Comparative study of microwave-assisted versus conventional heated reactions of biomass conversion into levulinic acid over hierarchical Mn3O4/ZSM-5 zeolite catalysts

[Display omitted] •The results from microwave-assisted reaction (600 W for 180 s) are comparable to the conventional reaction (130 °C for 4 h).•The LA yield from glucose in the microwave-assisted reaction (9.57%) is higher than the conventional reaction (6.93%).•The 1H and 13C NMR analyses indicate...

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Veröffentlicht in:Carbon resources conversion 2023-09, Vol.6 (3), p.245-252
Hauptverfasser: Helmi, Mazizah R.A., Rahayu, Dyah Utami C., Pratama, Arnia P., Khatrin, Irena, Ramadhani, Anita N., Krisnandi, Yuni K.
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Sprache:eng
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Zusammenfassung:[Display omitted] •The results from microwave-assisted reaction (600 W for 180 s) are comparable to the conventional reaction (130 °C for 4 h).•The LA yield from glucose in the microwave-assisted reaction (9.57%) is higher than the conventional reaction (6.93%).•The 1H and 13C NMR analyses indicate that the microwave-assisted process improves the purity of LA.•In the microwave-assisted process, the Mn3O4/ZSM-5 catalyst can be used for 3 cycles without significant damage. Conversion of delignified cellulose from rice husk biomass, and model compounds of cellobiose and glucose to levulinic acid (LA) over hierarchical Mn3O4/ZSM-5 catalyst was carried out using a household microwave method, and then compared to the established conventional thermos-reaction method. The hierarchical ZSM-5 was prepared using a double template method, aiming for micro and mesoporous systems developed in the structure. The as-prepared ZSM-5 were modified with Mn3O4 through incipient wetness impregnation with Mn2+ solution followed by calcination at 550 °C. The catalysts were characterized using various techniques such as powder XRD, SEM, BET, AAS, and FT-IR which indicated the hierarchical structure of MFI zeolite (Si/Al of 30–34) with Mn loading of 2.14 wt%. The conversion products were analyzed using HPLC, 1H NMR, and 13C NMR instruments. The microwave-assisted reaction using 600 W for 180 s using delignified cellulose, cellobiose, and glucose gave conversion of 37.27%, 46.35%, and 54.29%, respectively which is close to the conversion given by the conventional reaction carried out at 130 °C for 4 h (36.75%, 55.62%, and 60.9%, respectively). Interestingly, the LA yield from the microwave-assisted reaction (4.33%, 6.12%, and 9.57%) is higher than the yield from the conventional reaction, which only produced 5.2%, 4.88%, and 6.93% respectively. The microwave-assisted method is also shown to give less by-products compared to the thermochemical reaction. Therefore, it could be considered an alternative method for converting cellulose to LA.
ISSN:2588-9133
2588-9133
DOI:10.1016/j.crcon.2023.02.005