本文選題：單壁碳納米管 + 分散　； 參考：《北京服裝學(xué)院》2015年碩士論文

【摘要】：單壁碳納米管（SWCNTs）自被發(fā)現(xiàn)以來(lái)，因其獨(dú)特及優(yōu)異的物理化學(xué)性質(zhì)，使其在電子、復(fù)合材料、生物醫(yī)學(xué)等眾多領(lǐng)域都表現(xiàn)出了良好的發(fā)展前景。不同結(jié)構(gòu)的SWCNTs性質(zhì)不同，而目前制備手段生產(chǎn)出的SWCNTs均是不同手性、不同管徑的混合物，對(duì)于這類(lèi)混合物的分離和性能評(píng)價(jià)目前尚無(wú)適宜的方法和統(tǒng)一的評(píng)價(jià)標(biāo)準(zhǔn)。這種狀況不僅增加了SWCNTs的質(zhì)量控制難度，而且也極大地阻礙到了它的應(yīng)用。本論文正是基于此目的，從SWCNTs應(yīng)用的角度，對(duì)其分散與手性分離方法進(jìn)行了研究；另外，為了開(kāi)發(fā)適宜分離SWCNTs的凝膠色譜柱，本文還對(duì)制備殼聚糖微球色譜柱進(jìn)行了探索。 （1）通過(guò)采用十二烷基硫酸鈉（SDS）、脫氧膽酸鈉（DOC）、膽酸鈉（SC）、十二烷基苯磺酸鈉（SDBS）、Tritron X-405及十六烷基三甲基溴化銨（CTMAB）六種表面活性劑對(duì)SWCNTs進(jìn)行超聲分散，確定了紫外-可見(jiàn)-近紅外吸收光譜的吸光度以及共振比分別為評(píng)價(jià)SWCNTs的分散總濃度以及單分散濃度的參量。結(jié)果表明表面活性劑分散SWCNTs總濃度從高到低依次為：SDS DOC X405 SC CTMAB SDBS；SWCNTs單分散濃度從高到低依次為：DOC SC CTMAB X405 SDBS SDS。 （2）利用單根凝膠色譜技術(shù)，考察SDS、DOC、SC、SDBS及X405溶液五種流動(dòng)相對(duì)SWCNTs手性分離的影響。建立了由吸收光譜結(jié)果計(jì)算的面積百分比Si,j，及面積百分比極差之和∑Rsi作為定量表征指標(biāo)的方法，分別對(duì)同一流動(dòng)相和不同流動(dòng)相的分離效果進(jìn)行評(píng)價(jià)，結(jié)果表明SDS溶液作為流動(dòng)相對(duì)SWCNTs的分離效果較佳。 （3）利用單根凝膠色譜法，采用聚乙烯醇凝膠（Toyopearl）、聚丙烯酰胺凝膠(Bio Gel)作為填料對(duì)SWCNTs進(jìn)行手性分離，，并與傳統(tǒng)瓊脂糖凝膠（Sepharose）、丙烯葡聚糖凝膠（Sephacryl）對(duì)比，結(jié)果表明不同凝膠對(duì)SWCNTs手性的選擇性不同，Bio Gel凝膠對(duì)（8,3）、（7,5）、（10,2）手性SWCNTs選擇性較好；Sephacryl凝膠對(duì)（9,4）、（7,6）、（8,4）手性SWCNTs選擇性較好；Toyopearl對(duì)（8,6）手性SWCNTs選擇性較好；Sepharose對(duì)（9,5）、（10,5）、（8,7）手性SWCNTs選擇性較好。并根據(jù)上述結(jié)論，首次采用多種凝膠填料、多根色譜柱階梯法（（凝膠色譜柱填料的順序依次為：Bio Gel，Sephacry，Toyopearl，Sepharose）對(duì)SWCNTs進(jìn)一步分離，可得到手性指數(shù)種類(lèi)更為單一的SWCNTs。 （4）利用離心力場(chǎng)流儀分別對(duì)六種表面活性劑分散的SWCNTs樣品進(jìn)行分離，并用多角度光散射以及紫外檢測(cè)器實(shí)時(shí)在線(xiàn)檢測(cè)。通過(guò)對(duì)檢測(cè)結(jié)果的分析，發(fā)現(xiàn)無(wú)論樣品中碳納米管的分散情況如何，均可實(shí)現(xiàn)不同尺寸的分離，得到了SWCNTs的各個(gè)Rg分布圖。驗(yàn)證了此新方法對(duì)碳納米管分離的適用性。 （5）采用乳化交聯(lián)法，通過(guò)控制反應(yīng)過(guò)程的攪拌速度、殼聚糖濃度、醋酸濃度以及乳化劑含量，制備了成球效果好、粒徑均勻、性質(zhì)穩(wěn)定的殼聚糖微球。用這種微球色譜柱對(duì)SWCNTs進(jìn)行分離，結(jié)果顯示，由于殼聚糖微球的空間網(wǎng)狀結(jié)構(gòu)，對(duì)SWCNTs的分離效果較差，且沒(méi)有有效的流動(dòng)相使碳管與微球分開(kāi)開(kāi)來(lái)。但是，通過(guò)對(duì)殼聚糖微球-SWCNTs的表征，證明了殼聚糖微球能夠大量吸附碳納米管，且穩(wěn)定性、導(dǎo)電性均有所增強(qiáng)，并保持了各自?xún)?yōu)異的性質(zhì)。
[Abstract]:Since the discovery of the single wall carbon nanotube (SWCNTs), because of its unique and excellent physical and chemical properties, it has shown good prospects in many fields, such as electronics, composite materials, biomedicine and many other fields. The properties of different structures are different in the properties of SWCNTs. At present, the SWCNTs of the produced means of production is a mixture of different chiral and different pipe diameters. There is no suitable method and unified evaluation standard for the separation and performance evaluation of this kind of mixture. This situation not only increases the difficulty of the quality control of SWCNTs, but also greatly hinders its application. This paper is based on this purpose and studies the method of dispersion and chiral separation from the angle of SWCNTs application. In addition, in order to develop gel chromatographic column suitable for separation of SWCNTs, the preparation of chitosan microsphere chromatographic column was also explored.
(1) by using twelve alkyl sodium sulfate (SDS), sodium deoxycholate (DOC), sodium cholate (SC), twelve alkyl benzene sulfonate (SDBS), Tritron X-405 and sixteen alkyl three methyl ammonium bromide (CTMAB), six kinds of surfactant were used to disperse SWCNTs to determine the absorbance of ultraviolet visible near infrared absorption spectrum and the resonance ratio of SWC respectively. The total concentration of NTs and the parameters of the monodisperse concentration showed that the total SWCNTs concentration of the surfactant dispersed from high to low was SDS DOC X405 SC CTMAB SDBS, and the SWCNTs monodisperse concentration from high to low was in the order of DOC SC CTMAB.
(2) the effect of five kinds of flow relative to SWCNTs chiral separation of SDS, DOC, SC, SDBS and X405 solution was investigated by single gel chromatography. The separation efficiency of the same flow phase and the different mobile phase was established by the square method of the area percentage Si, J, the area percentage extreme difference and the sigma Rsi, calculated by the absorption spectrum. The results showed that SDS solution had better separation effect than SWCNTs.
(3) the chiral separation of SWCNTs by polyvinyl alcohol gel (Toyopearl) and polyacrylamide gel (Bio Gel) was used as a filler by single gel chromatography, and compared with the traditional agarose gel (Sepharose) and propylene dextran gel (Sephacryl), the results showed that the selectivity of different gels to SWCNTs was different, Bio Gel gel pair (8,3), 7,5 (7,5). (10,2) the selectivity of chiral SWCNTs is better; Sephacryl gel has good selectivity to (9,4), (7,6), (8,4) chiral SWCNTs, Toyopearl to (8,6) chiral SWCNTs is better, Sepharose pairs (9,5), and chiral selectivity is better. And according to the above conclusion, the first kind of gel filler, multi column chromatography (gel chromatography) The sequence of column packing is: Bio Gel, Sephacry, Toyopearl, Sepharose). Further separation of SWCNTs can result in a single SWCNTs. with a more chiral index.
(4) separate the SWCNTs samples of six kinds of surfactant by centrifugal force field flow meter, and use multi angle light scattering and UV detector on line detection. Through the analysis of the detection results, it is found that the dispersion of carbon nanotubes in the samples can be separated in different sizes, and each SWCNTs can be obtained. The Rg distribution map verified the applicability of the new method to the separation of carbon nanotubes.
(5) by controlling the mixing rate of the reaction process, the concentration of chitosan, the concentration of acetic acid and the content of emulsifier, the chitosan microspheres with good ball effect, uniform particle size and stable properties were prepared by emulsifying crosslinking method. The SWCNTs was separated by this microsphere column. The results showed that the space network structure of chitosan microspheres was used for SWCNTs The separation effect is poor, and there is no effective mobile phase to separate the carbon nanotubes from the microspheres. However, the chitosan microspheres have been characterized by the characterization of the chitosan microspheres -SWCNTs. It is proved that the chitosan microspheres can adsorb a large number of carbon nanotubes, and the stability and electrical conductivity are enhanced, and their excellent properties are maintained.
【學(xué)位授予單位】：北京服裝學(xué)院
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2015
【分類(lèi)號(hào)】：TB383.1

【參考文獻(xiàn)】

相關(guān)期刊論文 前1條

1 胡平,范守善,萬(wàn)建偉;碳納米管/UHMWPE復(fù)合材料的研究[J];工程塑料應(yīng)用;1998年01期

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