發(fā)布時(shí)間：2019-03-18 11:48

【摘要】：本課題分別用物理和化學(xué)的方法對(duì)多壁碳納米管(MWCNTs)進(jìn)行表面修飾,使其接枝親水基團(tuán),進(jìn)而改善其在溶劑中的分散性。將改性后的碳納米管與聚乙烯醇(PVA)共混,經(jīng)過濕法紡絲和熱拉伸制得PVA/MWCNTs復(fù)合纖維,并對(duì)其結(jié)構(gòu)和性能進(jìn)行了研究,主要研究內(nèi)容與結(jié)論如下:(1)通過傅克烷基化反應(yīng)將PVA接枝到MWCNTs的表面,通過對(duì)比優(yōu)化出最佳反應(yīng)條件,核磁共振(13C NMR)和拉曼光譜(Raman spectra)證明了PVA和碳管之間的化學(xué)鍵連接。將制得的功能化MWCNTs(f-MWCNTs)在溶劑(DMSO/H2O(vol ratio=3/1))中進(jìn)行分散,并在室溫下放置一定時(shí)間,觀察其分散情況,并通過紫外-可見分光光度計(jì)(UV-vis),透射電子顯微鏡(TEM)觀測其分散程度,結(jié)果表明碳納米管能夠在溶劑中均勻地分散。另外,傳統(tǒng)的以王水處理MWCNTs使其表面帶上羧基進(jìn)而改善其水溶性的方法也作為對(duì)比試驗(yàn)進(jìn)行。實(shí)驗(yàn)及測試結(jié)果表明,王水處理過的MWCNTs表面有嚴(yán)重的破壞,碳管表面的石墨烯層存在大量的缺陷,而傅克烷基化處理的碳納米管結(jié)構(gòu)幾乎沒有受到破壞。(2)將最佳分散的f-MWCNTs和PVA通過濕法紡絲工藝制備PVA/f-MWCNTs復(fù)合纖維并進(jìn)行熱拉伸。對(duì)制成的纖維進(jìn)行力學(xué),熱學(xué),表面形貌和導(dǎo)電性能進(jìn)行研究,結(jié)果表明,PVA/f-MWCNTs復(fù)合纖維的強(qiáng)度和模量與純PVA纖維對(duì)比分別增加了280.6%和421.0%。差示掃描量熱法(DSC)結(jié)果說明碳納米管的引入降低了PVA的結(jié)晶性能,而掃描電子顯微鏡(SEM)圖像間接說明了在復(fù)合纖維中,一開始隨著碳納米管含量的增加碳納米管與聚合物基體之間的結(jié)合力逐漸變大,而當(dāng)碳管含量達(dá)到一定的含量時(shí),會(huì)發(fā)生團(tuán)聚現(xiàn)象,進(jìn)而對(duì)復(fù)合纖維力學(xué)和導(dǎo)電性能都產(chǎn)生嚴(yán)重影響。王水處理的碳管在相同條件下所得纖維無論是熱穩(wěn)定性還是力學(xué)性能都遠(yuǎn)遠(yuǎn)低于f-MWCNTs復(fù)合纖維。(3)作為與化學(xué)修飾的對(duì)比,用迷迭香酸(RosA)和其他幾種分散劑(單寧酸,十二烷基苯磺酸鈉和原花青素)分別對(duì)碳納米管進(jìn)行表面修飾,在室溫條件下放置一段時(shí)間,觀察其分散性,并采用TEM,UV-vis光譜對(duì)溶液進(jìn)行表征,結(jié)果表明經(jīng)過RosA修飾的碳納米管(m-MWCNTs)能夠在室溫下穩(wěn)定分散在水溶液中達(dá)30天,TEM表明碳納米管的規(guī)整石墨烯結(jié)構(gòu)并沒有遭到破壞。核磁共振氫譜(1H NMR)和拉曼光譜結(jié)果表明多壁碳納米管和RosA之間存在???堆垛的相互作用。(4)把經(jīng)RosA修飾的碳管和聚乙烯醇溶液進(jìn)行共混,通過濕法紡絲以及熱拉伸的工藝制成PVA/m-MWCNTs復(fù)合纖維并進(jìn)行表征。DSC表明了m-MWCNTs的引入相當(dāng)于在體系中引入了成核劑,其結(jié)晶變得更加容易。力學(xué)性能的測試表明碳管的引入能夠提高纖維的強(qiáng)度和模量,同時(shí)不會(huì)對(duì)纖維表面造成大的影響。
[Abstract]:In this paper, the surface modification of multi-walled carbon nanotubes (MWCNTs) was carried out by means of physical and chemical methods, and the hydrophilic groups were grafted onto them to improve their dispersibility in solvent. The modified carbon nanotubes (CNTs) were blended with polyvinyl alcohol (PVA), and the PVA/MWCNTs composite fibers were prepared by wet spinning and hot drawing. The structure and properties of the composite fibers were studied. The main contents and conclusions are as follows: (1) PVA was grafted onto the surface of MWCNTs by Fourier alkylation, and the optimum reaction conditions were optimized by comparison. Nuclear magnetic resonance (13C NMR) and Raman spectroscopy (Raman spectra) proved the chemical bonding between PVA and carbon tube. The functionalized MWCNTs (f-MWCNTs) was dispersed in the solvent (DMSO/H2O (vol ratio=3/1) and placed at room temperature for a period of time to observe its dispersion. The dispersion was observed by ultraviolet-visible spectrophotometer (UV-vis). The degree of dispersion of CNTs was observed by transmission electron microscope (TEM). The results showed that CNTs could be dispersed uniformly in solvent. In addition, the traditional treatment of MWCNTs with Wang Shui to bring carboxyl groups on its surface and improve its water solubility was also carried out as a contrast test. The experimental and test results show that the surface of MWCNTs treated by Wang Shui has serious damage, and there are a lot of defects in the graphite layer on the surface of carbon tube. However, the structure of CNTs treated by Fourier alkylation was almost undamaged. (2) the best dispersed f-MWCNTs and PVA were prepared by wet spinning and hot drawing of PVA/f-MWCNTs composite fibers. The mechanical, thermal, surface morphology and conductive properties of the fibers were studied. The results showed that the strength and modulus of PVA/f-MWCNTs composite fibers were 280.6% and 421.0% higher than those of pure PVA fibers, respectively. The results of differential scanning calorimetry (DSC) (DSC) showed that the introduction of CNTs decreased the crystallization properties of PVA, while the (SEM) images of scanning electron microscopy (SEM) indirectly showed that in the composite fibers, the crystalline properties of CNTs were decreased. At first, with the increase of the content of carbon nanotubes, the bonding force between carbon nanotubes and polymer matrix gradually increased, but when the content of carbon nanotubes reached a certain content, there would be agglomeration phenomenon. Furthermore, the mechanical and conductive properties of composite fibers are seriously affected. The thermal stability and mechanical properties of the carbon tube treated by Wang Shui under the same conditions are much lower than that of the f-MWCNTs composite fiber. (3) as a comparison with the chemical modification, the fiber obtained by Wang Shui is much lower in thermal stability and mechanical properties. Carbon nanotubes (CNTs) were modified with rosemary acid (RosA) and other dispersants (tannic acid, sodium dodecyl benzene sulfonate and procyanidins) respectively. The dispersion of CNTs was observed at room temperature for a period of time. The dispersion of CNTs was observed by TEM,. The solution was characterized by UV-vis spectra. The results showed that RosA-modified carbon nanotubes (m-MWCNTs) could be stably dispersed in aqueous solution for up to 30 days at room temperature. TEM showed that the regular graphene structure of CNTs was not destroyed. Nuclear magnetic resonance (1H NMR) and Raman spectra show that there exists between multi-walled carbon nanotubes (MWNTs) and RosA. Stacking interaction. (4) blending of RosA modified carbon tubes and polyvinyl alcohol solution. PVA/m-MWCNTs composite fibers were prepared by wet spinning and hot drawing. It was shown that the introduction of m-MWCNTs was equivalent to the introduction of nucleating agent in the system, and its crystallization became easier. The test of mechanical properties shows that the introduction of carbon tube can improve the strength and modulus of the fiber, but it has no great effect on the surface of the fiber.
【學(xué)位授予單位】：蘇州大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2015
【分類號(hào)】：TB383.1;TQ342.94

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