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Issue 57, 2019
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Mechanochemistry-assisted hydrolysis of softwood over stable sulfonated carbon catalysts in a semi-batch process

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Abstract

The hydrolysis of lignocellulose is the first step in saccharide based bio-refining. The recovery of homogeneous acid catalysts imposes great challenges to the feasibility of conventional hydrolysis processes. Herein, we report a strategy to overcome these limitations by using stable sulfonated carbons as solid acid catalysts in a two-step process, composed of mechanocatalytic pretreatment and secondary hydrolysis in a semi-batch reactor. Without mechanocatalytic pre-treatment the hydrolysis of the insoluble substrate largely occurs through homogeneously catalyzed reactions. Ball-milling induced amorphization promotes a substantially higher substrate reactivity, because homogeneous hydrolysis occurs preferentially from less ordered structural domains in cellulose. In contrast, concerted ball-milling (CBM) of cellulose with the sulfonated carbon promotes a heterogeneously catalyzed hydrolysis to soluble oligosaccharides. By performing an in-depth physicochemical characterization of cellulose subjected to CBM treatment with different carbons, we reveal the crucial role of strong Brønsted acid sites in facilitating mechanocatalytic depolymerization. Recyclability experiments confirmed that despite being subject to profound structural changes during repeated pre-treatment/semi-batch hydrolysis cycles, the sulfonated carbon retained its catalytic activity. The combination of mechanocatalytic pretreatment with strong solid acids and hydrolysis in the semi-batch reactor was successfully extrapolated for the first time to the hydrolysis of real lignocellulose to achieve quantitative yields in C5 and high yields in C6 derived products.

Graphical abstract: Mechanochemistry-assisted hydrolysis of softwood over stable sulfonated carbon catalysts in a semi-batch process

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Supplementary files

Article information


Submitted
30 Sep 2019
Accepted
03 Oct 2019
First published
18 Oct 2019

This article is Open Access

RSC Adv., 2019,9, 33525-33538
Article type
Paper

Mechanochemistry-assisted hydrolysis of softwood over stable sulfonated carbon catalysts in a semi-batch process

D. Scholz, J. Xie, O. Kröcher and F. Vogel, RSC Adv., 2019, 9, 33525
DOI: 10.1039/C9RA07668A

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