoS2的生长和团聚,可以更大几率地提高Pt和MoS2助催化剂在光催化反应中的效率。因此,通过光化学法构建的Pt/MoS2/g-C3N4复合光催化剂,可以充分发挥各个组分的作用和优势,通过调控助催化剂和g-C3N4之间的协同作用,能够大幅增强g-C3N4光催化的性能,并用于分解水制氢和降解有机污染物。
所述的基于石墨相氮化碳的复合光催化剂的制备方法包括以下步骤:
(1)将g-C3N4粉体和一定量的四硫代钼酸铵(NH4)2MoS4加入到含有去离子水的光催化反应器中,搅拌形成均匀的悬浮液,加入空穴牺牲试剂,然后通入惰性气体0.5-2小时,排尽光催化反应器中的空气,在光照的条件下进行光化学反应,过滤、洗涤、干燥,得到MoS2/g-C3N4复合材料;
(2)将步骤1得到的MoS2/g-C3N4复合材料分散于含有空穴牺牲试剂的光催化反应器中,加入一定量的金属Pt前驱体,然后通入惰性气体0.5-2小时,排尽光催化反应器中的空气,在光照的条件下进行光化学反应,过滤、洗涤、干燥,得到Pt/MoS2/g-C3N4复合材料;
(3)将步骤2得到的Pt/MoS2/g-C3N4复合材料置于管式炉中,在通入惰性气体的条件下进行退火,最后得到Pt/MoS2/g-C3N4复合光催化材料。
所述步骤1和2中,空穴牺牲试剂选自Na2S/Na2SO3、KI、甲醇、乙醇、三乙醇胺中的任意一种。
所述步骤1和2中光化学反应指的是在可见光或紫外光的激发下进行的光催化反应,反应时间为0.1-10小时。
所述步骤1中MoS2/g-C3N4复合材料中MoS2的负载量为0.1-10 wt%。
所述步骤2中金属Pt前驱体为含铂的无机化合物。
优选的,所述步骤2中金属Pt前驱体为硝酸铂Pt(NO3)2、氯化铂PtCl4、氯铂酸H2PtCl6、氯铂酸钾K2PtCl6中的任意一种。
所述步骤2中Pt/MoS2/g-C3N4复合材料中Pt的负载量为0.1-5 wt%。
所述步骤3中退火温度为100-400℃,退火时间为0.5-6小时。
优选的,制备过程中使用的惰性气体为氮气或氩气。
本发明的原理为:
对于Pt/MoS2/g-C3N4复合光催化材料,在可见光激发下,g-C3N4带隙激发产生光生电子和光生空穴。由于Pt和MoS2的费米能级低于g-C3N4的导带电势,光生电子会从g-C3N4的导带跃迁至Pt或MoS2的表面,从而延长光生载流子的寿命,降低光生载流子的复合几率。其次,由于助催化剂Pt和MoS2具有更低的析氢电势,能降低光催化还原反应的势垒或者活化能,从而提高光催化反应的速率。其次,助催化剂Pt和MoS2在g-C3N4表面的沉积是通过g-C3N4表面的光生电子原位光还原反应所致,相比于常规合成方法可以有效抑制Pt或MoS2的生长或者团聚,这有利于降低光生载流子的迁移路径。最后,在惰性气氛下的后退火过程可以提高助催化剂的结晶度,增强助催化剂与g-C3N4之间的相互作用。因此,通过Pt和MoS2的光化学沉积,能显著增强g-C3N4的光催化性能,包括分解水制氢和光催化降解有机污染物。
本发明的优点是:
1、本发明所提供的制备方法,其操作简易,反应条件温和,且产率高,是一种环境友好的制备方法。
2、本发明通过光化学法将贵金属Pt和石墨相MoS2沉积于g-C3N4表面,能有效抑制Pt或MoS2的生长或团聚、提高光生载流子的分离效率、并降低光催化还原反应的活化能,制备过程中没有使用还原型或者氧化型试剂,如H2、NaBH4、NaOH等,合成工艺简单,可宏观制备。
3、本发明所制备的Pt/MoS2/g-C3N4复合光催化剂在可见光下具有优异的光催化性能,包括光解水制氢和降解有机污染物,且具有良好的光催化稳定性,有利于能源和环境领域的可持续发展。
附图说明
图1所示为实施例1制备的g-C3N4、MoS2/g-C3N4和Pt/MoS2/g-C3N4的X射线衍射谱图。
图2所示为实施例2制备的Pt/MoS2/g-C3N4的透射电镜图和高分辨透射电镜图。
图3所示为实施例2制备的g-C3N4、MoS2/g-C3N4、Pt/g-C3N4和Pt/MoS2/g-C3N4在可见光下光催化制氢的活性结果图。
图4所示为实施例3制备的g-C3N4、MoS2/g-C3N4、Pt/g-C3N4和Pt/MoS2/g-C3N4在可见光下光催化降解甲苯的活性结果图。
具体实施方式
以下结合具体的实例对本发明的技术方案做进一步说明:
实施例1
称取0.5克的g-C3N4粉体,加入到含有100毫升去离子水的光催化反应器中,搅拌,使g-C3N4粉体充分悬浮于去离子水中;
向上述悬浮液中加入203微升四硫代钼酸铵(NH4)2MoS4水溶液(浓度为40克/升),充分搅拌10分钟,然后密封光催化反应器;
向上述光催化反应器中通入氮气(流速40毫升/分钟)30分钟,以排尽反应器中残留的空气,然后开始在可见光下光照反应4小时。反应结束后,过滤、洗涤、干燥,得到MoS2含量为1 wt%的MoS2/g-C3N4复合材料;
称取上述得到的MoS2/g-C3N4复合材料200毫克,加入到含有120毫升去离子水的光催化反应器中,然后加入66微升氯铂酸H2PtCl6水溶液(浓度为40克/升),搅拌10分钟得到均匀的悬浮液。然后通入氮气以排尽反应器中残留的空气, 开始在可见光下光照反应3小时。反应结束后,过滤、洗涤、干燥,得到Pt含量为0.5 wt%的Pt/MoS2/g-C3N4复合材料;
最后,将上述Pt/MoS2/g-C3N4复合材料置于200℃的氮气管式炉中退火2小时,从而获得Pt/MoS2/g-C3N4复合光催化剂,其中MoS2的含量为1 wt%,Pt的含量为0.5 wt%。
对上述过程中的g-C3N4、MoS2/g-C3N4和Pt/MoS2/g-C3N4进行X射线衍射测试,其结构如图1所示。图1中,A为g-C3N4的X射线衍射谱图,B为MoS2/g-C3N4的X射线衍射谱图,C为Pt/MoS2/g-C3N4的X射线衍射谱图。MoS2/g-C3N4、Pt/MoS2/g-C3N4和g-C3N4的X射线衍射谱图并没有明显区别,三者均在衍射角度2θ为27.7°处有明显的衍射峰,对应g-C3N4类石墨结构的(002)面间衍射。同时,在MoS2/g-C3N4和Pt/MoS2/g-C3N4的XRD谱图中没有探测到MoS2和Pt颗粒的衍射峰,表明助催化剂的沉积并没有破坏g-C3N4的长程有序结构。
实施例2
称取1克的g-C3N4粉体,加入到含有120毫升去离子水的光催化反应器中,然后加入812微升四硫代钼酸铵(NH4)2MoS4水溶液(浓度为40克/升)和30毫升三乙醇胺TEOA,搅拌30分钟得到均匀的悬浮液。通入氩气以排尽反应器中残留的空气,密封光催化反应器,在紫外光下光照反应4小时。反应结束后,过滤、洗涤、干燥,得到MoS2含量为2 wt%的MoS2/g-C3N4复合材料;
称取上述得到的MoS2/g-C3N4复合材料500毫克,加入到含有150毫升去离子水的光催化反应器中,然后加入205微升硝酸铂Pt(NO3)2(浓度为40克/升)和30毫升三乙醇胺TEOA,搅拌20分钟得到均匀的悬浮液。然后通入氩气以排尽反应器中残留的空气, 开始在紫外光下光照反应4小时。反应结束后,过滤、洗涤、干燥,得到Pt含量为1 wt%的Pt/MoS2/g-C3N4复合材料;
最后,将上述Pt/MoS2/g-C3N4复合材料置于氩气300℃的管式炉中退火1小时,从而获得Pt/MoS2/g-C3N4复合光催化剂,其中MoS2的含量为2 wt%,Pt的含量为1 wt%。
对得到的Pt/MoS2/g-C3N4复合光催化剂进行透射电镜分析,其结果如图2所示。通过光化学沉积,MoS2和Pt分别以层状材料结构和纳米颗粒结构的形式负载于片状g-C3N4的表面。从高分辨电镜照片可以看出,层状材料结构的晶面间距为0.62 nm,对应于六方相硫化钼(002)的晶面,而纳米颗粒的晶面间距为0.225 nm,对应于立方相铂(111)的晶面,Pt纳米颗粒的平均粒径为4.7 nm。从图2可以得出,通过光化学沉积可以将Pt、MoS2和g-C3N4这三种组分紧密结合在一起,从而能够促进g-C3N4上光生电子能够有效地转移到Pt和MoS2上,促进光生载流子分离,达到增强g-C3N4光催化性能的目的。
以光催化分解水制氢来评估上述光催化剂的性能。光源为300瓦氙灯(北京泊菲莱科技有限公司,PLS-SXE300型,实际输出功率为47瓦,可见光输出功率为19.6瓦),通过外接半透半反镜和长通滤光片(波长≥420纳米),从而保证光催化反应的激发光为可见光。
具体的光催化实验步骤如下:(1)称取10毫克的光催化剂粉末,加入到含有80毫升去离子水和20毫升三乙醇胺TEOA的光催化反应器中,搅拌均匀;(2)密封光催化反应器,通入氩气,以排尽光催化反应器中残留的空气,然后开始光催化制氢反应;(3)每隔一个小时取一次样,利用气相色谱仪(科晓GC 1690C,分子筛填充柱,氩气为载气,TCD检测器)检测氢气产量,并计算8小时的平均产氢速率,其结果如图3所示。
图3是g-C3N4、MoS2/g-C3N4、Pt/g-C3N4和Pt/MoS2/g-C3N4在可见光光催化制氢的活性结果图。首先,对于单一组分g-C3N4而言,在可见光下的产氢速率为25.9 μmol/h,表现出较低的光催化制氢活性。其次,当在g-C3N4中加入一种助催化剂Pt或者MoS2,其光催化制氢性能得到了一定的提升。对于MoS2/g-C3N4和Pt/g-C3N4而言,其产氢速率分别为30.7和355 μmol/h,表明贵金属Pt更有利于光催化制氢。再次,当中g-C3N4中同时沉积两种助催化剂Pt和MoS2时,其光催化制氢速率得到了进一步提升,达到911.5 μmol/h。该产氢速率是单一组分g-C3N4的35.2倍,是MoS2/g-C3N4和Pt/g-C3N4的29.7和2.6倍,表明双助催化剂Pt和MoS2的协同沉积可以大幅增强g-C3N4光催化制氢的性能。
实施例3
称取2克的g-C3N4粉体,加入到含有150毫升去离子水的光催化反应器中,然后加入4.06毫升四硫代钼酸铵(NH4)2MoS4水溶液(浓度为40克/升)和20毫升甲醇CH3OH,搅拌45分钟得到均匀的悬浮液。通入氩气以排尽反应器中残留的空气,密封光催化反应器,在紫外光下光照反应4小时。反应结束后,过滤、洗涤、干燥,得到MoS2含量为5 wt%的MoS2/g-C3N4复合材料;
称取上述得到的MoS2/g-C3N4复合材料600毫克,加入到含有150毫升去离子水的光催化反应器中,然后加入750微升氯铂酸钾K2PtCl6水溶液(浓度为40克/升)和20毫升甲醇CH3OH,搅拌30分钟得到均匀的悬浮液。然后通入氩气以排尽反应器中残留的空气, 开始在紫外光下光照反应4小时。反应结束后,过滤、洗涤、干燥,得到Pt含量为2 wt%的Pt/MoS2/g-C3N4复合材料;
最后,将上述Pt/MoS2/g-C3N4复合材料置于250℃的氦气管式炉中退火1.5小时,从而获得Pt/MoS2/g-C3N4复合光催化剂,其中MoS2的含量为5 wt%,Pt的含量为2 wt%。
以光催化降解甲苯来评估上述光催化剂光催化降解有机污染物的性能。光源为300瓦氙灯(北京泊菲莱科技有限公司,PLS-SXE300型,实际输出功率为47瓦,可见光输出功率为19.6瓦),通过外接半透半反镜和长通滤光片(波长≥420纳米),从而保证光催化反应的激发光为可见光。
具体的光催化实验步骤如下:(1)称取200毫克的光催化剂粉末,在超声的作用下将其均匀地分散在含有5克的无水乙醇的培养皿(直径5厘米)中,然后在80℃下将其烘干;(2)将上述培养皿置于光催化反应器中,在常温常压下密封反应器。反应前,以100 毫升/分钟流量的高纯空气吹扫反应器,以排除反应器和气路管道中的CO2、甲苯等气体。密封采集窗口,保持系统压力为常压,其中氧气含量为22%,相对湿度为23%;(3)手动注射一定体积的甲苯气体于反应器中,等待30分钟,使反应器内甲苯气体与空气混合均匀,达到一个稳定浓度后,通过气相色谱仪(科晓GC 1690C,毛细管柱,氮气为载气,FID检测器)测定此时甲苯的初始浓度为220 ppmV;(4)开始光催化反应,并开始计时。4小时后,从反应器内采集一定体积的气体,通过气相色谱仪(科晓GC 1690C,毛细管柱,氮气为载气,FID检测器,甲烷转化炉)进行在线分析,分析光催化反应过程中甲苯的含量。
图4是g-C3N4、MoS2/g-C3N4、Pt/g-C3N4和Pt/MoS2/g-C3N4在可见光光催化降解甲苯的活性结果图。首先,对于单一组分g-C3N4而言,经过4小时的光催化反应,在可见光下对甲苯的降解率仅为21%。其次,当在g-C3N4中加入一种助催化剂Pt或者MoS2,光催化降解甲苯的性能也得到了一定的提升。对于MoS2/g-C3N4和Pt/g-C3N4而言,对甲苯的降解率分别提升至41%和47%。再次,当中g-C3N4中同时沉积两种助催化剂Pt和MoS2时,光催化降解甲苯的性能得到显著的增强,4小时可以将220 ppmV的甲苯降解93%,显示出良好的光催化降解有机污染物性能,表明双助催化剂Pt和MoS2的协同沉积也可以大幅增强g-C3N4光催化降解有机污染物的性能。
以上实施例的说明只是用于帮助理解本发明的方法及其核心思想。应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明原理的前提下,还可以对本发明进行若干改进和修饰,这些改进和修饰也落入本发明权利要求的保护范围内,如(1)本发明专利采用g-C3N4作为光催化剂,利用光化学法将助催化剂Pt和MoS2沉积到g-C3N4表面,来实现对g-C3N4光催化性能的增强。以此类推,也可以使用其他光催化材料,如TiO2、CdS等,通过光照沉积将助催化剂沉积到其表面,以实现对光催化性能的增强;(2)本发明专利通过构建Pt/MoS2/g-C3N4复合光催化剂,利用Pt和MoS2双助催化剂的协同作用来增强g-C3N4的光催化性能。以此类推,也可以将其他的石墨相材料(如MoSe2等)或者金属纳米颗粒(如Au、Pd、Ag等)沉积到g-C3N4表面。对所公开的实施例的上述说明,使本领域专业技术人员能够实现或使用本发明。对这些实施例的多种修改对本领域的专业技术人员来说将是显而易见的,本文中所定义的一般原理可以在不脱离本发明的精神或范围的情况下,在其他实施例中实现。因此,本发明将不会被限制于本文所述的这些实施例,而是要符合于本文所公开的原理和新颖特点相一致的最宽的范围。
Claims (10)
1.一种基于石墨相氮化碳的复合光催化剂,其化学式为Pt/MoS2/g-C3N4,其特征在于,通过光化学法将贵金属Pt和石墨相MoS2沉积于g-C3N4表面,增强g-C3N4的光催化性能,并用于分解水制氢和降解有机污染物。
2.根据权利要求1所述的基于石墨相氮化碳的复合光催化剂,其特征在于,所述光催化剂的制备方法包括以下步骤:
(1)将g-C3N4粉体和一定量的四硫代钼酸铵(NH4)2MoS4加入到含有去离子水的光催化反应器中,搅拌形成均匀的悬浮液,加入空穴牺牲试剂,然后通入惰性气体0.5-2小时,排尽光催化反应器中的空气,在光照的条件下进行光化学反应,过滤、洗涤、干燥,得到MoS2/g-C3N4复合材料;
(2)将步骤1得到的MoS2/g-C3N4复合材料分散于含有空穴牺牲试剂的光催化反应器中,加入一定量的金属Pt前驱体,然后通入惰性气体0.5-2小时,排尽光催化反应器中的空气,在光照的条件下进行光化学反应,过滤、洗涤、干燥,得到Pt/MoS2/g-C3N4复合材料;
(3)将步骤2得到的Pt/MoS2/g-C3N4复合材料置于管式炉中,在通入惰性气体的条件下进行退火,最后得到Pt/MoS2/g-C3N4复合光催化材料。
3.根据权利要求2所述的基于石墨相氮化碳的复合光催化剂的制备方法,其特征在于,所述步骤1和2中,空穴牺牲试剂选自Na2S/Na2SO3、KI、甲醇、乙醇、三乙醇胺中的任意一种。
4.根据权利要求2所述的基于石墨相氮化碳的复合光催化剂的制备方法,其特征在于,所述步骤1和2中光化学反应指的是在可见光或紫外光的激发下进行的光催化反应,反应时间为0.1-10小时。
5.根据权利要求2所述的基于石墨相氮化碳的复合光催化剂的制备方法,其特征在于,所述步骤1中MoS2/g-C3N4复合材料中MoS2的负载量为0.1-10 wt%。
6.根据权利要求2所述的基于石墨相氮化碳的复合光催化剂的制备方法,其特征在于,所述步骤2中金属Pt前驱体为含铂的无机化合物。
7.根据权利要求2所述的基于石墨相氮化碳的复合光催化剂的制备方法,其特征在于,所述步骤2中金属Pt前驱体为硝酸铂Pt(NO3)2、氯化铂PtCl4、氯铂酸H2PtCl6、氯铂酸钾K2PtCl6中的任意一种。
8.根据权利要求2所述的基于石墨相氮化碳的复合光催化剂的制备方法,其特征在于,所述步骤2中Pt/MoS2/g-C3N4复合材料中Pt的负载量为0.1-5 wt%。
9.根据权利要求2所述的基于石墨相氮化碳的复合光催化剂的制备方法,其特征在于,所述步骤3中退火温度为100-400℃,退火时间为0.5-6小时。
10.根据权利要求2所述的基于石墨相氮化碳的复合光催化剂的制备方法,其特征在于,制备过程中使用的惰性气体为氮气或氩气。
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