CN111167439B - 一种菊花状Pd纳米粒子 - Google Patents
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Abstract
一种菊花状Pd纳米粒子，涉及纳米材料技术领域，所述Pd纳米粒子的整体形状呈菊花状，菊花粒径约为60‑80 nm，比表面积在48.142‑51.601 m2 g‑1之间，所述菊花状Pd纳米粒子由若干个纳米片状花瓣组成，花瓣之间存在大量的空隙或孔道。本发明有益效果：本发明的菊花状Pd纳米粒子形貌均一，具有多孔自支撑结构，比表面积大，稳定性能好。
Description
技术领域
本发明属于纳米材料技术领域，具体涉及一种菊花状Pd纳米粒子。
背景技术
贵金属纳米粒子具有特殊的物理和化学性质，在催化领域具有极高的应用价值。其中，Pd纳米粒子在加氢、偶联和电化学等领域均显示出优异的催化性能。
目前，通过各种各样的方法，已经成功制备出不同形貌的Pd纳米粒子。例如，Zheng等以乙酰丙酮钯（Pd(acac)2）为前驱体，在DMF或苯甲醇溶解中，PVP和CTAB存在下，CO冲压1bar的情况下，100 ℃反应3 h制备出六边形Pd纳米片（Nature Nanotechnology, 2011, 6,28-32.）。Yu等以PdCl2为前驱体，在油胺和油酸混合溶剂中，高温160 ℃条件下制备出Pd纳米树枝（Nanoscale, 2013, 5, 3202-3207）。蒋等以Na2PdCl4为前驱物，N,N-二甲基十八胺和溴代乙酸钠的调节下，在不同的pH条件下，从水溶液中分别制备出Pd纳米立方、凹面的Pd纳米立方和Pd纳米海葵状结构（无机化学学报, 2017, 33, 1835-1842）。Tang等以K2PdCl4为原料，在聚二烯丙基二甲基氯化铵（PDDA）和甲醛的存在调控下，120 ℃水热合成了多孔Pd纳米片（Advanced Functional Materials, 2017, 27, 1603852.）。Wang等在含有H2PdCl4和甲醛的水溶液表面，加入少量含有油胺的氯仿溶液，60 ℃条件下反应130 min，从水溶液表面获得类立方结构的Pd纳米片（Chemistry of Materials, 2018, 30, 3308-3314.）。Yamauchi等以Na2PdCl4为前驱物，在氯化十六烷基吡啶（HDPC）和聚合物F127的共同调控下，从水溶液中制备出具有介孔的球形Pd纳米粒子（Chemical Communications,2014, 50, 11753-11756.）最近，他们又以H2PdCl4为前驱体，在四氢呋喃（THF）和水的混合溶剂中，在聚合物PS-b-PEO的调控下制备出孔径可调的介孔Pd球形纳米粒子（ChemicalScience, 2019, 10, 4054-4061.），等等。尽管目前为止，具有多种形貌的Pd纳米结构已经被成功的合成。然而，据我们所知，具有菊花状这种特殊结构的Pd纳米粒子仍然没有被合成出来。
发明内容
针对以上问题，本发明提供一种菊花状Pd纳米粒子，这种多孔自支撑结构，不仅具有较大的比表面积和较高的催化活性，而且使用过程中不易熔接团聚，具有长期的稳定性。
本发明为解决上述技术问题所采用的技术方案是：一种菊花状Pd纳米粒子，所述Pd纳米粒子的整体形状呈菊花状，菊花粒径为60-80 nm，比表面积在48.142-51.601 m2 g-1之间，所述菊花状Pd纳米粒子由若干个纳米片状花瓣组成，花瓣之间存在大量的空隙或孔道。
本发明所述纳米片状花瓣的个数为40-50个，每个纳米片状花瓣长20-40 nm，厚5nm，纳米片状花瓣头部宽度为10-15 nm。
本发明所述空隙或孔道以孔径为4.0 nm的介孔为主。
本发明的有益效果是：本发明提供了一种菊花状Pd纳米粒子，其形貌均一，具有多孔自支撑结构，比表面积大，稳定性能好。这种菊花状结构Pd纳米粒子由大量的花瓣组成，花瓣之间具有丰富的孔道，这种开放的孔道结构不仅使其具有较高的比表面积、大量的活性位点，还便利了试剂分子、中间物种和产物的进入和转出，再加上其洁净的表面使其具有优异的催化性能。而且，其具有自支撑结构的特点，在催化过程中不需要载体的使用，也不易团聚、熔接和溶解，因而具有较高的稳定性。作为催化剂，有望在催化加氢、脱氢、Suzuki、偶联反应以及电催化等领域得到广泛应用。
附图说明
图1为本发明低放大倍数菊花状Pd纳米粒子的TEM图；
图2为本发明高放大倍数菊花状Pd纳米粒子的TEM图；
图3为本发明菊花状Pd纳米粒子的HRTEM图；
图4为Pd纳米菊花的N2吸附脱附等温曲线图；
图5为Pd纳米菊花的孔径分布图。
具体实施方式
下面结合实施例对本发明的具体实施方式（实施例）进行描述，使本领域的技术人员能够更好地理解本发明。
一种菊花状Pd纳米粒子，所述Pd纳米粒子的整体形状呈菊花状，菊花粒径约为60-80 nm，比表面积为48.142 m2 g-1-51.601 m2 g-1，所述菊花状Pd纳米粒子由若干个纳米片状花瓣组成，花瓣之间存在大量的空隙或孔道。
进一步地，所述纳米片状花瓣的个数为40-50个，每个纳米片状花瓣长约20-40nm，厚约5 nm，纳米片状花瓣头部宽度为10-15 nm。
进一步地，所述空隙或孔道以孔径为4.0 nm的介孔为主。
本发明所述菊花状Pd纳米粒子的一种制备方法，包括如下步骤：
（1）将氯化1-十四烷基-3-基咪唑溶于去离子水中得到摩尔浓度为0.5 mol/L的氯化1-十四烷基-3-甲基咪唑离子液体，氯化1-十四烷基-3-基咪唑离子液体在反应介质溶液中的浓度为25-100 mmol/L；
（2）向步骤（1）中得到的氯化1-十四烷基-3-甲基咪唑离子液体加入Pd前驱体溶液，混合均匀， Pd前驱体为四氯钯酸钠；
（3）向步骤（2）得到的混合液中加入还原剂维生素C进行反应，维生素C溶液的浓度为100-200 mmol/L，反应环境为30-80 ℃水浴环境，反应时间为6-12 h；
（4）将步骤（3）反应后所得的产物经过离心、干燥即得菊花状Pd纳米粒子。
本发明的菊花状Pd纳米粒子形貌均一，具有多孔自支撑结构，比表面积大，稳定性能好。从说明书附图图1和图2可以看出，这种菊花状结构Pd纳米粒子由大量的花瓣组成，花瓣之间具有丰富的孔道。这种开放的孔道结构不仅使其具有较高的比表面积、大量的活性位点，还便利了试剂分子、中间物种和产物的进入和转出。再加上其洁净的表面使其具有优异的催化性能。而且，其还具有自支撑结构的特点，在催化过程中不需要载体的使用，也不易团聚、熔接和溶解，因而具有较高的稳定性。有望在催化加氢、脱氢、Suzuki、偶联反应以及电催化等领域得到广泛应用。在催化甲酸分解产氢实验中，在30 ℃，其转换频率(TOF)高达1411 h-1，且没有副产物CO的生成，表现出优异的催化活性和选择性。其催化活性明显优于中国专利CN110327966A制备的负载型Pd/ZrO2催化剂(TOF为1243 h-1)和中国专利CN109453762A制备的改性黏土矿负载的Pd催化剂(TOF最高为888 h-1)。
实施例1
一种菊花状Pd纳米粒子，所述Pd纳米粒子的整体形状呈菊花状，菊花粒径约为60nm，比表面积为48.142 m2 g-1，所述菊花状Pd纳米粒子由若干个纳米片状花瓣组成，花瓣之间存在大量的空隙或孔道，所述纳米片状花瓣的个数为40个，每个纳米片状花瓣长约20nm，厚约5 nm，纳米片状花瓣头部宽度为10 nm，所述空隙或孔道以孔径为4.0 nm的介孔为主。
实施例2
一种菊花状Pd纳米粒子，所述Pd纳米粒子的整体形状呈菊花状，菊花粒径约为80nm，比表面积为51.601 m2 g-1，所述菊花状Pd纳米粒子由若干个纳米片状花瓣组成，花瓣之间存在大量的空隙或孔道，所述纳米片状花瓣的个数为50个，每个纳米片状花瓣长约40nm，厚约5 nm，纳米片状花瓣头部宽度为15 nm，所述空隙或孔道以孔径为4.0 nm的介孔为主。
实施例3
一种菊花状Pd纳米粒子，所述Pd纳米粒子的整体形状呈菊花状，菊花粒径约为70nm，比表面积为50 m2 g-1，所述菊花状Pd纳米粒子由若干个纳米片状花瓣组成，花瓣之间存在大量的空隙或孔道，所述纳米片状花瓣的个数为45个，每个纳米片状花瓣长约30 nm，厚约5 nm，纳米片状花瓣头部宽度为13nm，所述空隙或孔道以孔径为4.0 nm的介孔为主。
Claims (3)
1.一种菊花状Pd纳米粒子，其特征在于：所述Pd纳米粒子的整体形状呈菊花状，菊花粒径为60-80 nm，比表面积为48.142 m2 g-1-51.601 m2 g-1，所述菊花状Pd纳米粒子由若干个纳米片状花瓣组成，花瓣之间存在大量的空隙或孔道；
所述菊花状Pd纳米粒子的制备方法，包括如下步骤：
（1）将氯化1-十四烷基-3-甲基咪唑溶于去离子水中得到摩尔浓度为0.5 mol/L的氯化1-十四烷基-3-甲基咪唑离子液体，氯化1-十四烷基-3-甲基咪唑离子液体在反应介质溶液中的浓度为25-100 mmol/L；
（2）向步骤（1）中得到的氯化1-十四烷基-3-甲基咪唑离子液体加入Pd前驱体溶液，混合均匀， Pd前驱体为四氯钯酸钠；
（3）向步骤（2）得到的混合液中加入还原剂维生素C进行反应，维生素C溶液的浓度为100-200 mmol/L，反应环境为30-80 ℃水浴环境，反应时间为6-12 h；
（4）将步骤（3）反应后所得的产物经过离心、干燥即得菊花状Pd纳米粒子。
2.根据权利要求1所述的一种菊花状Pd纳米粒子，其特征在于：所述纳米片状花瓣的个数为40-50个，每个纳米片状花瓣长20-40 nm，厚5 nm，纳米片状花瓣头部宽度为10-15 nm。
3.根据权利要求1所述的一种菊花状Pd纳米粒子，其特征在于：所述空隙或孔道以孔径为4.0 nm的介孔为主。
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