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HPLC 硅胶微球上碳纳米管的辐射接枝:理论与实际方面。

Radiation-induced grafting of carbon nanotubes on HPLC silica microspheres: theoretical and practical aspects.

机构信息

Department of Chemistry, University of Pavia, via Taramelli 12, 27100 Pavia, Italy.

出版信息

Analyst. 2013 Jul 7;138(13):3778-85. doi: 10.1039/c3an00163f.

Abstract

Multi-walled carbon nanotubes (MWCNTs) were grafted for the first time by γ-radiation onto silica microspheres in the presence of polybutadiene (PB) as the linking agent, obtaining a novel hybrid material with chromatographic properties, with an alternative approach to the existing procedures. The synthesis involves the one-pot γ-radiation-induced grafting of MWCNTs onto silica microspheres in the presence of PB as a linking agent. PB also serves as a coating layer of the silica particles, to which MWCNTs are anchored through stable chemical bonds formed via radical chain reaction with the polymer. The product (MWCNT-PB-modified silica) resulted in MWCNT bundles interlaying the silica particles which acted as a support and as a spacer. This new material highlights the unquestionable properties of CNTs also when grafted in a composite, thus allowing the disposition of a more robust material whose properties are still related to the nanotube structure. The grafting was confirmed by Raman spectroscopy. The surface area, determined by BET isotherms, resulted in 132 m(2) g(-1), about 34% lower than that of pure silica, pointing to the cross-linking effect of PB in the silica matrix. The evaluation of MWCNT-PB-modified silica as a LC stationary phase was performed by separation of aromatics, with satisfactory resolution and reproducibility, while structural selectivity was proved by isomer separation. A good resolution was obtained also for acid/basic compounds as barbiturates. A comparison with a commercial C18 sorbent highlighted the advantage in using the CNT column for separating aromatic hydrocarbons. Control experiments on the PB-coated silica column proved the key role of MWCNTs in the chromatographic performance.

摘要

多壁碳纳米管(MWCNTs)首次通过γ射线在聚丁二烯(PB)存在的情况下接枝到硅胶微球上,得到了一种具有色谱性能的新型杂化材料,这是一种替代现有方法的新方法。该合成方法涉及在 PB 作为连接剂的存在下,通过一锅γ射线诱导将 MWCNTs 接枝到硅胶微球上。PB 还作为硅胶颗粒的涂层,MWCNTs 通过与聚合物的自由基链反应形成的稳定化学键锚定在该涂层上。所得产物(MWCNT-PB 修饰的硅胶)导致 MWCNT 束交错排列在硅胶颗粒中,硅胶颗粒既充当支撑物又充当间隔物。这种新材料突出了 CNT 即使在复合材料中接枝也具有不可置疑的性能,从而允许使用更坚固的材料,其性能仍然与纳米管结构有关。接枝通过拉曼光谱得到证实。通过 BET 等温线确定的表面积为 132 m(2) g(-1),比纯硅胶低约 34%,表明 PB 在硅胶基质中的交联效应。通过分离芳烃评价 MWCNT-PB 修饰的硅胶作为 LC 固定相,得到了令人满意的分辨率和重现性,而通过异构体分离证明了结构选择性。酸/碱性化合物(巴比妥酸盐)也获得了良好的分离度。与商用 C18 吸附剂的比较突出了使用 CNT 柱分离芳烃的优势。在 PB 涂层硅胶柱上进行的对照实验证明了 MWCNTs 在色谱性能中的关键作用。

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