CN114956177B - 一种多酸衍生的镉钼双金属六棱柱纳米材料 - Google Patents
一种多酸衍生的镉钼双金属六棱柱纳米材料 Download PDFInfo
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- 239000002086 nanomaterial Substances 0.000 title claims abstract description 32
- LRWQWQFSOAMWKT-UHFFFAOYSA-N [Cd].[Mo] Chemical compound [Cd].[Mo] LRWQWQFSOAMWKT-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 239000011941 photocatalyst Substances 0.000 claims abstract description 10
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000002360 preparation method Methods 0.000 claims abstract description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 239000002131 composite material Substances 0.000 claims description 4
- -1 polytetrafluoroethylene Polymers 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 3
- 239000011148 porous material Substances 0.000 claims 2
- 238000005054 agglomeration Methods 0.000 claims 1
- 230000002776 aggregation Effects 0.000 claims 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 21
- 239000001257 hydrogen Substances 0.000 abstract description 21
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 21
- 230000001699 photocatalysis Effects 0.000 abstract description 20
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- DHRLEVQXOMLTIM-UHFFFAOYSA-N phosphoric acid;trioxomolybdenum Chemical compound O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.OP(O)(O)=O DHRLEVQXOMLTIM-UHFFFAOYSA-N 0.000 abstract description 7
- 238000000034 method Methods 0.000 abstract description 4
- 229910052724 xenon Inorganic materials 0.000 abstract description 4
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 3
- XIEPJMXMMWZAAV-UHFFFAOYSA-N cadmium nitrate Inorganic materials [Cd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XIEPJMXMMWZAAV-UHFFFAOYSA-N 0.000 abstract description 2
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 2
- 238000003860 storage Methods 0.000 abstract description 2
- 229910052717 sulfur Inorganic materials 0.000 abstract description 2
- NMHMNPHRMNGLLB-UHFFFAOYSA-N phloretic acid Chemical compound OC(=O)CCC1=CC=C(O)C=C1 NMHMNPHRMNGLLB-UHFFFAOYSA-N 0.000 abstract 1
- 238000000354 decomposition reaction Methods 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 229910052980 cadmium sulfide Inorganic materials 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 238000001000 micrograph Methods 0.000 description 4
- 229910052979 sodium sulfide Inorganic materials 0.000 description 4
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 229940101006 anhydrous sodium sulfite Drugs 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 3
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 150000001661 cadmium Chemical class 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 239000002803 fossil fuel Substances 0.000 description 2
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- 229910000510 noble metal Inorganic materials 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 206010034972 Photosensitivity reaction Diseases 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical group [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
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- 230000007613 environmental effect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000005431 greenhouse gas Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000036211 photosensitivity Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229940001482 sodium sulfite Drugs 0.000 description 1
- 235000010265 sodium sulphite Nutrition 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
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Abstract
本发明涉及光催化析氢领域一种多酸衍生的镉钼双金属六棱柱纳米材料的制备及其应用。本发明的目的是解决现有技术合成高性能光催化剂的制备方法复杂、原材料储备稀少、光催化活性较低和造价昂贵的问题。本专利设计与研制了一种多酸衍生的镉钼双金属六棱柱纳米材料CdS‑MoS2‑1。所采用的方法:以Keggin型磷钼酸、硫脲和硝酸镉为原料,采用一步水热合成方法,制备的多酸衍生的镉钼双金属六棱柱纳米材料可适用于以Na2S和Na2SO3为牺牲剂的光催化析氢反应,在以上条件中光催化平均产氢效率可达到1190μmol g‑1h‑1,并且具有优秀的光催化稳定性,在500W氙灯为光源的照射下进行30小时的5个循环测试中光催化活性没有明显下降,具有非常好的循环稳定性。
Description
技术领域
本发明涉及光催化析氢领域。
背景技术
世界人口的广泛增长推动了能源的消耗,世界也需要更多可再生的清洁能源。传统 能源中的化石燃料存在许多缺点,如燃烧产物为温室气体、储存有限等,化石资源的过度 消耗也导致对替代能源的需求不断增加。为了满足未来的能源需求,开发和寻找清洁且具有可再生性的替代能源成为一项重要任务。在各种可再生能源中,太阳能因其清洁、易获取和可再生等优点,可以作为缓解与化石燃料有关的环境问题和能源危机的可行替代品,将太阳能转化和储存为分子间的化学键已被考虑用于解决全球能源危机。其中,氢能也作为一种替代品,具有最高的能量密度、小密度、轻质量、可再生性以及燃烧产物对环境无污染等优点,所以,氢能被认为是最清洁燃料。它可以通过太阳光分解水来产生。为了扩 大氢能的潜力,有必要开发一种廉价高效的制氢方法。贵金属材料通常具有优秀的光催化 性能,例如,铂和贵金属氧化物。然而,铂族材料的高成本和稀缺性限制了其大规模和可 持续的应用。多金属氧酸盐(POMs)作为一种纳米尺寸的富氧金属簇合物,可以在不改变其结构的情况下进行多电子转移,并且允许分子水平的修饰,因此多酸可作为半导体光催 化剂的候选者。
发明内容
基于以上背景,本发明的目的是提供一种多钼酸构筑的镍金属硫化物的制备及其光 催化应用,制备方法简便,成本低。制备所得到的纳米材料具有较高的产氢速率和良好的稳定性
本发明的目的是这样实现的:
一种多酸衍生的镉钼双金属六棱柱纳米材料,包括以下步骤:
一、称取H3(PMo12O40)·6H2O(0.1902g,0.0956mmol),Cd(NO3)2·4H2O(0.193g,0.625mmol)和硫脲(0.2375g,3.125mmol)溶解于10mL的去离子水中,在室温条件 下搅拌1小时。
步骤一中所述的磷钼酸与金属镉盐的摩尔比为:(1~4):1;
二、将上述溶液转移至25mL聚四氟乙烯反应釜中,在200℃下保持24小时, 降温后得到CdS-MoS2双金属复合光催化剂,产物水洗数次,在60℃下干燥24小时。
上述的多酸衍生的镉钼双金属六棱柱纳米材料的应用,主要是在光催化分解水析氢 方面。
上述应用方法如下:以硫化钠和无水亚硫酸钠作为牺牲剂,光催化分解水产氢的体 系为产氢最高的催化体系,平均产氢效率为1190μmol g-1h-1,从而得出本发明的一种多酸衍生的镉钼双金属六棱柱纳米材料是一种高效的光催化分解水的光催化剂。
与现有技术相比,本发明具有如下特点:
本发明采用简单的一步水热合成法,以Keggin型磷钼酸,金属盐硝酸镉和硫源硫脲 为原料,制备了一种多酸衍生的镉钼双金属六棱柱纳米材料是一种高效的光催化分解水制 氢的光催化剂。本发明制备的一种多酸衍生的镉钼双金属六棱柱纳米材料不但具有良好光敏性的磷钼酸和强还原性金属镉原子,而且这种光催化剂具有纳米六棱柱结构,具有更多 的反应活性位点,从而具有良好的光催化分解水产氢的效果。以500W氙灯为光源,以 硫化钠和无水亚硫酸钠作为牺牲剂,平均产氢效率为1190μmol g-1h-1。并且,在此光源的照射下进行30小时的5个循环测试中光催化活性没有丧失,具有非常好的循环稳定 性。
本发明可获得一种多酸衍生的镉钼双金属六棱柱纳米材料。
附图说明
图1为本发明实施例一所制备的一种多酸衍生的镉钼双金属六棱柱纳米材料与MoS2(JCPDS Card No.37-1492)、CdS(JCPDS Card No.47-1179)XRD谱图。
图2为本发明实施例一所制备的一种多酸衍生的镉钼双金属六棱柱纳米材料扫描电 镜图。
图3为本发明实施例一所制备的一种多酸衍生的镉钼双金属六棱柱纳米材料透射电 镜图。
图4为本发明实施例一所制备的一种多酸衍生的镉钼双金属六棱柱纳米材料BET测 试图。
图5为本发明实施例一所制备的一种多酸衍生的镉钼双金属六棱柱纳米材料与Keggin型磷钼酸、硫化镉的光催化产氢速率对比图。
图6为本发明实施例一所制备的一种多酸衍生的镉钼双金属六棱柱纳米材料的催化 循环稳定性。
图7为本发明实施例一所制备的一种多酸衍生的镉钼双金属六棱柱纳米材料的实验 方案示意图。
具体实施方式
下面结合附图和实施例对本发明进行详细的说明。
实施例一,一种多酸衍生的镉钼双金属六棱柱纳米材料,包括如下制备步骤:
(1)称取H3(PMo12O40)·6H2O(0.1902g,0.0956mmol),Cd(NO3)2·4H2O(0.193g,0.625 mmol)和硫脲(0.2375g,3.125mmol)溶解于10mL的去离子水中,在室温条件下搅拌 1小时。
步骤一中所述的磷钼酸与金属镉盐的摩尔比为:(1~4):1
(2)将上述溶液转移至25mL聚四氟乙烯反应釜中,在200℃下保持24小时,降 温后得到CdS-MoS2双金属复合光催化剂,产物水洗数次,在60℃下干燥24小时。
下面结合附图及实施例,对本发明做进一步的说明:
如图1所示为一种多酸衍生的镉钼双金属六棱柱纳米材料与MoS2(JCPDS CardNo.37-1492)、CdS(JCPDS Card No.47-1179)XRD谱图。一种多钼酸构筑的镍金属硫 化物与MoS2(JCPDS,No.37-1492)、CdS(JCPDS Card No.47-1179)具有良好的匹配 性,具体来说,在2θ为14.1°、33.2°、39.4°和58.6°处的衍射峰分别对应MoS2的(002)、 (100)、(103)以及(110)晶面(JCPDS,No.37-1492)。在24.9°、26.5°、28.2°、36.7°、43.9° 和47.8°以及51.8°处的衍射峰归属于CdS(JCPDS,No.47-1179)的(400)、(033)、(042)、 (530)、(107)和(037)以及(028)晶面。
如图2所示为一种多酸衍生的镉钼双金属六棱柱纳米材料扫描电镜图,从图中可以 明显的观察到复合材料展现出了纳米六棱柱的结构。
如图3所示为一种多酸衍生的镉钼双金属六棱柱纳米材料透射电镜图,显示出了六 棱柱的结构,晶格间距为0.62nm和0.21nm分别归属于MoS2的(002)晶面和CdS的 (107)晶面。
如图4为一种多酸衍生的镉钼双金属六棱柱纳米材料BET测试图,证明材料中存在微孔和介孔,有利于材料和牺牲剂的接触,使光催化性能得到提升。
如图5为一种多酸衍生的镉钼双金属六棱柱纳米材料与Keggin型磷钼酸、硫化镉在 500W氙灯为光源的照射下以硫化钠和无水亚硫酸钠为牺牲剂光催化产氢速率对比图。光催化分解水产氢的体系为产氢最高的催化体系,平均产氢效率为1190μmol g-1h-1,从 而得出本发明的一种多酸衍生的镉钼双金属六棱柱纳米材料是一种高效的光催化分解水 的光催化剂。
如图6为一种多酸衍生的镉钼双金属六棱柱纳米材料在硫化钠和无水亚硫酸钠作为 牺牲试剂下30小时稳定性图。以500W氙灯为光源的照射下进行30小时的5个循 环测试。在循环30小时后光催化活性没有明显的下降,说明其具有非常好的循环稳定性, 证明了制备的一种多酸衍生的镉钼双金属六棱柱纳米材料可以作为非常稳定的光催化产氢的试剂。
Claims (1)
1.一种多酸衍生的镉钼双金属六棱柱纳米材料,其特征在于形貌呈现出层片穿插形成的六棱柱结构,六棱柱中存在孔隙宽度为1.96nm的微孔和2-30nm的介孔,相比于层片MoS2增大了其与牺牲剂的接触面积,并且改善了MoS2易发生团聚导致接触面积减小的问题;其制备方法包括以下步骤:
(1)、称取0.0956mmol H3(PMo12O40)·6H2O,0.625mmol Cd(NO3)2·4H2O和3.125mmol硫脲溶解于10mL的去离子水中,在室温条件下搅拌1小时;
(2)、将上述溶液转移至25mL聚四氟乙烯反应釜中,在200℃下保持24小时,降温后得到CdS-MoS2双金属复合光催化剂,产物水洗数次,在60℃下干燥24小时。
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