Comparison of Xylene and Ethyl Acetate as Solvent in the Isolation of Levulinic Acid from Conversion Reaction of Cellulose Rice Husk using Hierarchical Mn3O4/ZSM-5 Catalyst
Corresponding email: yuni.krisnandi@sci.ui.ac.id
Published at : 07 Oct 2022
Volume : IJtech
Vol 13, No 4 (2022)
DOI : https://doi.org/10.14716/ijtech.v13i4.5524
Angellinnov, F., Krisnandi, Y.K., Rahayu, D.U.C., Dhaneswara, D., 2022. Comparison of Xylene and Ethyl Acetate as Solvent in the Isolation of Levulinic Acid from Conversion Reaction of Cellulose Rice Husk using Hierarchical Mn3O4/ZSM-5 Catalyst . International Journal of Technology. Volume 13(4), pp. 880-889
| Fiona Angellinnov | Department of Metallurgical and Materials Engineering, Faculty of Engineering, Universitas Indonesia, Depok, 16424, Indonesia |
| Yuni K. Krisnandi | 1. Department of Chemistry, Faculty of Mathematics and Natural Sciences, Universitas Indonesia, Depok, 16424, Indonesia 2. Solid Inorganic Framework Laboratory, Department of Chemistry, Faculty of Ma |
| Dyah U C Rahayu | Department of Chemistry, Faculty of Mathematics and Natural Sciences, Universitas Indonesia, Depok, 16424, Indonesia |
| Donanta Dhaneswara | Department of Metallurgical and Materials Engineering, Faculty of Engineering, Universitas Indonesia, Depok, 16424, Indonesia |
Levulinic acid is a
platform chemical. This compound can be derived from conversion cellulose in
lignocellulosic biomass such as rice husk. Cellulose conversion to levulinic
acid can be enhanced with the help of a catalyst. Hierarchical Mn3O4/ZSM-5
was used as a catalyst in this study, which was made by wet impregnation of
ZSM-5 with Mn (II). Before the conversion reaction, rice husk was pretreated
with various chemical and mechanical methods to increase the amount of
cellulose. The chemical method used NaOH, while mechanical methods used
variations of ball milling and ultrasonication in phosphoric acid. The
pretreated rice husk was then converted to levulinic acid at 130°C for 10 h in
H3PO4 40% and H2O2 30% using hierarchical Mn3O4/ZSM-5 as a catalyst. The highest levulinic acid yield of 11.70% was
obtained from the delignification of rice husk. The product was then extracted
to obtain pure levulinic acid via solvent extraction using xylene and ethyl
acetate as the organic solvents. The GC-MS examination showed that ethyl
acetate is the best solvent and esterification agent in separating the
levulinic acid.
Catalyst; Cellulose; Hierarchical ZSM-5; Levulinic acid; Rice husk
Levulinic
acid is commonly used as a base material in many industries such as the food,
pharmaceuticals, agriculture, cosmetics, and petroleum (Kumar et al., 2019).
This compound can also be converted into biofuels, including
2methyltetrahydrofuran, ????-valerolactone, levulinate esters, and
1,4-pentanediol (Yan et al., 2015). However, precursor material used to synthesize
levulinic acid is no longer available due to its high cost. As a result,
lignocellulosic biomass is widely used as a low-cost alternative precursor (Rackemann & Doherty, 2011).
Rice
husk is a type of lignocellulosic biomass that is abundant in Indonesia. In the
conversion, the cellulose is hydrolyzed to obtain glucose, which is then can be
converted to hydroxymethylfurfural (5-HMF) as an intermediate product, and
finally to levulinic acid (Climent et al., 2014; Li et
al.,
2019).
However, cellulose in rice husk is bound to lignin and hemicellulose. To obtain pure
cellulose, pretreatment is required. The pretreatment can be performed using
chemicals via acid and/or basic solution (Harahap et al., 2019; Hermansyah et al., 2019), mechanical, or combination methods (Qu et al., 2017).
The
isolation of levulinic acid from the conversion reaction of cellulose rice husk
using xylene and ethyl acetate as solvents and hierarchical Mn3O4/ZSM-5
as a catalyst has been successfully carried out. The results of the conversion
reaction showed the highest yield of levulinic acid at the reaction time of 10
hours, with the yield from the highest to the lowest in delignified rice husk
(11.70%), dewax process only (5.17%), ball milling followed by ultrasonication
(4.43%), ball milling only (3.88%), and ultrasonication only (3.76%),
respectively. Based on the chromatogram from the GC-MS examination, 5-HMF was
not detected in the organic phase from the extraction with xylene. Meanwhile,
ethyl levulinate was seen in the chromatogram of the organic phase from the
extraction with ethyl acetate. In this case, ethyl acetate is a better solvent
than xylene for separating levulinic acid from 5-HMF. Ethyl acetate does not
only act as a solvent but also as an esterification agent that reacts with
levulinic acid resulting in ethyl levulinate.
This
work is funded by a PITTA B grant from the Directorate of Research and
Community Engagement (DRPM) Universitas Indonesia No.
NKB-0636/UN2.R3.1/HKP.05.00/2019.
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