10-fold parallel reactor

Reactor 5 [R 5] 10-fold Parallel Reactor with Exchangeable Flow Distribution Section... 

Figure 11.27 Automated synthesis station (A) and top view of a 49-fold parallel reactor (B).

Schuth s group developed in the past a number of reactors similar to conventional testing methods with different degrees of sample integration. For multiphase reactions a 25-fold stirrer vessel reactor was developed [70] and for heterogeneous gas-phase reactions a 16-fold fixed-bed reactor was presented [71], which was later followed by a 49-fold parallel reactor [135], The reactor in Figure 3.42 was used for methanol production from Syngas at up to 50 bar and was essentially an improved version of the 49-fold reactor described in [135],... 

Figure 3.55 Modular set-up of 48-fold parallel gas-phase screening reactor [38] (by courtesy of VDI-Verlag GmbH).

The Cytos Pilot System is a 10-fold parallelized version of the Cytos Lab System [18] with identical fluidic behavior. Thus, nine Cytos microreactors were used for production with a cumulative product mass flow of 0.6 kg h , while alternately one reactor was treated with tetrahydrofuran in a rinsing cycle at a mass flow rate of 0.4kgh to avoid clogging of the microchannels. The continuously running Cytos Pilot System was cooled by an electrically tempered cooling system. 

In the plant used for academic purposes [4], both the solvent and exhausted CO2 are wasted. In an industrial plant both streams should be recycled after purification, for obvious economic reasons. The precipitator size and plant-flow-rates are obtained by increasing 80-fold the relative quantities used in the pilot plant [4]. This scale factor was suggested by the company that supplied the drug. Two vessels, P, in parallel are needed while the former is running, the latter can be cleaned and the solid product can be recovered. Cleaning and product-recovery expenses are not directly evaluated in this example. In the pilot plant, the flow of THF-polymer-drug solution was 0.072 kg/h, and the CO2 flowed in the quantity of 1.08 kg/h (the ratio CO2 to solution equals 15). The precipitator was a 0.4-liter vessel. The actual precipitator scale-up is not considered here. The main factor to consider in scaling-up the precipitator is the nozzle scale-up. The nozzle-size, nozzle-shape, and number of nozzles per reactor volume, determine the precipitate size in a complex and still incompletely understood way [5-8], It is assumed that issues related to the injectors are already solved. 

A 15-fold glass tube parallel-packed bed reactor has been described [28-30], which is close to conventional catalyst testing equipment. The same authors also reported a 64-fold ceramic block reactor and a ceramic monolithic reactor for the screening of up to 250 catalysts in parallel. The individual catalysts were coated... 

A 15-fold glass tube parallel packed-bed reactor was introduced [67, 68], which is similar to conventional catalyst testing equipment (Figure 3.39). The premixed reactant gas is supplied by a 16-port valve either to the bypass or to one of the 15 reactors. By a second 16-port valve, the product gas stream of a selected reactor can be channeled to the quadrupole mass spectrometer. The full automation of the screening set-up allows the investigation of 15 catalysts per day [67]. 

Figure 3.42 Parallel 49-fold fixed-bed reactor for high-pressure use at the MPI-Muhlheim. Mounted reactor (left), schematic sectional view (right) and unmouted reactor parts (bottom) [135] (by courtesy of Elsevier Ltd.)...

A 20-fold scale-up has been performed using a more polar solvent (BTF), going from a 10 mL to an 80 mL vessel in the Discover, 3 x 20-fold (60 mmol) by employing the Voyager SF, and 6 x 20-fold (120 mmol) by employing parallel rotors in the MARS and microSYNTH reactors. Similar results regarding yield and product purity were obtained with each platform, demonstrating that the success of the reactions is neither dependent on the equipment used nor on the scale applied (Scheme 7). 

Other examples of scale-up involved a triphenylphosphine-free one-pot Wittig olefination, a one-step three-component synthesis of imidazo annulated pyridine and a metal-catalyzed Suzuki coupling. Kappe and co-workers also recently transferred conditions for reactions originally performed on a small scale with a mono-modal system, to scale-up by parallel synthesis in a multimodal batch reactor [13]. Typically, the scale-up was 100-fold, from 1 mmol examples included Biginelli condensations, Heck and Negishi couplings, and Diels-Alder cycloadditions with gaseous reactants. 

Further process intensification which results in a 10-fold higher throughput leads to a dramatic decrease in operating costs (Figure 13.8) and also a decrease in fixed costs. The main driver is the decline in the operator s salary. A similar result could be obtained by external numbering-up, that is, with 10 reactors in parallel. 

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