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Novel tubing microreactor for monitoring chemical reactions

机译:新型管道微反应器,用于监测化学反应

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There is an expanding interest in small-scale methods to evaluate catalysts and chemical reactions at a variety of conditions, ranging up to 6.9 MPa (1000 psig) and 300 degreesC. Multiwell parallel batch techniques are most commonly applied in high-throughput screening systems. In contrast, we describe here a rapid, serial, highly controllable method based on LC-type steel tubing rated for high pressures. The tube, containing a variety of flowing ingredients, such as carrier solvents, catalyst formulations, and reactants, is self-heated ohmically using electrical current from a power supply monitored and regulated with a precision of 0.01%. An array of voltage taps arranged along its length serves to sense the real-time temperature profile of the tube. Reactions are seen as temperature pulses progressing through the reactor, in zones of 200 muL each, and tracked with a temperature precision of 0.1 degreesC. A unique pressure controller was devised to maintain constant reactor pressures despite effluent viscosity fluctuations due to polymerization. Several chemical reaction systems have been characterized to date, including decomposition reactions of di-tert-butyl peroxide, polymerizations of styrene, formation of polyethylene from ethylene, and copolymerization of ethylene with I-octene. For ethylene polymerization, the amount of mass of polymer formed is proportional to the responses observed. [References: 10]
机译:在各种条件下(高达6.9 MPa(1000 psig)和300摄氏度),评估催化剂和化学反应的小规模方法受到了越来越多的关注。多孔平行批处理技术最常用于高通量筛选系统。相反,我们在此描述一种基于LC级钢管的高压,快速,高度可控的快速方法。含有多种流动成分(例如载体溶剂,催化剂配方和反应物)的试管使用来自电源的电流进行欧姆自加热,并以0.01%的精度进行调节。沿其长度排列的电压抽头阵列用于感测管的实时温度分布。反应被视为温度脉冲在反应器中传播,每个区域200μL,并以0.1摄氏度的温度精度跟踪。设计了独特的压力控制器,以保持恒定的反应器压力,尽管由于聚合反应造成的出水粘度波动。迄今为止,已经表征了几种化学反应体系,包括过氧化二叔丁基的分解反应,苯乙烯的聚合,由乙烯形成的聚乙烯以及乙烯与1-辛烯的共聚。对于乙烯聚合,形成的聚合物的质量与观察到的响应成比例。 [参考:10]

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