Experimental Setup (Microscale). Microfluidic continuous flow reactors consisted in stainless steel (SS) coils (1.58 mm o.d. x 500 μm i.d.) equipped with SS nuts, ferrules and unions (VALCO). In experiments involving crude glycerol, the reactor consisted in a SS coil (3 mm o.d. x 2.1 mm i.d.) equipped with reducing unions (1/8” to 1/16”, Swagelok). The reactors were thermoregulated with a HeidolphTM MR Hei-Tec® oil bath equipped with a Pt-1000 temperature sensor. Sections of the reactors that were not subjected to high temperatures were constructed from PEEK or PFA tubings (1.58 mm o.d. x 750 μm i.d.) equipped with PEEK/ETFE connectors and ferrules (IDEX/Upchurch Scientific). Feed solutions were handled with high force Chemyx Fusion 6000 syringe pumps equipped with SS syringes and Dupont Kalrez O-rings or with Knauer Azura P 4.1S HPLC pumps. Downstream pressure was regulated using a dome-type back pressure regulator (Zaiput Flow Technologies BPR-10) connected to a nitrogen cylinder to set the working pressure (11 bar). In-line NMR reaction monitoring was carried out using a 43 MHz Spinsolve™ carbon NMR spectrometer from Magritek® .
By: Romaric Gérardy, Julien Estager, Patricia Luis, Damien P. Debecker, and Jean-Christophe M. Monbaliu.
Published On: January 2021