Micromixing temperature

A microreactor was also applied to this reaction. The slit interdigital micromixer was purchased from IMM (Mainz, Germany). The width of the interdigital channels is 25 pm. HPLC pumps were used to feed the two reaction solutions. One is a mixture of Boc-AMP and 1.2 molar equivalents of r-BocaO. The other is a 50% aqueous KOH solution. The microreactor was immersed in a temperature controlled cooling bath at 15 °C. The product was quenched with an acid, and samples were taken for HPLC analysis. 

Establishing the process sensitivity with respect to the above-mentioned factors is crucial for further scale-up considerations. If the sensitivity is low, a direct volume scale-up is allowed and the use of standard batch reactor configurations is permitted. However, many reactions are characterized by a large thermal effect and many molecules are very sensitive to process conditions on molecular scale (pH, temperature, concentrations, etc.). Such processes are much more difficult to scale up. Mixing can then become a very important factor influencing reactor performance for reactions where mixing times and reaction times are comparable, micromixing also becomes important. 

Lob et al. 2006b). Because of the high reactor load and large exother-micity of the reaction, the heat releases are quite strong. In-line temperature measurements in a micromixer-capillary set-up cooled by a temperature bath confirm the existence of hot spots of much more than 50°C in the capillary (see Fig. 11). 

Lob P, Lowe H, Hessel V, Hubbard SM, Menges G, Balon-Burger M (2006b) Determination of temperature profile within continuous micromixer-tube reactor used for the exothermic addition of dimethyl amine to acrylonitrile and an exothermic ionic liquid synthesis. In Proceedings of AIChE Spring National Meeting, Orlando, 23-27 April, 2006... 

Micromixer for immediate Temperature controlled adjustment of a uniform adjustable delay loop initial composition... 

The reaction system, the experiment procedure, and the analytical method used for the determination of micromixing in the TIJ mixer are the same as those described in the last section of this book but Mahajan et al. correlated their experimental data not with impinging velocity w() but with the jet Reynolds number Re. Also, the researchers employed the measure of increasing both the initial concentration CBo and the reaction temperature to raise the sensitivity of the procedure. The characteristic reaction time constant tK = 200 ms at 25 °C and CBo = 2.5 mM, while rR = 65 ms at 35 °C and CB0 = 4.7 mM, which can be used to bound the micromixing times, rM, no greater than them, respectively. 

Yoshida and coworkers also developed a microreaction system for cation pool-initiated polymerization [62]. Significant control of the molecular weight distribution (Mw/Mn) was achieved when N-acyliminium ion-initiated polymerization of butyl vinyl ether was carried out in a microflow system (an IMM micromixer and a microtube reactor). Initiator and monomer were mixed using a micromixer, which was connected to a microtube reactor for the propagation step. The polymerization reaction was quenched by an amine in a second micromixer. The tighter molecular weight distribution (Mw/M = 1.14) in the microflow system compared with that of the batch system (Mw/M > 2) was attributed to the very rapid mixing and precise control of the polymerization temperature in the microflow system. 

Typical industrial process for the synthesis of phenyl boronic acid from phenylmag-nesium bromide and boronic acid trimethoxy ester requires strict temperature control (—25 to —55 °C) to minimize the formation of side products. Recently, Hessel and coworkers reported that a micromixer (width 40 pm and depth 300 pm)/ tubular reactor system gave the phenyl boronic acid at high yield (>80%) even at higher temperatures (22 or 50 °C) with minimum amounts of the side products (Scheme 4.48) [66]. They also achieved a pilot-scale production by employing a caterpillar minimixer (width range 600-1700 pm and depth range 1200-2400 pm). 

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