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181.
Toshimitsu Ichimori Shinichi Yamazaki Kunio Kimura 《Journal of polymer science. Part A, Polymer chemistry》2011,49(21):4613-4617
The influence of shear flow, especially the timing for the application of shearing, was examined to enhance the selectivity for the preparation of poly(p‐oxybenzoyl) (Pp‐OB) by using hydrodynamically induced phase separation during polymerization of 4‐(4‐acetoxybenzoyloxy)benzoic acid (p‐ABAD) and m‐acetoxybenzoic acid (m‐ABA). The polymers containing few m‐oxybenzoyl (m‐OB) moieties were obtained as precipitates even at high content of m‐OB moiety in feed (χf) under shear flow. The content of m‐OB moiety in the precipitates (χp) prepared under shearing throughout the polymerization at the shear rate (γ) of 489 s?1 was 6.3 mol % even at χf of 60 mol %. Especially, the Pp‐OB was obtained as the precipitates at χf of less than 50 mol %. The timing of the application of the shearing influenced the selectivity significantly, and the shearing just after the precipitation of the oligomers started was quite efficient to enhance the selectivity more. The χp of the precipitates prepared with shearing at γ of 489 s?1 just after the precipitation was only 3.9 mol % even at χf of 60 mol %. The shear flow reduced the difference in the reactivity between p‐ABAD and m‐ABA, resulting in the decrease in the selectivity with regard to the formation of p‐oxybenzoyl homo‐oligomer. However, the shear flow enhanced the difference in the miscibility between homo‐oligomers and co‐oligomers. This change in the miscibility by shear flow brought about the more rapid precipitation of homo‐oligomers, leading to the enhancement of the selectivity. © 2011 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem, 2011 相似文献
182.
Masahiro Kihara Shin‐Ichiro Kohama Shota Umezono Kanji Wakabayashi Shinichi Yamazaki Kunio Kimura 《Journal of polymer science. Part A, Polymer chemistry》2011,49(5):1088-1096
Poly(p‐oxybenzoyl) (POB) crystals were prepared by reaction‐induced crystallization during direct polymerization of p‐hydroxybenzoic acid in the presence of boronic anhydrides. Polymerizations were carried out at 300 °C in dibenzyltoluene at a concentration of 1% with three kinds of anhydrides of boronic acid such as 3,4,5‐trifluorophenylboronic acid (TFB), 4‐methoxyphenylboronic acid (MPB) and 4‐biphenylboronic acid (BPB). The POB crystals were formed as precipitates in the solution and the morphology was considerably influenced by both the structure of the boronic anhydride and its concentration (cB). Needle‐like crystals were firmed in the presence of TFB anhydride (TFBA) at cBs of 5 and 10 mol % by the spiral growth of lamellae. Spherical aggregates of slab‐like crystals were formed at cBs from 50 to 100 mol %. The polymerization with MPB anhydride and BPB anhydride (BPBA) also yielded the needle‐like crystals at cBs of 50 and 5 mol %, respectively. The polymerization with TFBA at lower cB was favorable to prepare the needle‐like crystal. Molecular weight was also influenced by the structure of the boronic anhydride and cB. Mn increased generally with cB and BPBA gave the highest Mn of 14.7 × 103 at cB of 100 mol %. The loose packing of the molecules in the crystal caused by the bulkiness of the end‐groups made the polymerization in the crystals more efficiently. Morphology and molecular weight of the POB crystals could be controlled by the chemical structure and the content of boronic anhydride. © 2010 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem, 2011. 相似文献
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The electrophoretic detection of two kinds of p-quinone anion radicals arising from the electrolysis of benzoquinone and chloranil was achieved by employing an acetonitrile medium. Sufficient dehydration of a running solution was necessary for the detection of the benzoquinone anion radical. Oxygen in the running solution also caused a serious decrease in the amount of the benzoquinone anion radical during electrophoresis. The addition of methanol as a hydrogen-donor decreased the electrophoretic mobility of the benzoquinone anion radical significantly, while that of the chloranil anion radical was little changed. This result is interpreted in terms of hydrogen-bonding interaction between the p-quinone anion radicals and methanol, reflecting the magnitude of their proton-accepting ability (benzoquinone anion radical > chloranil anion radical). 相似文献
186.
Toshinobu Kanai Hiroki Ishibashi. Yoshikazu Hayashi Kunio Oka Takaaki Dohmaru Tatsuo Ogawa Shoji Furukawa Robert West 《Journal of Polymer Science.Polymer Physics》2001,39(11):1085-1092
The thermochromic behavior of poly(di‐n‐octylsilane) {[Si(C8H17)2]n; PDOS} was studied by ultraviolet (UV) absorption, differential scanning calorimetry, and X‐ray diffraction measurements. The structure of PDOS in the low‐temperature phase strongly depended on not only the temperature but also the rate of cooling, that is, the thermal history. Temperature‐dependent UV absorption spectra were highly dependent on thermal hysteresis. Cooled rapidly (10 K/min), PDOS showed two absorption peaks at 3.32 and 3.51 eV in low‐temperature‐ordered phases, whereas a single absorption peak at 3.32 eV became predominant with slow cooling (0.3 K/min). The appearance of the two peaks at low temperatures suggested that a mixture of different conformations was introduced by rapid cooling. A fiber diffraction pattern measured at 240 K after rapid cooling also showed evidence of the existence of novel conformation. A temperature‐dependent powder X‐ray diffraction pattern changed significantly between 270 and 280 K. Rapid cooling reduced the intensity of the X‐ray diffraction peak in this temperature region. This intensity change was explained by the conformational mixture in the polymer. © 2001 John Wiley & Sons, Inc. J Polym Sci B: Polym Phys 39: 1085–1092, 2001 相似文献
187.
K. Araki T. Yoshikawa I. Ishii T. Goto H. Tanida B. Lüthi 《Physica B: Condensed Matter》2009,404(19):3187-3190
We performed ultrasonic measurements on a single crystal of PrMg3. The characteristic Curie-type softening was observed in temperature dependence of transverse mode (C11-C12)/2 below 8 K down to 0.8 K. This softening in PrMg3 is caused by a non-Kramers Γ3 doublet ground state having electric quadrupoles Ou and Ov and magnetic octupole Txyz. The elastic constant (C11-C12)/2 shows a minimum at 25 K, which cannot be explained by the quadrupole susceptibility based on the crystal electric field (CEF) levels. However, considering higher order (l=4) multipole, namely electric hexadecapole, the minimum around 25 K was well reproduced. At lower temperatures, a shoulder anomaly in elastic constant being deviated from the Curie-type softening was observed around 100-800 mK in (C11-C12)/2. This anomaly is unaffected by magnetic fields up to 14 T. 相似文献
188.
A 5-amino-8-hydroxyquinoline (AHQ)-modified gold nanoparticle (GNP) layer was fabricated on an inner wall of a silica capillary column by alternatively passing a citrate-stabilized GNP solution and an AHQ solution in a repeating fashion. The observations by a field emission scanning electron microscope showed that the thickness of the resulting GNP layer was about 0.15 microm. This column was then used as an open tubular solid-phase extraction column for cadmium, followed by electrothermal atomic absorption spectrometric determination. The detection limit of 0.009 ng ml(-1) was obtained. 相似文献
189.
Total synthesis of fumitremorgin B 总被引:2,自引:0,他引:2
Total synthesis of fumitremorgin B, one of the potent tremorgic mycotoxins, was achieved in 7 steps. 相似文献
190.
Norihiro Kobayashi Pi Sun Yayoi Fujimaki Toshifumi Niwa Tadashi Nishio Junichi Goto Hiroshi Hosoda 《Analytical sciences》2002,18(12):1309-1314
Measurement of cortisol levels in body fluids is important for monitoring pituitary gland and adrenal functions. To develop a specific and standardized enzyme-linked immunosorbent assay (ELISA), a novel monoclonal anti-cortisol antibody has been generated using a reasonably designed haptenic derivative. Spleen cells were prepared from the BALB/c or A/J mouse, which had repeatedly been immunized with a conjugate of 4-(2-carboxyethylthio)cortisol (CET) and bovine serum albumin, to be fused with P3/NS1/1-Ag4-1 myeloma cells. After four fusion experiments, one hybridoma clone secreting a practical antibody has been established. The resulting monoclonal antibody CS#38 (isotype gamma1, kappa) showed an affinity constant (K(a)) for cortisol of 1 x 10(9) M(-1) and provided a practical calibration curve (detection limit, 0.26 ng per assay) in a homologous ELISA system employing horseradish peroxidase-labeled CET as a labeled antigen. Cross-reactivities with related C-21 steroids were acceptably low: 11-deoxycortisol (4.3%), cortisone (4.0%), corticosterone (1.9%), progesterone (1.6%), 17alpha-hydroxyprogesterone (12%), 6beta-hydroxycortisol (8.4%), and tetrahydrocortisol (< 0.1%). Urinary and serum cortisol levels of healthy volunteers were determined by this method after methylene chloride extraction to be 39.0 +/- 17.0 microg/day (n = 7) and 80.8 +/- 38.9 ng/mL (n = 10), respectively, both of which are in the reference range. 相似文献