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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 Sustain. Chem. 2021, 2 309 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]. Figure 9. Diagram of the reactive dividing-wall column (based on [104]). Figure 9. Diagram of the reactive dividing-wall column (based on [104]). Membrane reactors also approach PI by diminishing the thermodynamic limitations, i.e., removing water from the reaction medium. Pervaporation and vapor permeation are already industrially well-established processes for water removal; the challenges faced with the use of these technologies for solketal synthesis are the catalyst activity and the mass transfer limitation. Roldán et al. avoided these problems by using K10 montmorillonite as catalyst dispersed in the reaction medium, thus handling catalysis and water removal separately, and preventing membrane contact with the liquid phase by promoting vapor permeation [54,119]. Qing et al., on the other hand, used a catalytically active membrane to react glycerol with cyclohexanone in a very similar system to solketal synthesis. The catalyst is constituted of three layers: the top being a catalytic layer, the middle a dense selective layer, and the bottom a porous support layer. The results were promising, and the behavior may be the same for the reaction of glycerol with acetone [119]. Moreira et al. also explored water removal as a strategy to conform to the PI guidelines. In a simple system already explained in Section 4.3., the authors exploit Amberlyst-35 affinity to water to shift the equilibrium toward the formation of solketal, transforming a simple fixed-bed reactor in an adsorptive reactor [11]. This was a remarkable study in comparison to other studies described Section 4.3 because many of the authors that employed fixed-bed columns mentioned the use of acetone as a stripping agent rather than the use of a separation strategy to favor glycerol conversion. Eze et al. proposed an interesting system where the biodiesel preparation and glycerol conversion would be carried at the same time (reaction coupling) so that the valorization of glycerol would occur in situ. To do so, the reactions would occur in two oscillatory baffled reactors in series packed with Amberlyst–70. Methanol and triacetin would be fed to the first reactor and the products would follow to the second, where acetone would be fed. A glycerol conversion of 80.6% was achieved [117]. Similarly, Al-Saadi et al. proposed a reaction coupling in batch catalyzed by p- Dodecylbenzenesulfonic acid (DBSA). This catalyst is a homogeneous strong Brønsted acid chosen because of the surfactant-like nature of the catalyst, the high rate of reaction, and the low corrosivity compared to mineral acid catalysts, according to the authors. The authors compared the effect of feeding acetone at the beginning of the process with feeding when almost complete triacetin conversion would be reached and found that the second strategy is much more efficient, achieving 82% glycerol conversion against 39.5% achieved by the first strategy [118].PDF Image | Continuous Valorization of Glycerol into Solketal
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