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1.
The crystallization behavior of well-defined star-shaped cubic silsesquioxane-poly(ethylene oxide) (CSSQ-PEO) and linear PEO were studied in terms of differential scanning calorimetry (DSC) and wide-angle X-ray scattering (WAXS). It was found in DSC analysis that the glass transition temperature (Tg) and the crystallization temperature (Tc) of CSSQ-PEO are different from those of linear PEO. The presence of CSSQ in PEO reduced the overall crystallization growth rate. This effect can be ascribed to the reduction of the mobility of the PEO crystallites in the presence of CSSQ and the star structure of the polymer. The Ozawa method is qualitatively satisfactory for describing the nonisothermal crystallizations of linear PEO and CSSQ-PEO. The presence of CSSQ leads to the diffusion- and nucleation-controlled mechanisms in the crystallization process of CSSQ-PEO whilst only the nucleation-controlled mechanism was observed in the case of linear PEO. The apparent activation energy required for crystallization was calculated using the Kissinger method. The isothermal crystallization morphology of PEO and CSSQ-PEO were also examined by cross-polarizing optical microscopy (CPOM). The CPOM images indicated the spherulite growth is slower in CSSQ-PEO as compared to linear PEO. It was also investigated that more number of PEO spherulites in CSSQ-PEO were observed, which sizes are markedly smaller than the spherulites developed in linear PEO. Wide-angle X-ray scattering (WAXS) studies showed that the crystallization peaks for linear PEO and CSSQ-PEO appeared at different temperature revealing the crystallization process and crystal growth rate are different from each other. However, no significant distortion of the crystal structure of PEO was evaluated in the presence of CSSQ. 相似文献
2.
A ternary blend system comprising poly(cyclohexyl methacrylate) (PCHMA), poly(α‐methyl styrene) (PαMS) and poly(4‐methyl styrene) (P4MS) was investigated by thermal analysis, optical and scanning electron microscopy. Ternary phase behaviour was compared with the behaviour for the three constituent binary pairs. This study showed that the ternary blends of PCHMA/PαMS/P4MS in most compositions were miscible, with an apparent glass transition temperature (Tg) and distinct cloud‐point transitions, which were located at lower temperatures than their binary counterparts. However, in a closed‐loop range of compositions roughly near the centre of the triangular phase diagram, some ternary blends displayed phase separation with heterogeneity domains of about 1 µm. Therefore, it is properly concluded that ternary PCHMA/PαMS/P4M is partially miscible with a small closed‐loop immisciblity range, even though all the constituent binary pairs are fully miscible. Thermodynamic backgrounds leading to decreased miscibility and greater heterogeneity in a ternary polymer system in comparison with the binary counterparts are discussed. © 2003 Society of Chemical Industry 相似文献
3.
Birong Zeng Kaibin He Haiyang Wu Jianyu Ye Xianghong Zheng Weiang Luo Yiting Xu Conghui Yuan Lizong Dai 《大分子材料与工程》2021,306(6):2100012
A zirconium hybrid polyhedral oligomeric silsesquioxane derivative (Zr–POSS–bisDOPO) is synthesized by the corner-capping and Kabachnik–Fields reactions. It is characterized by Fourier transform infrared spectroscopy (FTIR) and nuclear magnetic resonance spectroscopy (NMR), and then used as a flame retardant in diglycidyl ether of bisphenol A (DGEBA) to endow epoxy resin (EP) with flame retardancy. The flame retardancy, thermal stability, and mechanical properties of the cured EP/Zr–POSS–bisDOPO composites are investigated. The results show that when Zr–POSS–bisDOPO is added by 5–7 wt%, the EP/Zr–POSS–bisDOPO composites pass the UL-94 V-0 rating test. In addition, they have a better flame-retardant effect than pure EP. The combination of Zr atom embedded in the Si O cubic cage and the two phosphaphenanthrene substituent groups in one corner of cubic cage is expected to realize the Zr/Si/P ternary intramolecular hybrid synergistic effect and achieve the possibility of dispersing metal–POSS cages at a sub-micrometer-scale level into polymer matrix. It also proves that Zr–POSS–bisDOPO produces phosphorus-containing free radicals and terminates the chain reactions in gas phase. Meanwhile the Si O Si and Zr O units are retained in the solid phase, which promote the char formation and enhance the flame retardancy. This kind of Zr-doped POSS will be helpful for developing the new metal–POSS hybrid flame-retardant and polymer composites. 相似文献
4.
The poly(styrene‐co‐octavinyl‐polyhedral oligomeric silsesquioxane) (PS–POSS) organic–inorganic hybrid nanocomposites containing various percent of POSS were prepared via one‐step free radical polymerization and characterized by FTIR, high‐resolution 1H NMR, 29Si NMR, GPC, DSC, and TGA technologies. The POSS contents in these nanocomposites were determined using FTIR calibration curve. The result shows that the POSS contents in nanocomposites can be tailored by varying the POSS feed ratios. On the basis of the POSS contents in the nanocomposites and the 1H NMR spectra, the number of reacted vinyl groups of each octavinyl‐POSS macromonomer were calculated to be 6–8. DSC and TGA measurements indicate that the incorporation of POSS into PS homopolymer can apparently improve the thermal properties of the polymeric materials. The dramatic Tg and Tdec increases are mainly due to the formation of star and low cross‐linking structure of the nanocomposites, where POSS cores behave as the joint points and hinder the motion and degradation of the polymeric chains. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 2007 相似文献
5.
Theresa E. Gentle Alan R. Bassindale 《Journal of Inorganic and Organometallic Polymers》1995,5(3):281-294
We have recently reported the synthesis of octopus molecules of defined shape and size with molecular weights well into the thousands. These octopus molecules were made by placing eight pendant groups symmetrically about a central silsesquioxane core via the H2PtCl6 catalyzed hydrosilylation of 1-alkenes as well as vinyl- and allyl-siloxanes by T8 hydrogen silsesquioxane, (HSiO32)8. The chemistry of addition was studied and it was found that while the addition of the 1-alkenes to T8 was regioprecise with only -addition being observed, both - and -addition occurred with vinyl-siloxane. In addition, H-vinyl exchange on silicon was observed to occur with addition of vinyl-siloxane to T8. In the current studies, the effect of the hydrosilylation catalyst. homogeneous and heterogeneous, on the regioselectivity of addition and on the extent of exchange on silicon was evaluated. It was found that the heterogeneous catalysts Pt–C, sulfided Pt–C, and Rh–C required higher temperature and longer times to get complete reaction than the homogeneous catalysts. H2PtCl6 and the tetramethyldivinyldisiloxane complex of Pt. Pd supported catalysts were not effective catalysts for this hydrosilylation. The extent of exchange on silicon and the degree of the second mode of addition occurring were higher with the heterogenous catalysts and may be a result of the higher reaction temperatures. 相似文献
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8.
微波辐射对甲苯磺酸催化合成乙酸环己酯 总被引:15,自引:0,他引:15
以冰醋酸和环己醇为原料 ,环已烷为带水剂 ,对甲苯磺酸作催化剂 ,采用微波辐射技术 ,在常压下直接合成乙酸环己酯。最适宜反应条件为 :n(环己醇 )∶n(乙酸 ) =1 5∶1 0 ,对甲苯磺酸用量 0 2 0 g ,带水剂用量 5mL ,微波功率 5 95W ,辐射时间 15min ,产率达 97%以上 相似文献
9.
The phase behavior and motional mobility in binary blends of polystyrene (PS) and poly(cyclohexyl methacrylate) (PCHMA) have been investigated by solid state 13C NMR techniques. The blend miscibility has been studied by examining the 1H spin-relaxation times in the laboratory frame (T1H) and in the rotating frame (T1ρH) for the PCHMA/PS blends with various compositions and pure components. The T1ρH results show that PCHMA and PS are intimately mixed at the molecular level within the blends at all compositions. In addition, according to the results of carbon T1ρ relaxation time measurements, we conclude that mixing is intimate enough to cause a reduction in local chain mobility for PS, but an increase in side chain mobility for PCHMA. 相似文献
10.