Slug-flow micro-reactor

This class of hybrid components comprises chip micro-reactor devices, as described in Section 4.1.3, connected to conventional tubing. This may be H PLC tubing which sometimes has as small internals as micro channels themselves. The main function of the tubing is to provide longer residence times. Sometimes, flow through the tube produces characteristic flow patterns such as in slug-flow tube reactors. Chip-tube micro reactors are typical examples of multi-scale architecture (assembly of components of hybrid origin). 

P 53] Before operation, a start-up time of about 10 min was applied to stabilize pressure in the chip micro reactor ([R 6]) [20]. As a result, a stable flow pattern was achieved. The reactant solutions were filled into vials. Slugs from the reactant solutions were introduced sequentially into the micro chip reactor with the autosampler and propelled through the chip with methanol as driving solvent. The flow rates were set to 1 pi min The slug volume was reduced to 2.5 pi. 

The chip micro reactor ([R 6]) was only one part of a complex serial-screening apparatus [20]. This automated system consists of an autosampler (CTC-HTS Pal system) which introduces the reactant solutions in the chip via capillaries. A pumping system (p-HPLC-CEC System) serves for fluid motion by hydro dynamic-driven flow. A dilution system [Jasco PU-15(5)] is used for slug dilution on-chip. The detection system was a Jasco UV-1575 and analysis was carried out by LC/MS (Agilent 1100 series capLC-Waters Micromass ZQ). All components were on-line and self-configured. 

Figure 5.6 Flow pattern map for a gas/liquid flow regime in micro channels. Annular flow wavy annular flow (WA) wavy annular-dry flow (WAD) slug flow bubbly flow annular-dry flow (AD). Transition lines for nitrogen/acetonitrile flows in a triangular channel (224 pm) (solid line). Transition lines for air/water flows in triangular channels (1.097 mm) (dashed lines). Region 2 presents flow conditions in the dual-channel reactor ( ), with the acetonitrile/nitrogen system between the limits of channeling (I) and partially dried walls (III). Flow conditions in rectangular channels for a 32-channel reactor (150 pm) (T) and singlechannel reactor (500 pm) (A) [13].

A hydrodynamic characterization of the micro reactor is given in [12], A flow-pattem map reveals the existence of dispersed flow, annular flow, slug-dispersed... 

Benchmarking of the micro reactors themselves - slug flow vs. falling film... 

GL 18] [R 6b] [P 18] Using a stoichiometric amount of hydrogen and operating in the slug-flow mode, it was shown that the yield of a micro reactor exceeds that of a mini fixed-bed reactor (LHSV = 60 h ) [61]. A maximum yield of 30% was obtained for the micro reactor for the range of pressure investigated (10-35 bar). 

In advance, comparative fixed-bed measurements were undertaken. It was ensured that the performance of a plug-flow operation with both flows having the same direction is superior to trickle-bed operation, using counter-flow instead. The plug flow was assumed to model the slug-flow behavior in the micro reactor. 

A flow-pattern map was derived for nitrogen/acetonitrile flows in the dual-channel micro reactor [274]. Bubbly, slug, churn and annular flows as well as wavy annular and wavy annular-dry flows with smaller region of stability were found (see Figure 4.35). 

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