Polymerization of epoxide with aluminum complex/silanol catalyst. VII. Thermal and electrical properties of epoxy resin cured with the new catalyst

Curing catalyst for epoxy resins was newly found. The catalyst consists of aluminum complex and silanol. Lack of one component of the pair does not cure epoxy resins. The epoxy resins cured with the catalyst are characterized by excellent electrical properties, especially at high temperature, due to the absence of strong acid species in the cured epoxy resin matrix. Heat-resistant property of the resin was also excellent. These properties were compared with those of epoxy resin cured with commonly used BF₃ complex.     

Isotactic polypropylene hollow microfibers prepared by CO2 laser‐thinning

An isotactic polypropylene hollow microfiber was continuously produced by using a carbon dioxide (CO₂) laser‐thinning method. To prepare the hollow microfiber continuously, the apparatus used for the thinning of the solid fiber was improved so that the laser can circularly irradiate to the hollow fiber. Original hollow fiber with an outside diameter (OD) of 450 μm and an internal diameter (ID) of 250 μm was spun by using a melt spinning machine with a specially designed spinneret to produce the hollow fiber. An as‐spun hollow fiber was laser‐heated under various conditions, and the OD and the ID decreased with increasing the winding speed. For example, when the hollow microfiber obtained by irradiating the CO₂ laser to the original hollow fiber supplied at 0.30 m min^?1 was wound up at 800 m min^?1, the obtained hollow microfiber had an OD of 6.3 μm and an ID of 2.2 μm. The draw ratio calculated from the supplying and the winding speeds was 2667‐fold. The hollow microfibers obtained under various conditions had the hollowness in the range of 20–30%. The wide‐angle X‐ray diffraction patterns of the hollow microfibers showed the existence of the highly oriented crystallites. Further, the OD and ID decreased, and the hollowness increased by drawing hollow microfiber obtained with the laser‐thinning. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 102: 2600–2607, 2006     

Application of CO2 laser heating zone drawing and zone annealing to nylon 6 fibers

Nlon 6 fibers were zone drawn and zone annealed by using a continuous wave carbon dioxide laser to develop their mechanical properties. A laser‐heating zone drawing was carried out under a applied tension of 35.4 MPa at a power density of 9.65 W · cm^?2, and then the zone‐drawn fiber was annealed. A laser‐heating zone annealing was carried out in two steps at a power density of 9.65 W · cm^?2; the first step was carried out under 423 MPa and the second under 517 MPa. The treating temperature of the fiber heated by the CO₂ laser was measured by using an infrared thermographic camera equipped with a magnifying lens. The treating temperature at the zone drawing is 138°C, and those at the first and the second zone annealing are 121 and 125°C, respectively. The second laser‐heated zone‐annealed fiber has a birefringence of 65.2 × 10^?3, a degree of crystallinity of 54%, and a storage modulus of 21 GPa at 25°C. Wide‐angle X‐ray diffraction patterns for the laser‐heated zone‐drawn and the zone‐annealed fibers show (200) reflection and (002/202) doublet due to only an α form on the equator. The laser‐heated zone‐drawn fiber has a melting endotherm peaking at 216°C and a trace of shoulder on the higher temperature side of its peak, and the laser‐heated zone‐annealed fibers have a single melting endotherm peaking at 216°C. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 83: 1711–1716, 2002     

Studies on the nuclear magnetic resonance spectra of olefinic protons of conjugated fatty acid methyl esters

The NMR spectra of olefinic protons in the four representative conjugated fatty acid methyl esters, methylcis-9,trans-11-octadecadienoate, methyltrans-9,trans-11-octadecadienoate, methyl α eleostearate, and methyl β eleostearate, were studied. The chemical shift of each olefinic proton in these compounds was determined by considering their intramolecular environment. Coupling constants were also obtained as the results of spectral analysis.     

Fate of the chlorine and fluorine in a sub-bituminous coal during pyrolysis and gasification

The fate of the chlorine and fluorine present in a sub-bituminous coal from Indonesia during pyrolysis and gasification has been studied with fixed and entrained bed reactors. The rate profile for HCl evolved in the temperature programmed pyrolysis exhibits the main and shoulder peaks at 480 and 600 °C, respectively. Model experiments and subsequent Cl 2p XPS measurements show that HCl reacts with metal impurities and carbon active sites at 500 °C to be retained as inorganic and organic chlorine forms, from which HCl evolves again at elevated temperatures. It is suggested that the HCl observed in the coal pyrolysis may originate from the above-mentioned chlorine functionalities formed by secondary reactions involving the nascent char. In the CO₂ gasification of the 900 °C char at 1000 °C and 2.5 MPa, any measurable amounts of HCl and HF could not be detected even at a high conversion of 75 wt% (daf), suggesting the accumulation of these halogens in the residual char. When the coal is injected into an O₂-blown, entrained bed gasifier at 1200-1400 °C under 2.6 MPa, the partial oxidation proceeds to a larger extent at a higher O₂/coal ratio, whereas the chlorine and fluorine are enriched in the remaining char, and the extent of the enrichment at the latter stage of gasification is larger with the fluorine. The XPS measurements of the chars reveal the presence of the broad F 1 s peak, which can cover a wide range of binding energies attributable to inorganic and organic fluorine. The halogen enrichment during gasification is discussed in terms of secondary reactions of HCl and HF with char.     

Shape memorizing properties of a hydrogel of poly(vinyl alcohol)

Hydrogel prepared by repetitive freezing and thawing of poly(vinyl alcohol) aqueous solution was chemically crosslinked with glutaraldehyde. The chemically crosslinked hydrogel hardly changed its physical appearance, and showed good elasticity and strength as original gel. However, after treating in boiling water, it swelled a little, depending on the condition of the chemical treatment. The melted gel thus obtained showed shape memorizing property, that is, it could firmly hold nearly 200% of strain, keeping its original high elasticity. The strain could be released very quickly (< 1 s) in boiling water, and the gel was suggested to be applied to a new type of gel actuator. X-ray diffraction study revealed that the melted gel does not necessarily reform the physical crosslinks in exactly the same manner as the original gel in the process of shape restoring, but the distribution of the physical crosslinks can be restored as they were. It was suggested that the chemical crosslinks which remember the distribution of the physical crosslinks plays a critical roll in the shape restoring process.     

Decomposition of chlorofluorocarbons on TiO2ZrO2

The decomposition of chlorofluorocarbons (CFCs) in the presence of water was examined over a variety of solid acid catalysts. The TiO₂ZrO₂ catalyst was found to have the highest activity and longest life among the catalysts examined. The activity of the TiO₂ZrO₂ catalysts depended upon the content of TiO₂. At the contents of TiO₂ from 58 to 90 mole%, the TiO₂ZrO₂ catalysts exhibited high activity, and these catalysts were proven to contain TiZrO₄ crystal. From the study of the XRD peak intensity of the TiZrO₄ crystal, it was highest on the TZ-58 which contained 58 mole% of TiO₂, and decreased with increasing the content of TiO₂. Furthermore, the conversion of CFC113 measured at 673 K was highest at TZ-58, and decreased gradually with increasing TiO₂ content. Therefore, the TiZrO₄ crystal influences the activity of decomposition of CFC113. However, the TiO₂ZrO₂ catalyst was gradually deactivated during the reaction due to the elimination of titanium atoms. A good relationship was found between the activity on TiO₂ZrO₂ catalyst and bond energy of CCl in the compounds of chlorofluorocarbons and hydrochlorocarbons, suggesting that the rate controlling step was the cleavage of CCl bond.     

Residual amounts of chlorophylls and pheophytins in refined edible oils

The quantities of chlorophyll (CHL) A and B, and pheophytin (PHY) A and B in 10 kinds of refined edible oils were estimated by the fluorometric method. The results revealed that CHL and PHY were present in commercial edible oils. PHY A showed the highest content at ca. 67% in total pigments. Compositional ratios of CHL and PHY were similar in different kinds of plant oils. Through the analysis of rapessed oils at every refining step, we determined that PHY is not formed during oil refining. In the autoxidation of soybean oils to which various amounts of CHL mixtures had been added, the peroxide value of tested oils increased in proportion to the total chlorophyll content. In addition, the compositional changes of the 4 components during autoxidation were investigated.     

Controlling the familywise error rate in functional neuroimaging: a comparative review

Functional neuroimaging data embodies a massive multiple testing problem, where 100,000 correlated test statistics must be assessed. The familywise error rate, the chance of any false positives is the standard measure of Type I errors in multiple testing. In this paper we review and evaluate three approaches to thresholding images of test statistics: Bonferroni, random field and the permutation test. Owing to recent developments, improved Bonferroni procedures, such as Hochberg's methods, are now applicable to dependent data. Continuous random field methods use the smoothness of the image to adapt to the severity of the multiple testing problem. Also, increased computing power has made both permutation and bootstrap methods applicable to functional neuroimaging. We evaluate these approaches on t images using simulations and a collection of real datasets. We find that Bonferroni-related tests offer little improvement over Bonferroni, while the permutation method offers substantial improvement over the random field method for low smoothness and low degrees of freedom. We also show the limitations of trying to find an equivalent number of independent tests for an image of correlated test statistics.     

Gelation of poly(vinyl alcohol)/phenol/water solutions and gel spinning

The light transmittance of the gels of poly(vinyl alcohol) (PVA)/phenol/water solutions was examined for the entire range of phenol/water content. Excellent transparency was found for the gels with phenol contents of 70–95 vol %. In full consideration of the results for the transparency and melting temperature of the gels and the viscosity and gelation ability of solutions, the PVA solutions of 75 vol % phenol content were selected for the gel spinning. The maximum dynamic moduli of drawn filaments at 25°C (room temperature) were 42 GPa (15x) for atactic PVA and 45 GPa (14x) for syndiotacticity-rich PVA. © 1995 John Wiley & Sons, Inc.