CN114789052A - 一种一锅法制备RuIr(Pt，Pd，Rh)空心胶体球电催化剂的方法 - Google Patents
一种一锅法制备RuIr(Pt，Pd，Rh)空心胶体球电催化剂的方法 Download PDFInfo
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- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
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Abstract
本发明涉及RuIr(Pt，Pd，Rh)空心胶体球电催化剂及其制备方法，属于新型纳米催化材料制备领域。本发明所用材料合成方法为气/液界面自组装法。具体步骤如下：首先将聚乙烯吡咯烷酮和三水合氯化钌和三氯化铱(氯铂酸钾、氯亚钯酸钾、三氯化铑)溶解到乙二醇中，在溶液中加入甲醛溶液，充分混合后，将溶液转移聚四氟乙烯内衬的高压反应釜中，并将其放入恒温鼓风干燥箱中加热反应。将所得产物离心、洗涤和干燥后得到黑色粉末状固体即为所述RuIr(Pt，Pd，Rh)空心胶体球电催化剂。本发明制备方法简便易行，合成的催化材料性能稳定，实验条件绿色环保，实验条件温和适合大规模生产。
Description
技术领域
本发明涉及一种一锅法制备RuIr(Pt，Pd，Rh)空心胶体球电催化剂的方法，属于新型功能材料技术领域。
背景技术
随着世界经济急速发展和人口的不断增多，能源在人类生存发展过程中扮演着越来越重要的角色。但由于化石燃料的过度使用，以及燃烧化石燃料产生的二氧化碳、二氧化硫等污染物，使得能源危机和环境问题越来越突出。因此，降低煤炭、石油等燃料的使用比率，研究清洁、无污染的替代能源在现代社会尤为重要。氢气能源由于其能量密度高、燃烧热值高以及燃烧产物仅为水的特点，被公认为是最具有发展潜力的能源载体。目前，最有潜力的氢能绿色生产和利用的技术是电解水和燃料电池，其相关的反应均涉及多电子转移过程，迫切需要相应的电催化剂以提高其反应动力学。
胶体球是指由单分散胶体颗粒为结构单元，通过自组装的形式构筑成的纳米材料，具有典型的三维中空超结构，其外壳由紧密排列的胶体颗粒构成，有利于反应物在内部孔隙以及中空内核中的传质，因而具有巨大的气体吸附和催化潜力(Guan B Y, Yu L, LouX W. Chemically assisted formation of monolayer colloidosomes on functionalparticles[J]. Advanced Materials, 2016, 28(43): 9596-9601.)。然而，自组装胶体球的制备往往面临各种困难，如：制备方法复杂、产物不稳定等，限制了其在催化方向的发展。
Ru具有与铂相似电子特性，并且拥有与Ni类似的亲氧性，且其成本仅为Pt的五分之一，为电催化反应效率提升提供了独特的解决方案(Zhou Y, Xie Z, Jiang J, et al.Lattice-confined Ru clusters with high CO tolerance and activity for thehydrogen oxidation reaction[J]. Nature Catalysis, 2020, 3(5): 454-462.)。目前，Ru基Pt族合金作为解决各类电催化反应动力学缓慢问题的潜力材料，受到了研究人员的关注。通过Ru与Ir、Pt、Pd、Rh等Pt族金属进行合金化，调控其协同电子结构，可以获得针对不同电催化反应的优秀纳米材料。
然而，结合二者在催化方面的优势，将RuIr(Pt，Pd，Rh)合金纳米晶体作为组装单元，自组装为三维中空胶体球的方法还未见报道。
本发明通过一锅法，将粒径在2 nm以下的RuIr(Pt，Pd，Rh)合金纳米晶体作为组装单元，通过气/液界面自组装的方法，制备了RuIr(Pt，Pd，Rh)空心胶体球电催化剂。首次通过气/液界面自组装的方法，在一次反应中即可制备由RuIr(Pt，Pd，Rh)合金纳米晶体自组装的RuIr(Pt，Pd，Rh)空心胶体球，该电催化剂具备空心胶体球典型的三维中空超结构，可为催化反应提供三相反应界面，同时具备Ru基Pt族材料在电催化反应中的本征催化优势，拓展了自组装纳米材料在电催化方向的发展前景。
发明内容
针对现有技术的上述不足之处，本发明提供了一种一锅法制备RuIr(Pt，Pd，Rh)空心胶体球电催化剂的方法，采用气/液界面自组装法即可一锅反应制备尺寸均一，形貌规整的RuIr(Pt，Pd，Rh)空心胶体球电催化剂。其制备工艺简单、快速高效、成本低廉，适合大规模工业化生产。
本发明的目的是通过以下技术方案实现的：
1）按一定摩尔比分别称取聚乙烯吡咯烷酮(~360000)、三水合氯化钌和三氯化铱(氯铂酸钾、氯亚钯酸钾、三氯化铑)于烧杯中；
2）向步骤1）所用烧杯中加入乙二醇，并超声以促进聚乙烯吡咯烷酮(~360000)、三水合氯化钌和三氯化铱(氯铂酸钾、氯亚钯酸钾、三氯化铑)溶解到乙二醇中以形成棕色均质溶液；
3）向步骤2）烧杯中加入甲醛溶液并搅拌使其与原溶液互溶；
4）将步骤3）所得混合溶液转移至聚四氟乙烯内衬的高压反应釜中，将反应釜置于200 oC恒温鼓风干燥箱中反应2h；
5）将步骤4）所得反应混合物离心分离，并用乙醇洗涤3-4次，然后在60 oC下真空干燥后即得到最终产物。
本发明的有益效果：
（1）本发明提供了一种一锅法制备RuIr(Pt，Pd，Rh)空心胶体球电催化剂的方法，制备方法简单易操作，不需要特殊的设备，成本低廉且适于大规模制备，仅需一次反应即可制备RuIr(Pt，Pd，Rh)空心胶体球电催化剂，可以满足实际应用的需求；
（2）本发明制备的RuIr(Pt，Pd，Rh)空心胶体球电催化剂制备速度快，产物纯度高，提高了制备效率；
（3）本发明制备的RuIr(Pt，Pd，Rh)空心胶体球电催化剂对电催化反应具有良好的催化效果；
（4）本发明方法简便易行，不需要专用设备。
附图说明
图1为RuIr空心胶体球电催化剂TEM图像；
图2为RuPt空心胶体球电催化剂TEM图像；
图3为RuPd空心胶体球电催化剂TEM图像；
图4为RuRh空心胶体球电催化剂TEM图像。
具体实施方式
下面通过具体实施实例并结合附图对本发明的内容作进一步详细说明，但这些实施例并不限制本发明的保护范围。
实施例1
首先分别称取0.9 mmol聚乙烯吡咯烷酮(~360000)、0.045 mmol三水合氯化钌和0.015 mmol三氯化铱溶解到6 mL乙二醇中，在混合溶液中加入1.5 mL甲醛溶液使其互溶，形成棕色溶液，将溶液转移至聚四氟乙烯内衬的高压反应釜中，放入200 oC恒温鼓风干燥箱中反应2小时，然后离心分离，用乙醇超声清洗3-4次后在60oC真空干燥下烘干，制得RuIr合金空心胶体球电催化剂。
实施例2
首先分别称取0.9 mmol聚乙烯吡咯烷酮(~360000)、0.045 mmol三水合氯化钌和0.015 mmol氯铂酸钾溶解到6 mL乙二醇中，在混合溶液中加入1.5 mL甲醛溶液使其互溶，形成棕色溶液，将溶液转移至聚四氟乙烯内衬的高压反应釜中，放入200 oC恒温鼓风干燥箱中反应2小时，然后离心分离，用乙醇超声清洗3-4次后在60oC真空干燥下烘干，制得RuPt合金空心胶体球电催化剂。
实施例3
首先分别称取0.9 mmol聚乙烯吡咯烷酮(~360000)、0.045 mmol三水合氯化钌和0.015 mmol氯亚钯酸钾溶解到6 mL乙二醇中，在混合溶液中加入1.5 mL甲醛溶液使其互溶，形成棕色溶液，将溶液转移至聚四氟乙烯内衬的高压反应釜中，放入200 oC恒温鼓风干燥箱中反应2小时，然后离心分离，用乙醇超声清洗3-4次后在60oC真空干燥下烘干，制得RuPd合金空心胶体球电催化剂。
实施例4
首先分别称取0.9 mmol聚乙烯吡咯烷酮(~360000)、0.045 mmol三水合氯化钌和0.015 mmol三氯化铑溶解到6 mL乙二醇中，在混合溶液中加入1.5 mL甲醛溶液使其互溶，形成棕色溶液，将溶液转移至聚四氟乙烯内衬的高压反应釜中，放入200 oC恒温鼓风干燥箱中反应2小时，然后离心分离，用乙醇超声清洗3-4次后在60oC真空干燥下烘干，制得RuRh合金空心胶体球电催化剂。
Claims (4)
1.一种RuIr(Pt，Pd，Rh)空心胶体球电催化剂，所述纳米粒子为由粒径小于2纳米的RuIr/RuPt/RuPd/RuRh合金纳米晶体作为组装单元，自组装形成的空心结构的微球，粒径为230-370 nm。
2.一种RuIr(Pt，Pd，Rh)空心胶体球电催化剂的制备方法，其特征在于制备方法的步骤如下：
1）称取一定摩尔比的聚乙烯吡咯烷酮(~360000)、三水合氯化钌和三氯化铱(氯铂酸钾、氯亚钯酸钾、三氯化铑)溶解到乙二醇中；
2）将甲醛溶液加入到上述步骤1）所得溶液中，混合后转移到聚四氟乙烯内衬的高压反应釜中，在恒温鼓风干燥箱中进行加热反应；
3）离心并洗涤干燥得到黑色粉末状产品。
3.根据权利要求2所述的钌空心胶体球电催化剂，其特征在于，所用溶剂为乙二醇，气/液界面自组装的气囊模板为甲醛。
4.根据权利要求2所述的RuIr(Pt，Pd，Rh)空心胶体球电催化剂的制备方法，其特征在于，步骤2）所述反应温度区间为180-220 oC，反应时间为2到12小时。
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