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Sustain. Chem. 2021, 2 308 Author Reactive coupling Eze, 2018 Al–Saadi, 2019 Catalyst Loading 9 g 0.5 mol Table 4. Cont. Reaction Conditions 1 glycerol:4 acetone 2; 30 methanol:1 triacetin:4 acetone 3; 6 methanol:1 triacetin:4 acetone 4 T = 323 K P = N.A. Sol = Methanol Space time = 0.5 h 10 methanol: 1 triacetin: 7 acetone T = 323 K P = N.A. Space time = 8 h Results Xgly = 80.6% Xgly = 48.5% 3 Xgly = 80.6% 4 Ysolk = 82% Observations Ref Mesoscale oscillatory baffled reactors (meso-OBRs). Silica gel added as dehydrating agent to overcome the [118] thermodynamic equilibrium limitation. Catalyst Amberlyst 70–SO3H Amberlyst 70–SO3H Amberlyst A26–OH DBSA (p– Dodecylbenzene sulfonic acid) 2 [117] 1 Number of theoretical stages. 2 Synthesis of only solketal. 3 Synthesis of biodiesel and solketal in one reactor. 4 Synthesis of biodiesel and solketal in two reactors. Microwave irradiation has been explored as a heating intensification strategy in continuous and batch processes. According to the authors, heat transfer is more efficient because the microwave energy is transferred directly to the reaction molecules; moreover, since there is a faster response in comparison to conventional heating, the process is safer. Cablewski et al. produced solketal with pTSA and high excess of acetone in an apparatus that comprises a reaction coil inside a microwave cavity. The reactants were preheated and fed together with the catalyst continuously. Years later, Priya et al. tested a more environmentally friendly process in batch with several transition metals supported over Mordenite and stated that Cu-Mor performed better, which they attributed to the greater acidity of this catalyst [68,116]. Reactive distillation is an appealing PI strategy because it tackles the thermodynamic limitation by removing water from the reaction medium at the same time it integrates reaction and separation by distillation, eliminating the need for post-treatment processes. Clarkson et al. proposed to carry the reaction on a multitray reactive distillation column with deep stages containing Amberlyst-DPT in suspension. They proposed a 15 stages column, with 10 reactive stages. Pre-heated glycerol would be fed at the top of the column so it could flow down through all the stages and acetone would be fed at the bottom so it could pass up the column agitating the resin and stripping out the water generated. Solketal would be purified in the bottom three stages and collected with a purity of more than 99% [67]. A similar system was proposed by Li et al., followed by optimization in Aspen Plus software and comparison with a novel equipment, the reactive dividing-wall column (RDWC). The experimental parameters and results are shown in Table 4. As for the optimization results considering the energy consumption (reboiler duty), it was found that the ideal scenario is nine theoretical reaction stages, five theoretical rectifying stages, and six stages in the stripping section (solketal purification), with a G:A molar feed ratio of 1:2–3 and a reflux ratio of 2.4. The comparison of the optimized traditional process with the RDWC resulted in a reduction in energy consumption by 13.6%; therefore, the authors address the RDWC as a PI strategy. This column promotes a more efficient purification of the solketal because it simulates a distillation column (II) alongside the reactive distillation column (I) inside the same unit, as seen in Figure 9 [104].PDF Image | Continuous Valorization of Glycerol into Solketal
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