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Sustain. Chem. 2021, 2 306 Author Kowalska-Kus, 2020 Capillary Microreactor Huang, 2020 Zhang, 2020 Catalyst ZSM5 (H) Beta(P) USY(P) ZSM5 Film ZSM5 Film Table 3. Cont. Catalyst Loading 0.083 gcat/ggly 0.050 gcat/ggly 4.7 μm film thickness 0.00066 gcat/ggly Reaction Conditions G:A = 1:3 T = 323 K P = 1 bar Solv. = Methanol Space time = 5 min G:A = 1:2 T = 323 K P = N.A. Solvent Free Space time = 2.86 min G:A = 1:8 T = 323 K P = N.A. Solvent Free Space time = 2.86 min G:A = 1:5 T = 308 K P = N.A. Solvent Free Space time = 1.73 h Results Xgly = 85% Sel > 95% Xgly = 69% Sel > 95% Xgly = 85% Sel > 95% Ysolk = 30% Xgly = 62% Xgly = 68.4% Ref [111] [112] [113] [102] Continuously Stirred Tank Reactor Dmitriev, 2018 Sulfuric Acid 1 Weight hourly space velocity. 2 Not available. 3 Only result provided. Nanda et al. and Moreira et al. proposed a similar system for the solketal synthesis in a fixed-bed reactor, both at 313 K, and an acetone to glycerol molar ratio of 2; the first, with the ion-exchange resin Amberlyst–36, achieved a conversion of 74%, and the latter, with Amberlyst–35, achieved a conversion of 81%. It is important to emphasize that these conversion values were obtained under transient operation [11,51]. Additionally, Nanda et al. achieved a conversion of 94% using optimized conditions and an acetone to glycerol molar ratio of 4, like Guidi et al., who used the same resin under similar reaction conditions [51,107]. Oliveira et al. also proposed an analogous system, but with the use of Amberlyst–15, and achieved excellent conversion, but the excessive acetone was a problem that could not be overcome [106]. Kowalska-Kus ́ et al. compared the catalytic performance of three zeolites (H-Beta, H-Mordenite, and H-ZSM5), also in a fixed-bed reactor, with methanol as the solvent in mild conditions, and found conversion about 88%, with an acetone to glycerol molar ratio of 3. The H-ZSM5 needed a desilication and acid pre-treatment to enlarge the pores and achieve an acceptable conversion. Moreover, the zeolites presented a loss in their activities over time [110]. The same researcher investigated the performance of zeolites with crude glycerol and achieved good conversion rates after just 1 h of reaction, but there was a fast deactivation of the catalysts and there was almost no conversion after 6 h [111]. Still on a fixed-bed reactor, but with a different type of packing, Domínguez-Barroso et al. built a carbon-based monolithic structure from spiral-wound laminated cellulose, constituting a structured packed reactor. The structure was impregnated with methanesul- fonic acid solution with SO3H to provide the catalyst acidic sites. The authors reported a complete glycerol conversion at WHSV = 2.9 h−1 and no catalytic activity loss, which they attributed to the possible hydrophobic character of the monolithic structure [109]. Solketal synthesis was also tested in capillary microreactors with zeolite ZSM5 film, as proposed by Huang et al. and Zhang et al.; however, the results are not encouraging when considering scaling-up the process [112,113].PDF Image | Continuous Valorization of Glycerol into Solketal
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