CN105597780B - 自组装Pd-Cu双金属多枝状纳米晶催化剂及其制备和用途 - Google Patents
自组装Pd-Cu双金属多枝状纳米晶催化剂及其制备和用途 Download PDFInfo
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Abstract
本发明提供了一种自组装Pd‑Cu双金属多枝状纳米晶催化剂及其制备和用途。其制备方法的关键在于：利用异质Cu种诱导Pd种的成核，在保护力较弱的十二烷基苯磺酸钠做保护剂的条件下来调控Pd基纳米晶的形貌。该催化剂是第一例基于扩散限制凝聚形成机理的自组装Pd‑Cu双金属纳米晶。该催化剂展现了对乙醇电催化氧化较高催化活性，以及稳定性。且本方法具有工艺简单，成本低廉，操作方便，应用效果好等特点。
Description
技术领域
本发明属于纳米晶的材料合成领域。具体为对贵金属Pd的形貌控制。
背景技术
该纳米晶的形成机理为扩散限制凝聚(Diffusion-limited Aggregation,DLA)，该模型是由Witten和Sander于1981年共同提出来的，其基本思想是：首先置一初始粒子作为种子，在远离种子的任意位置随机产生一个粒子使其做无规行走，直至与种子接触，成为集团的一部分；然后再随机产生一个粒子，重复上述过程，这样就可以得到足够大的DLA团簇(cluster)。创始人之一Sander曾经总结过DLA的研究意义：
·模型用极其简单的算法抓住了广泛的自然现象的关键成分却没有明确的物理机制；
·.通过简单的运动学和动力学过程就可以产生具有标度不变性的自相似的分形结构，从而建立分形理论和实验观察之间的桥梁，在一定程度上揭示出实际体系中分形生长的机理；
·界面具有复杂的形状和不稳定性的性质，生长过程是一个远离平衡的动力学过程，但集团的结构却有稳定且确定的分形维数。
纳米晶的物化性质强烈的依赖于其形貌和尺寸。纳米晶的合成方法，是现代纳米材料研究领域的基石。基于该理论的Pd-Cu自组装大型团簇是第一例。
发明内容
本发明的目的是制备基于DLA理论的自组装Pd-Cu双金属纳米晶大团簇并研究其乙醇电氧化的催化性能。
所述的催化剂的制备方法，包括如下步骤：
(1)分别配置氯化铜，十二烷基苯磺酸钠，抗坏血酸，溴化钾，含有氯化钯的盐酸水溶液。
(2)将步骤(1)配置的氯化铜，十二烷基苯磺酸钠，抗坏血酸水溶液加入到壁厚耐压瓶中，在油浴锅中搅拌加热制备铜溶胶。
(3)在步骤(2)所制备的Cu溶胶中加入步骤(1)配置的溴化钾水溶液，并加入步骤(1)配置的含有氯化钯的盐酸水溶液制备得到钯铜双金属纳米晶。
所述的催化剂用于乙醇电催化氧化反应。
本发明所制备的Pd-Cu双金属纳米晶是第一例基于DLA理论下的自组装纳米团簇。制备的催化剂具有很好的稳定性以及较高的催化活性。制备条件温和，方法简易，无需特殊的设备，成本比较低廉。本方法具有工艺简单，操作方便，应用范围广等特点。
附图说明
附图1为：以阳离子表面活性剂十二烷基苯磺酸钠为模板的Pd-Cu自组装球示意图。
附图2为：Pd12.1Cu自组装球的透射电镜图表征。
附图3为：时间分辨的透射电镜图表征Pd12.1Cu自组装球的形成机理。
具体实施方式
实施例1：多枝状钯铜双金属纳米晶催化剂Pd12.1Cu的制备方法
首先，将1.7mg二水合氯化铜，87mg十二烷基苯磺酸钠，352.2mg抗坏血酸加入到15ml壁厚耐压瓶中，加水溶解完全，总体积为5mL。接着转移到80℃油浴中加热18h，反应完成后冷却至室温，超声5min至均匀的铜溶胶，加入24mg溴化钾，搅拌5min后转入15℃的恒温水浴中，以0.043L/h的注射速度将5mL 10mmol/L氯钯酸(其中含有44.3mg氯化钯和1.25mmol的盐酸水溶液)加到铜溶胶中。反应2h后，用水与乙醇的混合溶液洗涤3遍，干燥备用。
实施例2：乙醇电催化氧化的反应步骤
电极的制备：在三电极玻璃电解池中进行电化学测试。工作电极是将催化剂在超纯水的分散液滴在玻碳电极(玻碳电极，直径6mm，玻碳面3mm，面积0.07cm2)，自然烘干，滴加0.02％Nafion溶液至催化剂表面，干燥制备而成，铂丝为对电极，参比电极为Ag/AgCl。
电化学性能测试：在N2饱和的1M NaOH溶液中进行循环伏安扫描，扫面速度为50mV·s-1，扫描范围为-0.9～0.5V，待曲线稳定后，计算电化学活性面积。之后在N2饱和的1M EtOH+1M KOH溶液中进行乙醇电氧化性能测试，扫面速度为50mV·s-1，扫描范围为-0.9～0.5V。
电化学稳定性测试：在N2饱和的1M EtOH+1M KOH溶液中，扫描电压恒定在-0.3V，扫描时间为1500s。
Claims (7)
1.一种自组装Pd-Cu双金属多枝状纳米晶催化剂，化学简式为：Pd12.1Cu，其中含92.4％的钯元素，7.6％的铜元素；尺寸为50nm，该催化剂采用种子诱导法，以十二烷基苯磺酸钠作为保护剂制备而成，该催化剂用于乙醇的电氧化反应；催化剂的制备方法包括如下步骤：
(1)分别配置氯化铜，十二烷基苯磺酸钠，抗坏血酸，溴化钾，含有氯化钯的盐酸水溶液；
(2)将步骤(1)配置的氯化铜水溶液，十二烷基苯磺酸钠，抗坏血酸水溶液加入到壁厚耐压瓶中并旋紧旋塞，在油浴锅中搅拌80℃加热，反应18h制备铜溶胶；
(3)在步骤(2)所制备的铜溶胶中加入步骤(1)配置的溴化钾水溶液，转移到15℃的恒温水浴中，并加入步骤(1)配置的氯化钯的盐酸水溶液反应2h制备得到自组装钯铜双金属多枝状纳米晶；
(4)步骤(2)、(3)须按照一定的比例加入各物质的量。
2.一种权利要求1所述的催化剂的制备方法，包括如下步骤：
(1)分别配置氯化铜，十二烷基苯磺酸钠，抗坏血酸，溴化钾，含有氯化钯的盐酸水溶液；
(2)将步骤(1)配置的氯化铜水溶液，十二烷基苯磺酸钠，抗坏血酸水溶液加入到壁厚耐压瓶中并旋紧旋塞，在油浴锅中搅拌80℃加热，反应18h制备铜溶胶；
(3)在步骤(2)所制备的铜溶胶中加入步骤(1)配置的溴化钾水溶液，转移到15℃的恒温水浴中，并加入步骤(1)配置的氯化钯的盐酸水溶液反应2h制备得到自组装钯铜双金属多枝状纳米晶；
(4)步骤(2)、(3)须按照一定的比例加入各物质的量。
3.根据权利要求2所述的方法，其特征在于：所述步骤(1)中氯化铜水溶液的配置，是称取2.13g二水合氯化铜于25mL容量瓶中定容；十二烷基苯磺酸钠溶液的配置，是称取2.178g十二烷基苯磺酸钠于50mL容量瓶中定容；抗坏血酸水溶液的配置，是称取1.76g抗坏血酸在10mL容量瓶中定容；溴化钾溶液的配置，是称取7.5g溴化钾在25ml容量瓶中定容；氯化钯盐酸水溶液的配置，是称取0.0886mg氯化钯与5mL 0.5mol/L盐酸水溶液于50mL容量瓶中定容。
4.根据权利要求2所述的方法，其特征在于：所述步骤(2)中，用移液枪吸取20μL氯化铜溶液，其中含有1.7mg二水合氯化铜；2mL十二烷基苯磺酸钠，其中含有87mg十二烷基苯磺酸钠；2.1mL水；2mL抗坏血酸溶液，其中含有352.2mg抗坏血酸；加入到15mL壁厚耐压瓶中搅拌混匀后，在油浴锅 中80℃加热，反应时间为18h。
5.根据权利要求2所述的方法，其特征在于：所述步骤(3)中在Cu溶胶中加入80μL溴化钾溶液，其中含有溴化钾24mg，转移到15℃的恒温水浴中，并以0.043L/h的速度向Cu溶胶中注射5mL氯化钯的盐酸水溶液，其中含有44.3mg氯化钯，1.25mmol盐酸，反应时间为2h。
6.根据权利要求2所述的方法，其特征在于：所述步骤(4)中所加入的氯化铜，十二烷基苯磺酸钠，抗坏血酸，氯化钯，溴化钾的物质的量比为1:25:200:5:20。
7.权利要求1所述的催化剂在乙醇电催化氧化反应中的应用。
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