Preparation and characterization of vanadium(IV) oxide supported on SBA-15 and its catalytic performance in benzene hydroxylation to phenol using molecular oxygen

Preparation of dispersed transition metal oxides catalyst with low oxidation state still remains a challenging task in heterogeneous catalysis.In this study,vanadium oxides supported on zeolite SBA-15 have been prepared under hydrothermal condition using V 2 O 5 and oxalic acid as sources of vanadium and reductant,respectively.The structures of samples,especially the oxidation state of vanadium,and the surface distribution of vanadium oxide species,have been thoroughly characterized using various techniques,including N 2-physisorption,X-ray diffraction(XRD),transmission electron microscopy(TEM),X-ray photoelectron spectroscopy(XPS),UV-visible spectra(UV-Vis) and UV-visible-near infrared spectra(UV-Vis-NIR).It is found that the majority of supported vanadium was in the form of vanadium(IV) oxide species with the low valence of vanadium.By adjusting hydrothermal treatment time,the surface distribution of vanadium(IV) oxide species can be tuned from vanadium(IV) oxide cluster to crystallites.These materials have been tested in the hydroxylation of benzene to phenol in liquid-phase with molecular oxygen in the absence of reductant.The catalyst exhibits high selectivity for phenol(61%) at benzene conversion of 4.6%,which is a relatively good result in comparison with other studies employing molecular oxygen as the oxidant.     

Effective optical path length investigation for cubic diffuse cavity as gas absorption cell

A simple cubic-shaped cavity with a high-diffuse-reflectivity inner coating as a novel gas detection cell was developed. The effective optical path length (EOPL) was evaluated by comparing the oxygen absorption signal in the cavity and in air based on tunable diode laser absorption spectroscopy. The law for a spherical cavity was applied and modified to a cubic cavity as a function of reflectivity ρ, port fraction f, and the side length. Single-pass average path length of the cubic cavity was 0.723(7) times the side length. EOPL can be modified conveniently by adjusting the parameters of the cavity.     

Hierarchical nanostructured composite cathode with carbon nanotubes as conductive scaffold for lithium-sulfur batteries

Carbon nanotubes (CNTs) are excellent scaffolds for advanced electrode materials, resulting from their intrinsic sp2 carbon hybridization, interconnected electron pathway, large aspect ratio, hierarchical porous structures, and low cost at a large-scale production. How to make full utilization of the mass produced CNTs as building blocks for nanocomposite electrodes is not well understood yet. Herein, a composite cathode containing commercial agglomerated multi-walled CNTs and S for Li-S battery was fabricated by a facile melt-diffusion strategy. The hierarchical CNT@S coaxial nanocables exhibited a discharging capacity of 1020 and 740 mAh g-1 at 0.5 and 2.0 C, respectively. A rapid capacity decay of 0.7% per cycle at the initial 10 cycles and a slow decay rate of 0.14% per cycle for the later 140 cycles were detected. Such hierarchical agglomerated CNT@S cathodes show advantages in easy fabrication, environmentally benign, low cost, excellent scalability, and good Li ion storage performance, which are extraordinary composites for high performance Li-S battery.     

Synthesis and characterization of fluorine-containing cholesteric liquid crystalline polysiloxanes bearing trifluoromethyl-substituted mesogens

A series of side-chain liquid crystal (LC) polysiloxanes were synthesised with Poly(methylhydrogeno)siloxane, 4?-(undec-10-enoyloxy) biphenyl – 4 – yl 4- (trifluoromethyl) benzoate (M_th) and a chiral nematic (N*) LC monomer 1-allyl 10-(cholesteryl)-decanedioate (M_ch). The chemical structures and LC properties of the monomers and polymers were characterised by FTIR, ¹H-NMR, differential scanning calorimetry, thermogravimetric analysis, POM and X-ray diffractometer. M_ch is monotropic N* LC. The homopolymer derived from monomer M_ch is enantiotropic N* LC. Monomer M_th is a smectic A liquid crystal. The copolymers derived from M_ch and M_th are N* LCs. The temperatures at which 5% weight loss occurred are greater than 300°C for all the fluoro-containing polymers, and the residue weights of the samples at 600°C increased slightly as the content of trifluoromethyl mesogens increased in the polymers. The glass transition temperatures of the polymers increased as trifluoromethyl mesogens increased, too. The N*–I phase transition temperatures show a negative deviate from ideal or linear behaviour. The values of the enthalpy changes for the cholesteryl containing polymers are rather low and this is attributed to the biaxiality of cholesteryl moiety which tends to reduce the change in the orientational order at the N*–I transition. Compared to the monomers, the polymers show wider mesophase region.     

Nano n‐propylsulfonated γ‐Al2O3: a new,efficient and reusable catalyst for synthesis of spiro[indoline‐3,4‐pyrazolo[3,4‐e][1,4]thiazepine]diones in aqueous media

Nano n‐propylsulfonated γ‐Al₂O₃ is easily prepared by the reaction of nano γ‐Al₂O₃ with 1,3‐propanesultone. This reagent can be used as an efficient catalyst for the synthesis of spiro [indoline‐3,4‐pyrazolo[3,4‐e][1,4]thiazepine]diones in aqueous media. This new method consistently has the advantages of excellent yields and short reaction times. Further, the catalyst can be reused and recovered several times. Copyright © 2013 John Wiley & Sons, Ltd.