由乙腈一步法制备乙酸丁酯的研究

以丁醇和制备丙烯腈的副产物乙腈为原料 ,采用一步法合成了乙酸丁酯。通过正交实验得到了影响反应的 4种因素。确定了最佳的工艺条件为 :催化剂的量为样品质量的 40 % ;n(CH3CN)∶ n(C4 H9OH) =1∶ 1 .0 5 ;反应温度为 1 0 5℃ ;反应时间为 8h。在此反应条件下 ,乙酸丁酯的收率为 88.8% ,纯度可达 99.5 %。并用气相色谱及红外光谱对产品的纯度进行了表征     

用环境友好催化剂合成丙酸异丁酯的研究

报道了以固载杂多酸盐TiSiW12O40/TiO2为环境友好催化剂，对以丙酸和异丁醇为原料合成丙酸异丁酯的反应条件进行了研究。实验表明：TiSiW12O40/TiO2是合成丙酸异丁酯的良好催化剂，最佳反应条件为：n（醇）：n(酸）=1.2:1，催化剂用量为反应物料总质量的2.0%。反应时间1.0h，反应温度106-125℃，上述条件下，丙酸异丁酯的收率可达79.1%。     

Some factors affecting the electrical properties of carbon-black-loaded butyl rubber during vulcanization

Butyl rubber mixtures loaded with 70 phr general purpose furnace black (GPF) and tetramethyl thiuram disulphide (TMTD)/S as vulcanizing system were prepared. The kinetics of their electrical conductivity development during the vulcanization process were followed by using an especially devised system. It was found that the increase in the electrical conductivity during vulcanization obeys an exponential growth function with time constant τ, which markedly decreases with increasing vulcanization temperature as well as with the efficiency of the vulcanizing system. After completion of the vulcanization process, about 80 min, the samples obtained possess reasonable stability and reproducibility of electrical conductivity.     

溶液中微量甲基异丁基酮的分析方法

研究了微量甲异丁基酮在氟氧铌酸（H2NbOF5)及氟钽酸（H2TaF7)溶液中存在的形式，找到利用碘仿-硫代硫酸钠联合滴定的方法，来标定微量甲基异丁基酮在H2NbOF5及H2TaF7溶液中的含量，本方法在钽铌冶炼过程中操作简便易行且结果重现性好。     

聚氨酯/聚(甲基丙烯酸甲酯-甲基丙烯酸丁酯)互穿聚合物网络聚合物的阻尼性能

采用本体聚合法合成出一系列阻尼性能良好的聚氨酯/聚(甲基丙烯酸甲酯-甲基丙烯酸丁酯)(PU/P(MMA-BMA))互穿聚合物网络(IPN)聚合物,通过动态力学分析方法表征了PU/P(MMA-BMA)IPN聚合物的阻尼性能。探讨了加入催化剂、高温后处理、交联剂用量及PU与P(MMA-BMA)的质量比对PU/P(MMA-BMA)IPN聚合物阻尼性能的影响。实验结果表明,经高温后处理后,以二月桂酸二丁基锡为催化剂、交联剂二乙烯基苯用量(占MMA和BMA的摩尔分数)为1.5%、PU与P(MMA-BMA)的质量比接近1或小于1时,PU/P(MMA-BMA)IPN聚合物具有良好的阻尼性能。     

固体超强酸合成乙酸丁酯

本文讨论了固体超强酸催化剂合成乙酸丁酯的方法，比较了各类固体超强酸的优劣，为工业化生产乙酸丁醋筛选超强酸催化剂提供极具价值的参考依据。     

A Semi‐Batch Process for Nitroxide Mediated Radical Polymerization

Summary: A semi‐batch process using nitroxide mediated polymerization, was explored for the design of low molecular weight solvent‐borne coatings, typical of those used in the automotive industry. While living radical polymerization (LRP) offers many advantages in the control of polymer chain microstructure that may confer important physical and chemical property benefits to coatings, adapting LRP to a semi‐batch process poses significant challenges in the design and operation of the process. Using styrene monomer, various two‐component initiating systems (free radical initiator, 4‐hydroxy‐TEMPO) were studied to understand the effects of different initiators on the course of polymerization. In addition, an alkoxyamine was synthesized and used as the initiating source. The initiators Luperox 7M75 and Luperox 231 give higher polymerization rates and reasonable control over polymerization, while benzoyl peroxide (BPO), Vazo 67, and the alkoxyamine are less effective. The number of polymer chains in the final product is always less than the theoretical value, reflecting poor initiation efficiency, probably resulting from undesirable termination reactions that become important due to the nature of the semi‐batch process. Adding camphorsulfonic acid (CSA) or charging initiator concurrently with monomer during semi‐batch feed, can increase the polymerization rate while maintaining the living character of the polymerization. The copolymerization of styrene and butyl acrylate is also shown to exhibit living character.

Schematic representation of the exchange reaction to produce N‐TEMPO capped polymer chains.     

Ce和La改性固体超强酸S2O82-/ZrO2-SiO2催化剂合成及其酯化性能研究

以Zr(NO₃)₄·5H₂O和Na₂SiO₃·9H₂O为原料,利用共沉淀法制备前驱体,浸渍添加稀土Ce和La,一定温度焙烧后制得掺杂稀土S₂O₈^2-/ZrO₂-SiO₂固体超强酸。通过XRD、FT-IR和SEM对催化剂进行表征,以硬脂酸的酯化合成反应为探针,考察制备条件对催化剂性能的影响以及催化剂的重复使用率。结果表明,相对于未改性的S₂O₈^2-/ZrO₂-SiO₂催化剂,添加了Ce或La的固体超强酸酯化催化活性及重复使用性能均有提高。     

IIR/EPDM共混物的物理机械性能

研究了IIR／EPDM并用体系中共混比、硫磺硫化体系以对共混性能的影响。结果表明，IIR与EPDM相容性较好，而且可以达到共硫化；IIR。EPDM质量比为75／25时，共混物的物理机械性能和老化性能较好；用硫黄、低硫高促进剂和无硫硫化体系都得到性能良好的共混物，其中以前者硫化的共混物性能最为突出。     

Effect of miscibility and forced compatibility on damping properties of CIIR/PAc blend

In this study, a kind of novel damping materials was prepared based on the blend of chlorinated butyl rubber (CIIR) and polyacrylate (PAc) synthesized by different molar ratio of butyl methacrylate and ethyl acrylate. Research results from experiments and analyses by employing DMA, TEM, and FTIR show that whether at a cocured system or noncocured system, it can be achieved to shift a loss peak of CIIR towards a higher temperature region and to keep the damping value from markedlly decreasing, which broadens the effective damping function area of CIIR to the vicinity of ambient temperature. In the former system, the thermodynamical miscibility of CIIR and PAc, to some extent, is predominated by the molecular design of PAc, while in the latter system, covulcanized networks play a more significant role in improving compatibility and abating the peak split, though the suppression effect of thermal stress on the transition of CIIR T_ll transition still can not be neglected. Furthermore, transition state derived from the cocuring CIIR and PAc cannot make the phase separation completely take place, and consequently results in the deformation of phase morphology of the cocured CIIR/PAc blend. It is the influence of thermodynamics miscibility and forced compatibility in different size that makes the suppression effect of foreign PAc on CIIR T_ll transition be controllable. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 102: 3127–3133, 2006