A strategy for the functionalization of single-walled carbon nanotubes is reported. The synthesis involved the conversion of fluorinated single-walled carbon nanotubes to the thiolated derivative assisted by phosphorous pentasulfide. The thiol group is then quantitatively oxidized to the sulfonic acid group. The extent of oxidation of the thiol precursor is confirmed using X-ray photoelectron spectroscopy, which proved to be immensely useful to discriminate between the -SH and -SO 3 H with a chemical shift for the sulfur 2p (approx. 5 eV). The functionalized carbon nanotubes were further characterized by infrared spectroscopy, thermogravimetric analysis, and transmission electron microscopy which revealed a significant change in morphology between the fluoro carbon nanotubes, the thiol and sulfonic acid-modified carbon nanotubes.
Porous silica was synthesized via the sol-gel process using clay obtained locally from Ijero-Ekiti in Ekiti State, Nigeria and compared with silica synthesized under similar conditions from sodium metasilicate (Na 2 SiO 3 ) obtained comercially. The clay was initially refluxed with sodium hydroxide (NaOH) for 2 hours to extract SiO 2 to form Na 2 SiO 3 , which was subsequently hydrolyzed to form a gel. The gel obtained was washed with deionized water to get rid of impurities, dried and calcined at 800˚C for 3 hours. The obtained silica powders were characterized using atomic absorption spectrophotometer, Fourier transform infrared (FTIR) spectroscopy, X-ray diffraction (XRD) and scanning electron microscopy (SEM). Results showed that the vibrational modes and diffraction patterns of the silica derived from commercial Na 2 SiO 3 and that prepared from clay were similar containing pure amorphous SiO 2 . The morphology of the commercially obtained silica showed better arrangement of particles and exhibited slightly lesser porosity (62.4%) compared to that derived from clay which had a porosity of 65.5%. The result indicates that clay has a potential for use as an environmentally safe and economic starting material for preparing porous silica instead of high quality precursors.
Boron-10 enriched boric acid, H310BO3, was converted to the corresponding sodium borohydride, Na10BH4, in essentially quantitative yields, by using slightly modified literature methods involving the formation of butyl borate, (n-OBu)310B, first and then reacting it with NaH in mineral oil. The oxidation reaction of Na10BH4 with I2 in diglyme and subsequent addition/purification in dioxane gave Na[10B3H8]0.3(C4H8O2) that reacted further with NiCl2 in either anhydrous benzene or heavy mineral oil at 110 degrees C to produce the corresponding 10B5H9 as the first isolated 10B-enriched liquid boron hydride in a laboratory environment. Treatment of this 10B5H9 with NaH or t-BuLi in 2:1 molar ratio underwent a cage expansion reaction to produce the [M]10B9H14 that undergoes a redox reaction in situ with anhydrous NiCl2 in n-hexane to yield the corresponding fused cage anti-10B18H22 as the only solid borane product in 42% yield, thus establishing new synthetic routes for the preparation of 10B-enriched polyhedral boranes.
Aminopropyltriethoxysilane and aminopropyl-phosphonic ester modified carbon nanotubes were prepared by reacting fluorinated carbon nanotubes (F-CNTs) with the 3-aminopropyltriethoxysilane or 3-aminopropyl-phosphonic acid reagents at 120 °C temperature, using pyridine as the base catalyst. These functionalized carbon nanotubes, APTES-CNTs, 1, and APPA-CNTs, 2, were characterized by transmission electron microscopy (TEM), infrared spectroscopy (IR), and thermogravimetric analysis (TGA). The homogeneous dispersion of these functionalized CNTs (0.1%) in silica were also accomplished by sol-gel processing. The TEM confirmed uniform dispersion of the functionalized CNT in silica.
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