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131.
采用溶胶-凝胶法,将聚(苯乙烯-co-丙烯酸)(PSA)膜材料和氯化镁的复合物包覆在以硅胶为载体的TiCl3催化剂上,负载TiCl4后制得Ziegler-Natta复合催化剂.采用红外光谱、激光粒度仪和扫描电镜对催化剂进行了表征,结果表明该复合催化剂呈核壳结构.同时,考察了复合催化剂中膜的厚度和反应中的氢气含量对催化剂的聚合活性和聚乙烯性能的影响,实验发现,膜厚约为3μm的核壳结构复合催化剂活性良好,其具有带诱导期的平稳型动力学曲线;膜厚1.5μm的复合催化剂的活性接近于实验所用的以硅胶为载体的TiCl3催化剂,且其具有相似的衰减型动力学曲线.研究同时表明,不同的膜厚能够调节复合催化剂的氢调性能及所得聚乙烯的分子量分布. 相似文献
132.
133.
Li Li Wang XiaochunWei xiantao Chen YonghuGuo Changxin Yin Min 《Physica B: Condensed Matter》2011,406(3):609-613
Lutetium oxide nanopowders codoped with Tm3+ and Yb3+ were synthesized by the reverse-strike co-precipitation method. Effects of precipitant solution pH on the structural, morphological and upconversion luminescent properties of Lu2O3:2%Yb, 0.2%Tm nanopowders had been investigated. The results show that pH value of the precipitant (NH4HCO3) solution has a significant effect on the particle size, morphology and upconversion emission intensity of the Lu2O3:2%Yb, 0.2%Tm nanopowders. All the samples obtained from different pH value of precipitant solution can be readily indexed to pure cubic phase of Lu2O3, indicating good crystallinity. The upconversion emission intensity of Lu2O3:2%Yb, 0.2%Tm nanopowders obtained from the precipitant solution with pH=11 is the strongest. The enhancement of the upconversion luminescence is suggested to be the consequence of reducing the number of OH− groups and the enlarged nanopowder size. The strong blue, weak red and near infrared emissions from the prepared nanopowders were observed under 980 nm laser excitation, and attributed to the 1G4→3H6, 1G4→3F4 and 3H4→3H6 transitions of Tm3+ ion, respectively. 相似文献
134.
C. Martos B. Coto J.L. Peña R. Rodríguez D. Merino-Garcia G. Pastor 《Journal of Crystal Growth》2010,312(19):2756-2763
The deposition of inorganic salts (“scales”) such as calcium carbonate is an important flow assurance problem during crude oil production. The knowledge of the features of the precipitated solids, mainly the particle size and morphology, is crucial to understand the nature of the solids and to avoid or reduce the effect of their deposition. For instance, the use of additives is one of the most usual procedures to mitigate this problem. Additives interact with scale-forming substances either by increasing the induction time, or by inhibiting crystal growth, changing the morphology of solids. 相似文献
135.
Emil Byström Anna Nordborg Fredrik Limé Ngoc Phuoc Dinh Knut Irgum 《Journal of separation science》2010,33(11):1563-1570
A combined surface activation and “grafting to” strategy was developed to convert divinylbenzene particles into weak cation exchangers suitable for protein separation. The initial activation step was based on plasma modification with bromoform, which rendered the particles amenable to further reaction with nucleophiles by introducing Br to a surface content of 11.2 atom‐%, as determined by X‐ray photoelectron spectroscopy. Grafting of thiol‐terminated glydicyl methacrylate telomers to freshly plasma activated surfaces was accomplished without the use of added initiator, and the grafting was verified both by reduction in bromine content and the appearance of sulfur‐carbon linkages, showing that the surface grafts were covalently bonded. Following grafting the attached glydicyl methacrylate telomer tentacles were further modified by a two‐step procedure involving hydrolysis to 2,3‐hydroxypropyl groups and conversion of hydroxyl groups to carboxylate functionality by succinic anhydride. The final material was capable of baseline separating four model proteins in 3 min by gradient cation exchange chromatography in a fully aqueous eluent. 相似文献
136.
间接原子吸收光谱法测定氢溴酸山莨菪碱 总被引:3,自引:0,他引:3
研究了原子吸收光谱法间接测定氢溴酸山莨菪碱。在溶液pH为 5 1~ 5 3,当四苯硼钠过量时可完全沉淀氢溴酸山莨菪碱 ;加入过量的氯化钾沉淀滤液中剩余的四苯硼钠 ;干过滤 ,用原子吸收分光光度计在76 6 5nm波长下测定滤液中过量的钾 ,因四苯硼钠与氢溴酸山莨菪碱和氯化钾均按 1∶1的计量关系生成沉淀 ,可以直接计算得到氢溴酸山莨菪碱的含量。对氢溴酸山莨菪碱注射液进行了测定 ,测定结果准确。方法简单快速 ,回收率在 96 %~ 10 3%之间 ,相对标准偏差为 1 4 %。该方法可进一步推广原子吸收光谱法在其他相关药物测定方面的应用。 相似文献
137.
The behavior of copper precipitation in cast multicrystalline silicon (mc-Si) annealed at different temperatures under air cooling (30 K/s) or slow cooling (0.3 K/s) was investigated by scanning infrared microscopy (SIRM). Comparing to Czochralski-grown silicon (Cz-Si), copper precipitated more easily in mc-Si, and the lowest temperature of copper precipitation in mc-Si was about 700 °C, lower than that in Cz-Si. It was also observed that copper preferably precipitated on grain boundaries so that near the grain boundaries the denuded zone formed. The results indicate that the defects including dislocations, grain boundaries and microdefects, as the heteronucleation sites, enhanced copper precipitation. Moreover, cooling rates had a great influence on the copper precipitation, especially at lower annealing temperatures. Generally air cooling led to the formation of high density of copper-precipitate colonies. 相似文献
138.
Preparation of a novel molecularly imprinted polymer for the highly selective extraction of baicalin
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The selective extraction of baicalin is important to its quality control especially when the matrices are complicated. In this work, a novel molecularly imprinted polymer was prepared for the selective extraction of baicalin in herbs. The molecularly imprinted polymer was synthesized by the copolymerization of 4‐vinyl pyridine and ethylene glycol dimethacrylate in the presence of baicalin by a precipitation polymerization method. After the optimization of parameters for molecularly imprinted polymer preparation, including the functional monomer, porogen, sampling solvent, and washing solvent, good selectivity was obtained, with an imprinting factor of about 4, which is much better than that achieved by the bulk‐polymerization method. The performances of the prepared molecularly imprinted polymers were systematically investigated, including adsorption kinetics, isotherm experiment, and Scatchard analysis. On the basis of the good adsorptive capability of the prepared molecularly imprinted polymer, it was also applied for the pretreatment of baicalin in Scutellaria baicalensis Georgi. The result showed that most of the matrices were removed and baicalin was selectively enriched. 相似文献
139.
Shaohong Zhou Liang Yuan Xin HuaAuthor Vitae Lingling XuAuthor VitaeSongqin Liu 《Analytica chimica acta》2015
Demand is increasing for ultrasensitive bioassays for disease diagnosis, environmental monitoring and other research areas. This requires novel signal amplification strategies to maximize the signal output. In this review, we focus on a series of significant signal amplification strategies based on polymeric nanocomposites and polymerization. Some common polymers are used as carriers to increase the local concentration of signal probes and/or biomolecules on their surfaces or in their interiors. Some polymers with special fluorescence and optical properties can efficiently transfer the excitation energy from a single site to the whole polymer backbone. This results in superior fluorescence signal amplification due to the resulting collective effort (integration of signal). Recent polymerization-based signal amplification strategies that employ atom transfer radical polymerization (ATRP) and photo-initiated polymerization are also summarized. Several distinctive applications of polymers in ultrasensitive bioanalysis are highlighted. 相似文献
140.
Marcin Konkol Tetsuya Kohno Tatsuya Miyatake 《Journal of organometallic chemistry》2011,696(9):1792-2956
The tetradentate [OSSO]-type bis(phenol) ligands, [{2,2′-(HOC6H2-4,6-R2)2CH2SCH2CH2SCH2}] (R = tBu, 2; Br, 3) react with MBz4 (M = Zr, Hf) to yield the corresponding dibenzyl complexes, [M{2,2′-(OC6H2-4,6-R2)2CH2SCH2CH2SCH2}Bz2] (R = Br, M = Zr, 4Br; Hf, 5Br; R = tBu, M = Hf, 5) in a good to very good yield. Zirconium diamido complexes, [Zr{2,2′-(OC6H2-4,6-R2)2CH2SCH2CH2SCH2}(NMe2)2] (R = tBu, 6; Br, 6Br) were prepared in a reaction of the corresponding disodium salt of 2 or 3 generated in situ with ZrCl2(NMe2)2(THF)2. Heating of 6 with TMSCl at 35 °C afforded zirconium dichloro complex, [Zr{2,2′-(OC6H2-4,6-tBu2)2CH2SCH2CH2SCH2}Cl2] (7), whereas the titanium analog 8 was prepared in a direct reaction with TiCl4. While for complexes 4Br, 5, 5Br, 6, 6Br and 7 single C2-symmetric isomers were observed in solution at room temperature, as revealed by the NMR spectroscopic data, titanium complex 8 formed as a mixture of cis-α (8a) and cis-β (8b) isomers in a ratio of approx. 20:80% (measured in CD2Cl2). The VT NMR studies revealed a reversible conversion of 8a into 8b above 60 °C. The X-ray crystal structure determination of complexes 4Br, 5Br and 7 confirmed their C2-symmetrical configuration in the solid state with cis-arranged benzyl/chloro groups and the trans-coordination of two bulky phenolato moieties. The zirconium dibenzyl complexes exhibit good catalytic activities in homopolymerization of 1-hexene (atactic poly(1-hexene), PDI = 1.5-1.7) and vinylcyclohexane (isotactic poly(vinylcyclohexane), PDI = 1.2-1.8) upon activation with a co-catalyst. In both polymerizations no increase of activity was observed for the complex 4Br with electron-withdrawing substituents on phenolate rings. Moreover, polymerization of liquid propylene catalyzed by the titanium dichloro isomeric mixture 8 afforded at 5 °C ultrahigh molecular weight atactic/isotactic polypropylene mixtures. 相似文献