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search.filters.applied.f.access: openAccess × Type: Article × Subject: Synthesis (chemical) × WGL Institute: IPF ×

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Now showing 1 - 3 of 3
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    High molecular weight mechanochromic spiropyran main chain copolymers via reproducible microwave-assisted Suzuki polycondensation
    (Cambridge : RSC Publ., 2015) Metzler, Lukas; Reichenbach, Thomas; Brügner, Oliver; Komber, Hartmut; Lombeck, Florian; Müllers, Stefan; Hanselmann, Ralf; Hillebrecht, Harald; Walter, Michael; Sommer, Michael
    Suzuki–Miyaura polycondensation (SPC) is widely used to prepare a variety of copolymers for a broad range of applications. Although SPC protocols are often used in many instances, the limits of this method and issues of molecular weight reproducibility are not often looked at in detail. By using a spiropyran-based (SP) mechanochromic copolymer, we present an optimized protocol for the microwave-assisted synthesis of a mechanochromic, alternating copolymer P(SP-alt-C10) via SPC that allows the reproduction of molecular weight distributions. Several parameters such as microwave power, temperature, stoichiometry, and ligand are screened, leading to molecular weights up to Mw ∼ 174 kg mol−1. The process of optimization is guided by NMR end group analysis which shows that dehalogenation, oxidative deborylation and SP cleavage are the limiting factors that impede further increase of molar mass, while other classical side reactions such as protiodeborylation are not observed. Embossing films of P(SP-alt-C10) yields the colored merocyanine (MC) copolymer P(MC-alt-C10) that undergoes a thermally facilitated back reaction to P(SP-alt-C10). DFT suggests that the barrier of the SP → MC transition has two contributions, with the first one being related to the color change and the second one to internal bond reorganizations. The barrier height is 1.5 eV, which suggests that the ease of the thermally facilitated back reaction is either due to residual energy stored in the deformed polymer matrix, or arises from an MC isomer that is not in the thermodynamically most stable state.
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    Studies towards synthesis, evolution and alignment characteristics of dense, millimeter long multiwalled carbon nanotube arrays
    (Frankfurt, M. : Beilstein-Institut zur Förderung der Chemischen Wissenschaften, 2011) Mahanandia, P.; Schneider, J.J.; Engel, M.; Stühn, B.; Subramanyam, S.V.; Nanda, K.K.
    We report the synthesis of aligned arrays of millimeter long carbon nanotubes (CNTs), from benzene and ferrocene as the molecular precursor and catalyst respectively, by a one-step chemical vapor deposition technique. The length of the grown CNTs depends on the reaction temperature and increases from ~85 μm to ~1.4 mm when the synthesis temperature is raised from 650 to 1100°C, while the tube diameter is almost independent of the preparation temperature and is ~80 nm. The parallel arrangement of the CNTs, as well as their tube diameter can be verified spectroscopically by small angle X-ray scattering (SAXS) studies. Based on electron diffraction scattering (EDS) studies of the top and the base of the CNT films, a root growth process can be deduced.
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    Hollow Au@TiO2 porous electrospun nanofibers for catalytic applications
    (Cambridge : RSC, 2020) Kumar, Labeesh; Singh, Sajan; Horechyy, Andriy; Formanek, Petr; Hübner, René; Albrecht, Victoria; Weißpflog, Janek; Schwarz, Simona; Puneet, Puhup; Nandan, Bhanu
    Catalytically active porous and hollow titania nanofibers encapsulating gold nanoparticles were fabricated using a combination of sol-gel chemistry and coaxial electrospinning technique. We report the fabrication of catalytically active porous and hollow titania nanofibers encapsulating gold nanoparticles (AuNPs) using a combination of sol-gel chemistry and coaxial electrospinning technique. The coaxial electrospinning involved the use of a mixture of poly(vinyl pyrrolidone) (PVP) and titania sol as the shell forming component, whereas a mixture of poly(4-vinyl pyridine) (P4VP) and pre-synthesized AuNPs constituted the core forming component. The core-shell nanofibers were calcined stepwise up to 600 °C which resulted in decomposition and removal of the organic constituents of the nanofibers. This led to the formation of porous and hollow titania nanofibers, where the catalytic AuNPs were embedded in the inner wall of the titania shell. The catalytic activity of the prepared Au@TiO2 porous nanofibers was investigated using a model reaction of catalytic reduction of 4-nitrophenol and Congo red dye in the presence of NaBH4. The Au@TiO2 porous and hollow nanofibers exhibited excellent catalytic activity and recyclability, and the morphology of the nanofibers remained intact after repeated usage. The presented approach could be a promising route for immobilizing various nanosized catalysts in hollow titania supports for the design of stable catalytic systems where the added photocatalytic activity of titania could further be of significance. This journal is © The Royal Society of Chemistry.