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Sustain. Chem. 2021, 2 318 acetals and ketals. BASF SA patented a process of reaction preferentially in batch with continuous distillation of the azeotrope acetone-water, ideally after the equilibrium was reached, and continuous addition of fresh acetone. The azeotrope would have to be treated by distillation or absorption with desiccants, but the products would be obtained with purities of 95 to 99.5%, high enough for many applications, according to the authors, so further downstream would be unnecessary [64]. Guangzhou Yintian New Material Co. proposed a similar process to the proposed by Clarkson et al. [67,132]. Aiming to replace the traditional and energy-intensive distillation, Roche Vitamins Inc. and Evonik Degussa presented pervaporation or vapor permeation for downstream separation. The basic flowsheet of the first comprises at least three modules of a reactor with acidic ion exchange resin, followed by a vessel with basic ion exchange resin and then the pervaporation unit. The vessel with the basic ion exchange resin is required for the formation of other acetals and ketals that have acidic compounds as by-product, but not for glycerol ketalization. As for the second, at least two modules of a reactor followed by the pervaporation unit, with more acetone fed between the first membrane module and the second reactor and, in the end, another module to remove unreacted acetone. The inventors have not specified the type of reactor in which the reaction would be carried; however, both stated the importance of installing a heat exchanger between the reaction and separation sections [127,128]. Arkema France SA proposed a promising PI strategy based on the separation of water by adsorption in a Simulated Moving Bed Reactor (SMBR). The equipment comprises a series of columns packed with a hybrid acid solid that perform catalysis and selective adsorption of one of the reaction products. There are two inlet streams where the reactants and the eluent are fed and two outlet streams, where the products are withdrawn. Since the thermodynamic equilibrium is surpassed, as water is continuously separated, high conversions are achieved. Nonetheless, a later treatment step is required to remove the eluent from the products, but much less energy-demanding than the traditional separation of unreacted acetone and water [129]. Arkema France SA also invented a reactive liquid-liquid extraction methodology to allow the continuous process and to enhance conversion. During the reaction, part of the fraction containing the cyclic acetal products would be continuously removed from the continuous phase, driving the reaction towards product formation [130]. Relying on another PI strategy, Guangzhou Yintian New Material Co. patented a process in which the reaction occurs in a membrane reactor. The reactants would be continuously fed in a shell and tube membrane reactor with a heterogeneous catalytic layer and the water formed as by-product would permeate in the membrane and be removed from the medium. The benefits of the process are high conversion due to overcoming the thermodynamic limitation, diminished or no need for products downstream separation, that the catalyst is easily recovered, and that wastewater production is avoided [131]. China Petroleum & Chemical Corporation approached the thermodynamic limitation problem by using tin or titanium (or both) silicalite molecular sieves in form of powder mixed with the heterogeneous catalyst. The invention stated that the preferred types of reactor used would be tank, fixed bed, moving bed, suspended bed, or slurry bed, but it was not specified whether a downstream separation would be required [133–136]. The other patents exhibited in Table 5 are more well-known processes of reaction in tank or fixed-bed reactors with homogeneous or heterogeneous catalyst and separation in distillation columns, with small particularities among them. These inventions are relevant to the industry once they are the most industrially accepted and supported by years of extensive know-how on the operation. 6. Conclusions and Future Prospects Like almost all other sectors, the glycerol market was affected by the COVID-19 crisis mainly because many biodiesel plants have diminished production. Despite that, it was attested by the Independent Commodity Intelligence Services that glycerol supply isPDF Image | Continuous Valorization of Glycerol into Solketal
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