Low‐temperature photoinitiation solution polymerization behavior of N‐vinylcarbazole in tetrahydrofuran

N‐Vinylcarbazole (VCZ) was solution‐polymerized in tetrahydrofuran (THF) at ?20, 0, and 20°C using the photoinitiation method; the effects of the amount of solvent, polymerization temperature, and photoinitiator concentration were investigated. On the whole, the experimental results corresponded to predicted ones. Low polymerization temperature using photoinitiation proved to be successful in obtaining poly(N‐vinylcarbazole) (PVCZ) of a high molecular weight with a smaller temperature rise during polymerization; nevertheless of free radical polymerization by 2,2′‐azobis(2,4‐dimethylvaleronitrile) (ADMVN). The photo‐solution polymerization rate of VCZ in THF was proportional to the 0.47 power of ADMVN concentration. The molecular weight was higher and the molecular weight distribution was narrower with PVCZ polymerized at lower temperatures. For PVCZ prepared in THF at ?20°C using a photoinitiator concentration of 0.00005 mol/mol of VCZ, a weight‐average molecular weight of 510,000 was obtained, with a polydispersity index of 1.73, and a degree of lightness converged to about 99%. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 86: 3667–3672, 2002     

Characterization of pressure signals in a bubble column by wavelet packet transform

All experiments of pressure fluctuations were carried out in a bubble column with a moderately large column of 0.376 m ID. The recently developed technique of wavelet packet transform based on localized wavelet functions is applicable to analysis of the fluctuating signals. The time series of pressure fluctuation signals have been analyzed by means of wavelet packet transform components, decomposition through best basis algorithm and timefrequency representation. By resorting to this technique, the objects in bubbly flow regime have fine scales and frequencies than ones in churn-turbulent flow regime. Thus, this wavelet packet transform method enables us to obtain the frequency content of local complex flow behaviors in a bubble column.     

Separation of Triacylglycerol Species from Interesterified Oils by High-Performance Liquid Chromatography

Using a 1,3-regioselective lipase as a catalyst, soybean oil and olive oil were interesterified with the short-chain triacylglycerol tributyrin (1,2,3-tributyrylglycerol) to produce mixtures of structured triacylglycerols (SL-TAG). The SL-TAG were purified by column chromatography and analyzed by both normal-phase (silica column; NP_SIL) and reversed-phase [octadecyl silane (ODS) column] high-performance liquid chromatography (HPLC). Individual SL-TAG molecular species were detected by evaporative light-scattering detection, and characterized by mass spectrometry. NP_SIL HPLC successfully separated the newly synthesized SL-TAG into two groups of TAG: one composed of one butyryl group and two long-chain fatty acyl groups (from soybean or olive oil); the second was composed of two butyryl groups and one long-chain fatty acyl group. The SL-TAG species were further analyzed by reversed-phase HPLC which gave a more detailed separation of the TAG species present in the two SL-TAG.     

Synthesis and biological activity of phthalimide‐based polymers containing 5‐fluorouracil

The attachment of anticancer agents to polymers is a promising approach towards reducing the toxic side‐effects and retaining the potent antitumour activity of these agents. A new tetrahydrophthalimido monomer containing 5‐fluorouracil (ETPFU) and its homopolymer and copolymers with acrylic acid (AA) and with vinyl acetate (VAc) have been synthesized and spectroscopically characterized. The ETPFU contents in poly(ETPFU‐co‐AA) and poly(ETPFU‐co‐VAc) obtained by elemental analysis were 21 mol% and 20 mol%, respectively. The average molecular weights of the polymers determined by gel permeation chromatography were as follows: M_n = 8900 g mol^?1, M_w = 13 300 g mol^?1, M_w/M_n = 1.5 for poly(ETPFU); M_n = 13 500 g mol^?1, M_w = 16 600 g mol^?1, M_w/M_n = 1.2 for poly(ETPFU‐co‐AA); M_n = 8300 g mol^?1, M_w = 11 600 g mol^?1, M_w/M_n = 1.4 poly(ETPFU‐co‐VAc). The in vitro cytotoxicity of the compounds against FM3A and U937 cancer cell lines increased in the following order: ETPFU > 5‐FU > poly(ETPFU) > poly(ETPFU‐co‐AA) > poly(ETPFU‐co‐VAc). The in vivo antitumour activities of all the polymers in Balb/C mice bearing the sarcoma 180 tumour cell line were greater than those of 5‐FU and monomer at the highest dose (800 mg kg^?1). © 2002 Society of Chemical Industry     

Effect of water pretreatment on CO<Subscript>2</Subscript> capture using a potassium-based solid sorbent in a bubbling fluidized bed reactor

A bubbling fluidized bed reactor was used to study CO₂ capture from flue gas by using a potassium-based solid sorbent, sorbKX35 which was manufactured by the Korea Electric Power Research Institute. A dry sorbent, sorbKX35, consists of K₂CO₃ for absorption and supporters for mechanical strength. To increase initial CO₂ removal, some amount of H₂O was absorbed in the sorbent before injecting simulated flue gas. It was possible to achieve 100% CO₂ removal for more than 10 minutes at 60°C and a residence time of 2 s with H₂O pretreatment. When H₂O pretreatment time was long enough to convert K₂CO₃ of sorbKX35 into K₂CO₃ · 1.5H₂O, CO₂ removal was excellent. The results obtained in this study can be used as basic data for designing and operating a large scale CO₂ capture process with two fluidized bed reactors. This work was presented at the 6 ^th Korea-China Workshop on Clean Energy Technology held at Busan, Korea, July 4–7, 2006.     

Effects of Y2O3 and ZrO2 on the Densification of Si3N4-Zr(Y)O2 Composites

The effects of ZrO₂ and Y₂O₃ on the densification of hotpressed Si₃N₄-Zr(Y)O₂ composites have been studied. High density could not be obtained by the addition of pure or 3-mol%-Y₂O₃-doped ZrO₂ in this composite; however, nearly full density (>97%) could be obtained in Si₃N₄ using 6- and 8-mol%-Y₂O₃-doped ZrO₂. It is concluded that Y₂O₃ diffusing out from the added Zr(Y)O₂ promoted the densification and that ZrO₂ also had some role in the formation of an oxynitride glass.     

Fabrication of Patterned Inorganic–Organic Hybrid Film for the Optical Waveguide by Microfluidic Lithography

Inorganic–organic hybrid materials for the optical waveguide were synthesized by the sol–gel process starting from the acid-catalyzed solutions of phenyltrimethoxysilane, methyltriethoxysilane, and tetraethylorthosilicate. The control of the refractive index in the organically modified silicate films was achieved by varying the content of phenyltrimethoxysilane incorporated as a refractive index modifier. A single spin-coating with the precursor solution produced a crack-free buffer layer of 22-μm thickness with a dense microstructure. For the fabrication of the patterned guiding layer on top of the buffer layer, the microfluidic lithography method was used. The patterned microlines of the linewidth of 20–35 μm with a sharp edge definition could form by filling the precursor solutions into the microchannels associated with the polydimethylsiloxane microfluidic device. The patterned guiding layer was optically transparent as similar as the bare quartz glass at the wavelength above 500 nm and had a low propagation loss of 0.77 dB/cm at 1310 nm.     

Universal yield stress function for biocompatible chitosan based-electrorheological fluid: Effect of particle concentration

Electrorheological (ER) response of biocompatible particles suspended in an insulating silicone oil, was investigated under several different applied external electric field strengths. Chitosan, a biodegradable polysaccharide, was used as anhydrous ER materials. The effect of particle volume concentration on their ER response was examined by focusing on the measurement for rheological and electrical properties. The yield stress of chitosan suspended in silicone oil system as a function of applied electric field strength showed different value of slopes for different particle concentrations, however, all data points collapse onto a universal scaling function.     

Synergic influence of a surfactant and ultrasonication on the preparation of soluble,conducting polydiphenylamine/silica‐nanoparticle composites

Conducting polydiphenylamine was used to encapsulate silica nanoparticles through the oxidative polymerization of diphenylamine in the presence of ultrasonic irradiation. The polymerization was performed in the presence of sodium lauryl sulfate as a surfactant. Experiments performed in the absence of ultrasound clearly demonstrated that the application of ultrasonication played multiple roles in the preparation of a composite of polydiphenylamine with silica nanoparticles. Ultrasonication dispersed the silica nanoparticles, converted sodium lauryl sulfate to lauryl alcohol, and augmented the dispersion of the silica‐nanoparticle/polydiphenylamine composite in an organic medium. Silica‐nanoparticle/polydiphenylamine composites were also prepared in the absence of ultrasound and/or sodium lauryl sulfate. The silica‐nanoparticle/polydiphenylamine composites were characterized with Fourier trans form infrared spectroscopy, ultraviolet–visible/near‐infrared spectroscopy, and thermogravimetric analysis. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 102: 3912–3918, 2006     

Amelioration of mechanical brittleness in hyperbranched polymer. 1. Macroscopic evaluation by dynamic viscoelastic relaxation

Hyperbranched poly(ether ketone)-b-linear poly(ether ketone)-b-hyperbranched poly(ether ketone) (HLHPEK) triblock copolymers with two different block compositions were prepared as an approach to improve the mechanical brittleness of hyperbranched poly(ether ketone) (HPEK). From the time-temperature superposition of dynamic shear moduli, G′(ω) and G″(ω), of HPEK and two HLHPEKs, it was investigated that the junction points between G′(ω) and G″(ω) shifted to the higher frequencies and the rubbery plateau region spread wider over the reduced frequency axis as the linear blocks were introduced and their compositions were increased. Such changes in viscoelastic response were consequences of increase in the amount of chain entanglements additionally formed by the linear blocks. In order to verify the effect of the linear block incorporation on amelioration of the mechanical brittleness, the degree of brittleness and its improvement were evaluated from the temperature dependence of the shift factors, a_Ts, experimentally obtained during the superposition of the dynamic moduli and of the average viscoelastic relaxation times, τ_HNs, determined with empirical Havriliak-Negami distribution function. From the nonlinear curve fittings of the a_Ts and the τ_HNs by the Vogel-Tamman-Fulcher equation, the degree of brittleness for HPEK and HLHPEK triblock copolymers were quantified as values of the material parameter D, an indicative of deviation from the linear Arrhenius behavior and a measure of fragility of the given material. The tendency of increasing D values with the linear block compositions confirmed substantial improvement of the mechanical brittleness in the HLHPEK triblock copolymers compared to HPEK. Therefore, the approach to copolymerize HPEK with its chemically analogous linear counterpart was verified to be an effective strategy to impart molecular entanglements and hence ameliorate the mechanical brittleness on the basis of macroscopic rheological evaluation.