碳纖維載鎳復合材料的制備及其性能研究
發(fā)布時間:2018-05-06 15:02
本文選題:鎳納米粒子 + 碳纖維 ; 參考:《內(nèi)蒙古工業(yè)大學》2015年碩士論文
【摘要】:過渡金屬鎳基催化劑由于其催化性能和電化學性能優(yōu)異而得到人們的廣泛關(guān)注。本論文結(jié)合靜電紡絲法、浸漬法、摻雜法及高溫焙燒技術(shù)制備一種新型一維鎳基復合納米材料,并研究了復合材料催化加氫性能和電化學性能,主要的研究內(nèi)容如下:(1)靜電紡絲法制備的復合納米纖維膜浸泡于硝酸鎳溶液中一定時間,通過高溫焙燒獲得負載鎳納米粒子的碳纖維復合材料。通過傅立葉紅外光譜(FTIR)、掃描電子顯微鏡(SEM)、透射電子顯微鏡(TEM)、X射線光電子能譜(XPS)等表征手段對所制備的復合納米纖維進行了一系列表征,結(jié)果表明制備的復合納米纖維形貌規(guī)整、纖維表面光滑無節(jié)點、鎳納米粒子均勻負載到碳纖維上。復合催化劑應(yīng)用到催化芳香型硝基加氫制取芳香胺反應(yīng)中,通過實驗參數(shù)的考察,確定了最佳實驗條件。研究了該材料制作成超級電容器電極材料的電學性能。(2)通過紡絲前驅(qū)體溶液中摻入硝酸鎳,紡絲后獲得含有鎳離子的前驅(qū)體復合纖維膜,經(jīng)過預氧化階段、高溫焙燒過程后獲得含有鎳納米粒子的碳纖維催化材料。利用該方法可以有效控制復合材料的活性中心含量,對所制備的復合催化材料進行一系列表征測試,結(jié)果表明鎳納米粒子均勻分布于碳纖維基體內(nèi)。考察了不同比例和不同碳化溫度制備的催化劑催化芳香型硝基化合物加氫制取芳香胺反應(yīng),結(jié)果表明碳化溫度為600℃、聚丙烯腈單體AN和硝酸鎳的摩爾比為10獲得的催化劑催化性能最優(yōu)。電化學測試結(jié)果表明內(nèi)摻硝酸鎳的電極材料電化學性能優(yōu)于純碳纖維材料。(3)為改善制備所得復合材料的柔軟性,紡絲前驅(qū)體溶液中摻入一定比例的有機鎳鹽(乙酰丙酮鎳),經(jīng)過靜電紡絲、預氧化、高溫焙燒過程后獲得Ni NPs/CNFs催化劑。系統(tǒng)研究了復合催化劑應(yīng)用于催化加氫反應(yīng)中的催化性能,結(jié)果表明:聚丙烯腈單體AN與乙酰丙酮鎳的摩爾比為10、碳化溫度為600℃、反應(yīng)時間為6 h、催化劑用量為0.05 g催化反應(yīng)轉(zhuǎn)化率最高,TEM測試表明平均粒徑為8 nm的鎳納米粒子均勻分布于碳纖維載體內(nèi)。電化學性能測試循環(huán)伏安曲線可知當掃描速率為2 m V/s時,比電容達到最大值60 F g-1,且呈現(xiàn)隨掃描速率增大電容值逐漸減小的趨勢?傊,將鎳納米粒子與碳纖維結(jié)合制備的新型材料,有效改善傳統(tǒng)催化劑的弊端,為后續(xù)的新型催化劑的開發(fā)提供新的思路,同時也為納米鎳基材料在催化領(lǐng)域和電化學領(lǐng)域提供一定的理論基礎(chǔ)。
[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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