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first step operating at 8.5 wt% ST-DVB-SO3H, 323 K, and a glycerol to acetone molar ratio equal to 1:10, obtaining 84% solketal yield in the first step, followed by removal of formed water, and another reaction under the same conditions to achieve 98% solketal yield. The two-stage plant (Figure 12) was found to be the most economically appealing, because the separation costs were lower than the one-stage processes, resulting, according to the au- Sustain. Chem. 2021, 2 313 thors, in a Net Present Value (NPV) 45.7% higher when compared with (I) and 0.57% higher when compared with (II); therefore, (III) will be described further [25]. Figure 12. Flowsheet of the industrial solketal production plant proposed by Al-Saadi et al. [25]. An even deeper analysis was proposed by Chol et al. in a study that compared three The flowsheet comprises two mixers, the first to unite recycled and fresh acetone, scenarios comprising the treatment of crude glycerol and its valorization into solketal followed by the second where glycerol is inserted. Then, the stream is heated in a heat and glycerol carbonate. The authors concluded that the most economically advantageous exchanger up to the reaction temperature, which occurs in a plug-flow reactor packed flowsheet performs the valorization into both products, with glycerol equally divided for with the catalyst. The first reaction’s product stream is separated in a distillation column, both routes [124]. the acetone recovered as distillate is reinserted in the second reactor and the bottom The flowsheet (Figure 13) will be briefly described, with more focus on the solketal stream containing glycerol, water, and solketal is fed to a separation unit (not specified), production steps. Initially, crude glycerol and methanol were fed into a mixer to lower glycerol where water is removed. The products stream is cooled in a heat exchanger prior to being viscosity so the mixture can undergo a saponification reaction using KOH in the first reactor. The fed to the second reactor, where almost all the remainder glycerol is converted. What fol- resultant stream was fed to a second reactor to be acidified using HCl before being transferred lows is the second distillation column, where acetone is collected and recycled back to the to a gravity separator for sedimentation, where glycerol (bottom layer) was separated from free system and solketal is the bottom product with a content of 98% solketal and 2% glycerol. fatty acids (light liquids) and vapors. The resultant glycerol was cooled in a heat exchanger According to the authors, the separation cost is lower because, in the second reaction, only prior to solvent extraction using petroleum ether in a liquid-liquid extraction vessel. Petroleum 0.16% of the products’ stream is water. The cost of producing solketal in the described ether was then recovered in a flash separator for reuse and glycerol was neutralized with plant, considering a capacity of 100,000 t/years and a 20-year lifetime, was estimated at KOH in another reactor. Then, the resultant glycerol was fed into a membrane separator, $2058/ton, well below the selling value reported by the authors US$3000/ton [25]. where impurities were separated from the glycerol, methanol, and water solution, and in An even deeper analysis was proposed by Chol et al. in a study that compared three turn, vaporized in a flash separator. Glycerol was cooled and split into two streams. Half scenarios comprising the treatment of crude glycerol and its valorization into solketal and of the glycerol was converted into glycerol carbonate by feeding it to a mixer, where it was glycerol carbonate. The authors concluded that the most economically advantageous combined with recovered methanol, then heated and inserted in the reactor with dibutyltin oxide (catalyst) and excess CO2. The other half of glycerol, i.e., the stream leading to solketal production, was pressurized (12,000 kPa) before being fed into a conversion reactor with acetone and heterogeneous catalyst Amberlyst-15. The reaction was carried at 343 K for 1.5 h. The separation was promoted by a flash separator, where acetone with trace water was vaporized and recovered and the solketal stream was split into pure solketal and a recycle stream that was sent back to the reactor to improve conversion, since glycerol conversion is only 35% but can be enhanced with product recycle, according to the authors [124]. The economic analysis of implementing this industrial flowsheet is also promising, the cost of treating one ton of crude glycerol would be US$5045, while the revenue cost would be US $8036, resulting in a profit of almost US $3000/ton of glycerol. The total investment cost was expected to be recovered within three years of operation; considering that the first three years would be dedicated to building the facility, complete recovery is made within six years. According to the authors, these margins are decent for a biodiesel plant and the increased profit indicate that it would be worth it investing in crude glycerol purification and valorization plant [124].PDF Image | Continuous Valorization of Glycerol into Solketal
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