摘要Pd作为一种优良的催化剂,可以催化众多有机反应。将Pd负载在SiO2上可以提高Pd的稳定性,减少在催化过程中的损失,并且纳米级SiO2粒子具有较大的比表面积,可以吸附反应底物产生富集效果,提高催化反应效率。本实验通过正硅酸甲酯的溶胶凝胶反应在反相细乳液中形成纳米SiO2粒子,随后伴随着水合联氨的气体扩散过程原位还原Pd盐,制备得到具有Janus形态的Pd/SiO2纳米复合粒子。通过X射线衍射,可以测得Pd纳米粒子的晶体结构。通过形态研究证实合成的Pd/SiO2纳米复合粒子具有Janus结构。氮气吸附结果显示Pd/SiO2纳米复合粒子具有介孔结构。通过改变K2PdCl4的用量可以有效的调节纳米催化粒子中Pd纳米粒子的大小和含量。Janus形的Pd/SiO2纳米复合粒子在对硝基苯酚与NaBH4的还原反应中表现出了优良的催化活性。47766
Abstract As a kind of excellent catalysts, Pd can catalyze various organic reactions. Pd loads on the surface of SiO2 which will improve its stability and reduces the loss in the process of catalyze. On the other hand, the large specific surface area of SiO2 nanoparticles will adsorb reactant and improve the efficiency of catalytic reaction.
Our experiment preparation the Janus Pd/SiO2 nanocomposite particles (NCPs) through a combination of the sol–gel process of tetramethoxysilane in inverse miniemulsions and in situ reduction of Pd salts via a gas diffusion process of hydrazine. The formation of Pd nanoparticles (NPs) was verified by X-ray diffraction. The Janus morphology of the Pd/SiO2 NCPs was confirmed by microscopic observation. The Pd/SiO2 NCPs displayed a mesoporous structure. The content of Pd NPs in the NCPs could be conveniently adjusted by the K2PdCl4 loading. The mesoporous Janus Pd/SiO2 NCPs show a good catalytic activity towards the reduction of p-nitrophenol with NaBH4.
毕业论文关键词:Pd; SiO2; 催化剂; 反相细乳液
Key words: Pd; SiO2; Catalyst; Inverse Miniemulsion
1.引言 4
2.实验部分 5
2.1实验材料与设备 5
2.1.1实验材料 5
2.1.2实验设备 5
电感耦合等离子发射光谱仪 6
2.2合成纳米催化剂过程 6
2.2.1合成Pd盐/SiO2粒子 6
2.2.2形成Janus结构的Pd/SiO2纳米复合粒子 7
2.2.3热处理 7
2.3 对硝基苯酚催化 7
2.4 性能表征 7
2.4.1 透射电镜(TEM) 8
2.4.2 场发射扫描电镜(FESEM) 8
2.4.3 动态散射粒径测试(DLS) 8
2.4.4 氮气吸附分析 8
2.4.5热重分析(TGA) 8
2.4.6傅里叶变换红外测试(FT-IR) 8
2.4.7 X射线衍射分析(XRD) 8
2.4.电感耦合等离子体质谱法(ICP-MS) 9
3. 结果与讨论 9
3.1 Janus形态的Pd/SiO2纳米复合粒子的合成及其性能 9
3.2 调整Pd/SiO2纳米复合粒子的Pd含量 14
3.3 Janus形态的Pd/SiO2纳米复合粒子的形成机理 15 Pd/SiO2纳米复合粒子的制备及其催化性能研究:http://www.youerw.com/huaxue/lunwen_49972.html