碳纤维载镍复合材料的制备及其性能研究

发布时间：2018-05-06 15:02

  本文选题：镍纳米粒子 + 碳纤维　； 参考：《内蒙古工业大学》2015年硕士论文

【摘要】：过渡金属镍基催化剂由于其催化性能和电化学性能优异而得到人们的广泛关注。本论文结合静电纺丝法、浸渍法、掺杂法及高温焙烧技术制备一种新型一维镍基复合纳米材料,并研究了复合材料催化加氢性能和电化学性能,主要的研究内容如下:(1)静电纺丝法制备的复合纳米纤维膜浸泡于硝酸镍溶液中一定时间,通过高温焙烧获得负载镍纳米粒子的碳纤维复合材料。通过傅立叶红外光谱(FTIR)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)、X射线光电子能谱(XPS)等表征手段对所制备的复合纳米纤维进行了一系列表征,结果表明制备的复合纳米纤维形貌规整、纤维表面光滑无节点、镍纳米粒子均匀负载到碳纤维上。复合催化剂应用到催化芳香型硝基加氢制取芳香胺反应中,通过实验参数的考察,确定了最佳实验条件。研究了该材料制作成超级电容器电极材料的电学性能。(2)通过纺丝前驱体溶液中掺入硝酸镍,纺丝后获得含有镍离子的前驱体复合纤维膜,经过预氧化阶段、高温焙烧过程后获得含有镍纳米粒子的碳纤维催化材料。利用该方法可以有效控制复合材料的活性中心含量,对所制备的复合催化材料进行一系列表征测试,结果表明镍纳米粒子均匀分布于碳纤维基体内。考察了不同比例和不同碳化温度制备的催化剂催化芳香型硝基化合物加氢制取芳香胺反应,结果表明碳化温度为600℃、聚丙烯腈单体AN和硝酸镍的摩尔比为10获得的催化剂催化性能最优。电化学测试结果表明内掺硝酸镍的电极材料电化学性能优于纯碳纤维材料。(3)为改善制备所得复合材料的柔软性,纺丝前驱体溶液中掺入一定比例的有机镍盐(乙酰丙酮镍),经过静电纺丝、预氧化、高温焙烧过程后获得Ni NPs/CNFs催化剂。系统研究了复合催化剂应用于催化加氢反应中的催化性能,结果表明:聚丙烯腈单体AN与乙酰丙酮镍的摩尔比为10、碳化温度为600℃、反应时间为6 h、催化剂用量为0.05 g催化反应转化率最高,TEM测试表明平均粒径为8 nm的镍纳米粒子均匀分布于碳纤维载体内。电化学性能测试循环伏安曲线可知当扫描速率为2 m V/s时,比电容达到最大值60 F g-1,且呈现随扫描速率增大电容值逐渐减小的趋势。总之,将镍纳米粒子与碳纤维结合制备的新型材料,有效改善传统催化剂的弊端,为后续的新型催化剂的开发提供新的思路,同时也为纳米镍基材料在催化领域和电化学领域提供一定的理论基础。
[Abstract]:Transition metal nickel-based catalysts have attracted wide attention due to their excellent catalytic and electrochemical properties. In this paper, a novel one dimensional nickel based composite nanomaterials were prepared by electrospinning, impregnation, doping and high temperature roasting. The catalytic hydrogenation and electrochemical properties of the composites were studied. The main research contents are as follows: (1) carbon fiber composite film prepared by electrospinning method was immersed in nickel nitrate solution for a certain time. Carbon fiber composites loaded with nickel nanoparticles were prepared by calcination at high temperature. The composite nanofibers were characterized by Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The surface of the fiber is smooth without nodes, and the nickel nanoparticles are uniformly loaded onto carbon fiber. The composite catalyst was applied to the catalytic hydrogenation of aromatic nitro to aromatic amines. The optimum experimental conditions were determined by the investigation of experimental parameters. The electrical properties of the material made into electrode material of supercapacitor were studied. The composite fiber membrane containing nickel ion was obtained by adding nickel nitrate into the solution of spinning precursor, and the film was preoxidized. Carbon fiber catalytic materials containing nickel nanoparticles were prepared after calcination at high temperature. This method can effectively control the active center content of the composite materials and make a series of characterization tests on the composite catalytic materials. The results show that the nickel nanoparticles are uniformly distributed in the carbon fiber matrix. The catalytic hydrogenation of aromatic nitro compounds to aromatic amines was investigated using catalysts prepared at different ratios and different carbonation temperatures. The results showed that the carbonation temperature was 600 鈩，

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