CN110202127A - 亚10纳米孪晶二十面体PdCuPt纳米合金的合成方法及应用 - Google Patents
亚10纳米孪晶二十面体PdCuPt纳米合金的合成方法及应用 Download PDFInfo
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- 238000010189 synthetic method Methods 0.000 title claims abstract description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910052751 metal Inorganic materials 0.000 claims abstract description 21
- 239000002184 metal Substances 0.000 claims abstract description 21
- 239000002243 precursor Substances 0.000 claims abstract description 17
- 239000011259 mixed solution Substances 0.000 claims abstract description 15
- 150000002940 palladium Chemical class 0.000 claims abstract description 15
- 150000003057 platinum Chemical class 0.000 claims abstract description 15
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 13
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 claims abstract description 9
- YASYEJJMZJALEJ-UHFFFAOYSA-N Citric acid monohydrate Chemical compound O.OC(=O)CC(O)(C(O)=O)CC(O)=O YASYEJJMZJALEJ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 125000005211 alkyl trimethyl ammonium group Chemical group 0.000 claims abstract description 9
- 229960002303 citric acid monohydrate Drugs 0.000 claims abstract description 9
- 239000002904 solvent Substances 0.000 claims abstract description 7
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 20
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims description 12
- 238000006722 reduction reaction Methods 0.000 claims description 8
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 3
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- 238000004176 ammonification Methods 0.000 claims description 2
- 150000001879 copper Chemical class 0.000 claims description 2
- JKDRQYIYVJVOPF-FDGPNNRMSA-L palladium(ii) acetylacetonate Chemical compound [Pd+2].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O JKDRQYIYVJVOPF-FDGPNNRMSA-L 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
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- 239000010949 copper Substances 0.000 claims 1
- 238000002604 ultrasonography Methods 0.000 claims 1
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- 229910021529 ammonia Inorganic materials 0.000 abstract description 13
- -1 mantoquita Chemical class 0.000 abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 6
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- 238000003786 synthesis reaction Methods 0.000 abstract description 5
- 238000006555 catalytic reaction Methods 0.000 abstract description 4
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- 238000000034 method Methods 0.000 description 7
- 239000011943 nanocatalyst Substances 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 4
- 238000005265 energy consumption Methods 0.000 description 3
- 239000002159 nanocrystal Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
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- 230000009286 beneficial effect Effects 0.000 description 1
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- QNZRVYCYEMYQMD-UHFFFAOYSA-N copper;pentane-2,4-dione Chemical compound [Cu].CC(=O)CC(C)=O QNZRVYCYEMYQMD-UHFFFAOYSA-N 0.000 description 1
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- 239000010948 rhodium Substances 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000010944 silver (metal) Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
本发明公开了亚10纳米孪晶二十面体PdCuPt纳米合金的合成方法及应用，其特征在于：（1）将金属前驱体钯盐、铜盐、铂盐与十烷基三甲基溴化铵和二水合柠檬酸三钠加入到有机溶剂DMF和油胺的混合溶剂中，室温搅拌20~40分钟，直至混合溶液均匀。（2）将步骤（1）所得混合溶液转移到高压反应釜中反应9~24小时，温度保持在160~190℃。（3）将步骤（2）反应得到的产物自然冷却后进行洗涤，离心分离出亚10纳米孪晶二十面体PdCuPt纳米合金，并将其分散在乙醇溶剂中保存。（3）亚10纳米孪晶二十面体PdCuPt纳米合金可用于电催化还原氮合成氨。
Description
技术领域
本发明涉及亚10纳米孪晶二十面体PdCuPt纳米合金的合成方法及在氮还原反应中的应用。
背景技术
氨是世界上产量最大的化工产品之一，在全球经济中占有重要的地位，传统的合成氨工艺是在高温高压条件下利用铁基催化剂将高纯度的氮气和氢气转化为氨，这种方法耗能高，污染严重，因此，寻找一种绿色环保、低能耗的合成氨方法对国民经济的可持续发展具有重要的意义，电催化还原氮气可实现氨的常温常压合成。孪晶纳米晶体是一种独特的纳米结构，到目前一元的孪晶纳米晶体 Fe、Ag、Au、Pd、Pt、Rh、Ru 和二元的孪晶纳米晶体PdNi、PdPt、PtNi、PtCu等已有相关报道，而三元10纳米以下的孪晶二十面体纳米合金尚未有文献报道。
发明内容
本发明要解决的技术问题是：获得一系列亚10纳米孪晶二十面体PdCuPt纳米合金，该种合成方法简单，产物形貌统一，尺寸和成分可控，在常温常压对氮气还原成氨具有优异的电催化性能。
本发明的技术方案是：亚10纳米孪晶二十面体PdCuPt纳米合金的合成方法及应用，（1）将金属前驱体钯盐、铜盐和铂盐与十烷基三甲基溴化铵及二水合柠檬酸三钠加入到二甲基甲酰胺和油胺的混合溶剂中，其中金属前驱体钯盐、铜盐和铂盐的金属摩尔比为4:1:1-1:4:1，投入量控制在0.025mmol ~ 0.1mmol，室温搅拌10~40分钟，直至混合溶液搅拌均匀；（2）将步骤（1）所得混合溶液转移到高压反应釜中反应9~24小时，温度保持在160~190℃;（3）将步骤（2）反应得到的产物自然冷却到室温后进行洗涤，离心分离出亚10纳米孪晶二十面体PdCuPt纳米合金，并将其分散在乙醇溶剂中保存。
步骤(1)中所述的金属钯盐前驱体为乙酰丙酮钯；金属铜盐前驱体为乙酰丙酮铜；金属铂盐前驱体为乙酰丙酮铂；十烷基三甲基溴化铵及二水合柠檬酸三钠的质量均控制在80~140 mg，有机溶液二甲基甲酰胺和油胺的比例为2:1~1:2。
步骤（2）中所述的高压反应釜中温度保持在160~190℃，反应时间为9~24小时。
所述的亚10纳米孪晶二十面体PdCuPt纳米合金在常温常压下可用于氮还原合成氨。
本发明的有益效果：（1）由该方法可以控制合成亚10纳米孪晶二十面体PdCuPt纳米合金产物形貌。（2）该催化剂的形貌是现有所记载的三元合金PdCuPt文献中新颖的形貌，具有优异的氮电催化活性。用这种催化剂去催化氮气还原为氨是一种绿色环保、低能耗的合成氨方法。
本发明使用液相法成功合成了亚10纳米PdCuPt三元孪晶二十面体纳米合金。并且可以对其尺寸和成分加以调控。所合成的亚10纳米孪晶二十面体PdCuPt纳米合金在电催化合成氨中表现出高的产氨速率和选择性。
附图说明
图1为亚10纳米孪晶二十面体PdCuPt合金纳米催化剂透射电子显微镜观察结果图和高分辨率透射电子显微镜图；
图2为亚10纳米孪晶二十面体PdCuPt合金纳米催化剂X射线衍射结果图；
图3为亚10纳米孪晶二十面体PdCuPt合金纳米在常温常压下催化剂氮气还原为氨的产氨速率和法拉第效率图。
具体实施方式
实施例1：
（1）将金属前驱体钯盐、铜盐、铂盐与十烷基三甲基溴化铵和二水合柠檬酸三钠加入到有机溶剂二甲基甲酰胺和油胺的混合溶剂中，其中金属前驱体钯盐、铜盐、铂盐的金属摩尔比为3:2:1，室温搅拌30分钟，直至混合溶液均匀；
（2）将步骤（1）所得混合溶液转移到高压反应釜中反应24小时，温度保持在180℃；
（3）将步骤（2）反应得到的产物自然冷却后进行洗涤，离心分离出亚10纳米孪晶二十面体PdCuPt纳米合金，并将其分散在乙醇溶剂中保存。
实施例2：
亚10纳米孪晶二十面体PdCuPt合金纳米催化剂的合成方法及在常温常压下氮还原中的应用，（1）将金属前驱体钯盐、铜盐、铂盐与十烷基三甲基溴化铵和二水合柠檬酸三钠加入到有机溶剂DMF和油胺的混合溶剂中，其中金属前驱体钯盐、铜盐、铂盐的金属摩尔比为2:3:1，室温搅拌30分钟，直至混合溶液均匀；
（2）将步骤（1）所得混合溶液转移到高压反应釜中反应18小时，温度保持在180℃；
（3）将步骤（2）反应得到的产物自然冷却后进行洗涤，离心分离出亚10纳米孪晶二十面体PdCuPt合金纳米催化剂，并将其分散在乙醇溶剂中保存。
实施例3：
亚10纳米孪晶二十面体PdCuPt合金纳米催化剂的合成方法及在常温常压下氮还原中的应用，（1）将金属前驱体钯盐、铜盐、铂盐与十烷基三甲基溴化铵和二水合柠檬酸三钠加入到有机溶剂二甲基甲酰胺和油胺的混合溶剂中，其中金属前驱体钯盐、铜盐、铂盐的金属摩尔比为4:1:1，室温搅拌30分钟，直至混合溶液均匀；
（2）将步骤（1）所得混合溶液转移到高压反应釜中反应12小时，温度保持在180℃；
（3）将步骤（2）反应得到的产物自然冷却后进行洗涤，离心分离出亚10纳米孪晶二十面体PdCuPt纳米合金，并将其分散在乙醇溶剂中保存。
实施例4：
亚10纳米孪晶二十面体PdCuPt合金纳米催化剂的合成方法及在常温常压下氮还原中的应用，（1）将金属前驱体钯盐、铜盐、铂盐与十烷基三甲基溴化铵和二水合柠檬酸三钠加入到有机溶剂DMF和油胺的混合溶剂中，其中金属前驱体钯盐、铜盐、铂盐的金属摩尔比为1:4:1，室温搅拌20分钟，直至混合溶液均匀；
（2）将步骤（1）所得混合溶液转移到高压反应釜中反应24小时，温度保持在180℃；
（3）将步骤（2）反应得到的产物自然冷却后进行洗涤，离心分离出亚10纳米孪晶二十面体PdCuPt纳米合金纳米，并将其分散在乙醇溶剂中保存。
Claims (7)
1.亚10纳米孪晶二十面体PdCuPt纳米合金的合成方法，其特征在于：(1)将金属前驱体钯盐、铜盐和铂盐与十烷基三甲基溴化铵、二水合柠檬酸三钠加入到二甲基甲酰胺和油胺的混合溶液中，室温10～40分钟，直至混合溶液搅拌超声均匀；(2)将步骤(1)所得混合溶液转移到高压反应釜中反应9～24小；(3)将步骤(2)反应得到的产物自然冷却到室温后进行洗涤，离心分离出亚10纳米孪晶二十面体PdCuPt纳米合金纳。
2.根据权利要求1所述的一种亚10纳米孪晶二十面体PdCuPt纳米合金的合成方法，其特征在于：步骤(1)中所述的金属钯盐前驱体为乙酰丙酮钯；金属铜盐前驱体为乙酰丙酮铜；金属铂盐前驱体为乙酰丙酮铂。
3.根据权利要求1所述的亚10纳米孪晶二十面体PdCuPt纳米合金的合成方法，其特征在于：所述的钯盐前驱体、铜盐前驱体和铂盐前躯体的摩尔比为4:1:1-1:4:1。
4.根据权利要求1所述的亚10纳米孪晶二十面体PdCuPt纳米合金的合成方法，其特征在于：所述的十烷基三甲基溴化铵和二水合柠檬酸三钠的用量均控制在80～140mg。
5.根据权利要求1所述的亚10纳米孪晶二十面体PdCuPt纳米合金的合成方法，其特征在于：所述的溶剂二甲基甲酰胺和油胺的体积比为2:1～1:2。
6.根据权利要求1所述的亚10纳米孪晶二十面体PdCuPt纳米合金的合成方法，其特征在于：步骤(2)中所述的高压反应釜中温度保持在160～190℃，反应时间为9～24小时。
7.如权利要求书1-6之一亚10纳米孪晶二十面体PdCuPt纳米合金用于氮气还原反应生成氨。
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