Reactive Chromatography Applied to Ethyl Levulinate Synthesis: A Proof of Concept
Abstract
:1. Introduction
2. Materials and Methods
2.1. Materials
2.2. Methods
2.2.1. Chromatographic Reactor Setup
2.2.2. Take-up Test
3. Results and Discussion
3.1. Dowex 50WX8 Take-up Tests
3.2. Reactive Chromatography Results
Effect of the Stream Flow Rate
3.3. Effect of the Reactor Temperature
4. Conclusions
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Acknowledgments
Conflicts of Interest
Abbreviations
LA | Levulinic acid |
EL | Ethyl levulinate |
EtOH | Ethanol |
H2O | Water |
List of symbols | |
T | Temperature [K] |
t | Time [s] |
Volume of dried resin [cm3] | |
Volume of swelled resin [cm3] | |
Swelling coefficient [%] |
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Catalyst | Particle Size [μm] | Crosslinking Degree [%] | Ionic Form | Total Exchange Capacity [meq/cm3] | Density [g/cm3] | Water Retention Capacity [%] | Max. Operative Temperature [°C] |
---|---|---|---|---|---|---|---|
Dowex 50WX8 | 150–300 | 8 | H+ | 1.7 | 0.8 | 50–56 | 120 |
Test | cLA [mol/L] | cEL [mol/L] | T [K] | Q [cm3/min] | P [bar] | ΔP [kg/cm2] |
---|---|---|---|---|---|---|
C1 | 6 | - | 303 | 0.8 | 2 | 9 |
C2 | 6 | - | 303 | 0.9 | 2 | 10 |
C3 | 6 | - | 303 | 1.1 | 2 | 13 |
C4 | 6 | - | 303 | 2.5 | 2 | 30 |
C5 | 6 | - | 303 | 5 | 2 | 54 |
C6 | - | 6 | 303 | 0.8 | 2 | 9 |
C7 | - | 6 | 303 | 0.9 | 2 | 10 |
C8 | - | 6 | 303 | 1.1 | 2 | 13 |
C9 | - | 6 | 303 | 2.5 | 2 | 30 |
C10 | - | 6 | 303 | 5 | 2 | 54 |
C11 | 6 | - | 313 | 1.1 | 2 | 13 |
C12 | 6 | - | 313 | 1.7 | 2 | 21 |
C13 | 6 | - | 313 | 1.8 | 2 | 23 |
C14 | 6 | - | 313 | 1.9 | 2 | 24 |
C15 | 6 | - | 313 | 2.5 | 2 | 30 |
C16 | - | 6 | 313 | 1.1 | 2 | 13 |
C17 | - | 6 | 313 | 1.7 | 2 | 21 |
C18 | - | 6 | 313 | 1.8 | 2 | 23 |
C19 | - | 6 | 313 | 1.9 | 2 | 24 |
C20 | - | 6 | 313 | 2.5 | 2 | 30 |
C21 | 6 | - | 323 | 1.8 | 2 | 23 |
C22 | 6 | - | 323 | 2.0 | 2 | 26 |
C23 | 6 | - | 323 | 2.5 | 2 | 30 |
C24 | 6 | - | 323 | 5.0 | 2 | 54 |
C25 | - | 6 | 323 | 1.8 | 2 | 23 |
C26 | - | 6 | 323 | 2.0 | 2 | 26 |
C27 | - | 6 | 323 | 2.5 | 2 | 30 |
C28 | - | 6 | 323 | 5.0 | 2 | 54 |
Molar Fractions [–] | α [%] | |||
---|---|---|---|---|
LA | EtOH | EL | H2O | |
1 | - | - | - | 51.6 |
- | 1 | - | - | 58.5 |
- | - | 1 | - | 45.7 |
- | - | - | 1 | 57.5 |
0.8 | 0.2 | - | - | 45.7 |
0.5 | 0.5 | - | - | 49.0 |
0.2 | 0.8 | - | - | 52.8 |
0.8 | - | 0.2 | - | 45.1 |
0.5 | - | 0.5 | - | 36.1 |
0.2 | - | 0.8 | - | 45.1 |
0.8 | - | - | 0.2 | 49.2 |
0.5 | - | - | 0.5 | 51.0 |
0.2 | - | - | 0.8 | 56.2 |
- | 0.8 | 0.2 | - | 52.1 |
- | 0.5 | 0.5 | - | 44.2 |
- | 0.2 | 0.8 | - | 47.7 |
- | 0.8 | - | 0.2 | 54.9 |
- | 0.5 | - | 0.5 | 52.8 |
- | 0.2 | - | 0.8 | 57.9 |
- | - | 0.8 | 0.2 | 45.1 |
- | - | 0.5 | 0.5 | 50.6 |
- | - | 0.2 | 0.8 | 57.4 |
Test | T [K] | Q [cm3/min] | XLA [%] * |
---|---|---|---|
C1 | 303 | 0.8 | 100 |
C2 | 303 | 0.9 | 87 |
C3 | 303 | 1.1 | 58 |
C4 | 303 | 2.5 | 0 |
C5 | 303 | 5.0 | 0 |
C11 | 313 | 1.1 | 100 |
C12 | 313 | 1.7 | 65 |
C13 | 313 | 1.8 | 67 |
C14 | 313 | 1.9 | 68 |
C15 | 313 | 2.5 | 0 |
C21 | 323 | 1.8 | 100 |
C22 | 323 | 2.0 | 100 |
C23 | 323 | 2.5 | 0 |
C24 | 323 | 5.0 | 0 |
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Rossano, C.; Pizzo, C.L.; Tesser, R.; Di Serio, M.; Russo, V. Reactive Chromatography Applied to Ethyl Levulinate Synthesis: A Proof of Concept. Processes 2021, 9, 1684. https://doi.org/10.3390/pr9091684
Rossano C, Pizzo CL, Tesser R, Di Serio M, Russo V. Reactive Chromatography Applied to Ethyl Levulinate Synthesis: A Proof of Concept. Processes. 2021; 9(9):1684. https://doi.org/10.3390/pr9091684
Chicago/Turabian StyleRossano, Carmelina, Claudio Luigi Pizzo, Riccardo Tesser, Martino Di Serio, and Vincenzo Russo. 2021. "Reactive Chromatography Applied to Ethyl Levulinate Synthesis: A Proof of Concept" Processes 9, no. 9: 1684. https://doi.org/10.3390/pr9091684