反相高效液相色谱法测定meso-四苯基卟啉钴的纯度

采用反相高效液相色谱法测定合成meso-四苯基卟啉钴的纯度;以甲醇乙腈二氯甲烷(体积比为55∶35∶10)为流动相,ShimpackCLCODS柱(150mm×6.0mmi.d,5μm)为分离柱,流速为1.5mL/min,检测波长420nm;meso四苯基卟啉钴的测定在1.0～10μg/mL时线性关系良好(相关系数r=0.9993),加标回收率为97.03%～101.42%,重复进样的相对标准偏差RSD为0.64%～2.92%(n=5)。方法的准确度高,精密度好,实际应用效果好。     

Propylene epoxidation in a microreactor with electric heating

Gas phase propylene epoxidation on gold catalysts has attracted wide attention from industry and academia due to its high selectivity. However, it suffers from low propylene conversion and rapid catalyst deactivation. Experiments showed that propylene conversion could be increased by raising H₂, O₂, or C₃H₆ concentration in the feed, but the feed compositions were within the explosion limit. It was also shown that the activity of the used catalyst could be fully recovered, but the regeneration temperature was 280 °C, much higher than that for reaction. Therefore a microchannel reactor was devised to suppress explosion and was constructed with Fecralloy, to raise the temperature rapidly for catalyst regeneration by electric heating. In two minutes the temperature of the reactor could be raised from 50 to 300 °C. Catalysts were coated on the alloy belt by dip coating, and the performance of the reactor was evaluated under different operating conditions. Results showed that in the microreactor the overall reaction rate was controlled mainly by the intrinsic reaction rate, and also influenced by film diffusion to a certain extent. The deactivated catalyst was regenerated in the microchannel reactor and the activity was fully recovered.     

Voidage characteristics and prediction of bed expansion in liquid-solid inverse fluidized bed

Studies on voidage fluctuations, axial voidage profile and bed expansion are carried out by measuring the local void fraction using particles of wide ranging characteristics in liquid-solid inverse fluidized bed. The quality of fluidization is elucidated by the local voidage fluctuations. The RMS voidage fluctuation depicts a maximum with respect to average bed void fraction and increases with increase in Archimedes number. The fluidization quality has been quantified using average normalized RMS voidage fluctuation in terms of Transition number. The axial void fraction is almost uniform throughout the bed except for particles with size distribution. All the literature and present experimental data on bed expansion are unified in terms of Richardson and Zaki equation using experimental terminal velocities. A new correlation is proposed for predicting the wall effect corrected experimental terminal velocities, as a substitute for standard drag equation. The bed expansion data are also predicted using the drift flux model.     

低密度泡沫玻璃的研究与应用

低密度泡沫玻璃是利用碎玻璃制造的一种气孔率大于90%的隔热保温材料,它具有强度高、导热系数小、吸水率低、不吸湿、耐腐蚀等特性,在潮湿环境下抗冻性能好,是一种优良的低温、超低温隔热保温材料。该产品用途广泛,所用的原材料简单易得,但生产工艺过程比较复杂,生产过程控制精度要求较高,容易产生各种缺陷而影响产品的质量。本文对低密度泡沫玻璃的生产工艺过程进行详细的分析研究,提出相应的措施,确保产品的低密度和高成品率,提高产品的性能,扩大产品的使用范围。     

近十年常温干法精脱硫专利技术发展动态

收集了近十年来国内的常温干法精脱硫专利，并分类列举出各种脱硫剂的物化性质和几种常温精脱硫工艺，重点阐述了该技术的优缺点及其未来发展方向。     

美国能源部的浆态床F－T合成技术

浆态床Ｆ－Ｔ合成技术是美国能源部Ｆ－Ｔ合成技术的主要开发项目。本文就浆态相Ｆ－Ｔ合成催化剂的开发、中试示范实验和浆态反应器的化工基础研究作一扼要的介绍。     

喷动床反应模型的研究进展

喷动床是一种可实现热量重复循环的高效反应器 .介绍了目前喷动床研究中出现的各种反应模型 ,从等温和非等温两个方面讨论了一维轴向、流管、半分割和流动反应耦合等各类模型的基本思想和理论及各自的特点 ,并提出了进一步发展的方向 .     

High temperature polymerization of propylene catalyzed by MgCl2‐supported Ziegler–Natta catalyst with various cocatalysts

Four cocatalysts, referred to as ethylaluminoxanes, were synthesized by the reaction between triethylaluminium (AIEt₃) and water under various molar ratios of H₂O/Al at ?78°C. Aluminoxanes were used as cocatalysts for a MgCl₂‐supported Ziegler–Natta catalyst for propylene polymerization at temperatures ranging from 70 to 100°C. When the polymerization was activated by AlEt₃, the activity as well as the molecular weight and isotacticity of the resulting polymer gradually dropped as the temperature varied from 70 to 100°C. When ethylaluminoxane was employed as the cocatalyst, good activity and high molecular weight and isotacticity were obtained at 100°C. Furthermore, when the cocatalyst varied from AlEt₃ to ethylaluminoxane, the atactic fraction and polymer fraction with moderate isotacticity decreased and the high isotactic fraction slightly increased, which indicated that the variation of the cocatalyst significantly affects the isospecificity of active sites. It was suggested that the reactivity of the Al‐Et group and the size of the cocatalyst were correlated to the performance of the Ziegler–Natta catalyst at different temperatures. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 100: 1978–1982, 2006     

Effect of Twin-Plane Reentrant Edge on the Coarsening Behavior of Barium Titanate Grains

When BaTiO₃ ceramics were sintered at relatively low temperatures (≤1250°C), the grains with reentrant edges caused by a (111) double twin grew exclusively. As a result, a microstructure with a bimodal grain-size distribution composed of platelike large grains and fine matrix grains was obtained. In contrast, at the usual sintering temperature between 1250° and 1350°C, grains containing a (111) double twin did not exhibit any growth advantage. In this case, a coarse and uniform microstructure was obtained. When this coarse-grained specimen was further heat-treated at 1365°C, the grains possessing a double twin were observed to grow exclusively again. The results were explained in terms of a coarsening process controlled by two-dimensional nucleation.