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Extraction and characterization of lignin from olive pomace: a comparison study among ionic liquid, sulfuric acid, and alkaline treatments

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Abstract

Olive pomace is a phytotoxic by-product in the olive oil production. Lignin is a biopolymer present in the olive pomace in remarkable percentages, which has a great variety of potential industrial uses. The extraction of lignin using the ionic liquid triethylammonium hydrogen sulfate resulted in recovery yields as high as 40% of the available lignin in the dry olive pomace. This percentage was obtained after optimizing conditions such as temperature, extraction time, and water content in the ionic liquid. This is the first time such a high percentage of extraction has been achieved when evaluating this type of feedstock. For comparison, two other extraction methods (sulfuric acid and alkaline treatments) were used to assess their extracting performances. Lignin was quantified after developing a rapid, robust, and reliable method by Fourier transform infrared spectroscopy (purity of 101 ± 16%) and characterized by proton nuclear magnetic resonance and gel permeation chromatography. The assay total phenolic content (TPC) revealed high content of phenolic groups (212 ± 26.9 mg of gallic acid equivalents per g of lignin). The high purity and TPC conferred on the extracted lignin a potentially high antioxidant activity. In addition, a 67-fold scale-up extraction of initial mass loading was performed obtaining same results as in the lower scale. Thus, the extraction of lignin using this methodology is expected to mitigate the disposal of the olive pomace and provide certain revenue to the oil mill.

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Acknowledgements

The authors would like to thank the Catalan Government for the quality accreditation given to their research group 2017 SGR 828. This work has been partially funded by the Spanish government (CTQ2015-70982-C3-1-R, MINECO/FEDER). E.C. would like to thank “Banco Santander” for Grant X15016 in the framework of the “UdL Impuls” project. The “Cooperativa de l’Albi” is greatly acknowledged for fruitful discussions and kindly providing all olive pomaces.

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  1. Department of Chemistry, University of Lleida, ETSEA, Av. Rovira Roure 191, Lleida, Spain

    Enrique Cequier, Johanna Aguilera, Mercè Balcells & Ramon Canela-Garayoa

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  1. Enrique Cequier
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ESM 1

Enclosed in the supporting information there are complementary discussions, the FT-IR method validation, figures (Fig. S1–19) corresponding to ionic liquid, lignin and triglycerides spectra (FT-IR and NMR) and GPC determinations, and tables (Table S1–4) of the ratios flesh/stone, lignin content of the substrates determined by FT-IR and reference method, the T test: paired two samples for means, and the ionic liquid recovery and the effectiveness of the re-extractions. (DOCX 1730 kb)

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Cequier, E., Aguilera, J., Balcells, M. et al. Extraction and characterization of lignin from olive pomace: a comparison study among ionic liquid, sulfuric acid, and alkaline treatments. Biomass Conv. Bioref. 9, 241–252 (2019). https://doi.org/10.1007/s13399-019-00400-w

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