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Preparation and characterization of carboxylated cellulose nanocrystals from Oxytenanthera abyssinica (Ethiopian lowland bamboo) cellulose via citric acid anhydrous hydrolysis catalyzed by sulfuric acid

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Abstract

Acid hydrolysis, which uses concentrated mineral acids to produce cellulose nanocrystals (CNC), is expensive, overdegrades the cellulose material, and is hazardous to human and the environment. Thus recently, research has concentrated on using organic acids to produce CNC for economic and environmental concerns. This study used citric acid anhydrous (85–100 wt%) with a smaller amount of sulfuric acid (0–15wt%) as a catalyst to prepare carboxylated nanocrystals from Oxytenanthera abyssinica cellulose. The highest yield (89.7%) was obtained with a reaction condition of a 9:1wt% ratio of citric acid anhydrous to sulfuric acid, temperature (80 °C), and reaction time (5 h). The carboxyl functionalization of cellulose nanocrystals was affirmed through the conductometric titrimetric method and Fourier transform infrared spectroscopy. The conductometric titration showed a maximum carboxylate concentration of 0.75 ± 0.08 mmol/g; this gave the CNC stable dispersibility. Based on scanning electron microscopy characterization, mostly spherical-like shapes of carboxylated cellulose nanocrystals were obtained. The dynamic light scattering analysis showed that the particle possesses a particle size of 68.06 ± 1.05 nm with a maximum absolute value zeta potential of -33 mV. The x-ray diffraction analysis found cellulose crystallinity in the 60.37 to 81.3% range. The thermal gravimetric analysis showed that rapid mass loss occurred between 245 and 400 °C, with a maximum weight loss of 95%. Introducing the carboxylic group from citric acid anhydrous to cellulose can enhance the application of cellulose. Since the carboxylic groups are simultaneously introduced to the surface of cellulose during the hydrolysis process, it has the advantage of reducing the amount and chemical prices that cost for series and long-step surface functionalizing reactions. Citric acid could be easily recovered through a rotary evaporator, and since it is obtained from fruits, the carboxylic CNC formed has lower toxic risks. These environmentally friendly, sustainable, and nontoxic properties gave the produced carboxylic CNC high potential application for the production of biofilms, food packaging material, UV protection, drug delivery, and new bio-based nanomaterials.

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Authors and Affiliations

  1. Bio-process and Biotechnology Centre of Excellence, Addis Ababa, Ethiopia

    Limenew Abate Worku, Rakesh Kumar Bachheti & Mesfin Getachew Tadesse

  2. Department of Industrial Chemistry, College of Applied Sciences, Addis Ababa Sciences and Technology University, P.O. Box-16417, Addis Ababa, Ethiopia

    Limenew Abate Worku, Rakesh Kumar Bachheti & Mesfin Getachew Tadesse

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All authors contributed to the study conception and design. Material preparation, data collection, and analysis were performed by Limenew Abate Worku. The first draft of the manuscript was written by Rakesh Kumar Bachheti, Mesfin Getachew Tadesse, and Limenew Abate Worku. All authors commented on previous versions of the manuscript. All authors read and approved the final manuscript. All authors also worked on revision of the article.

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Worku, L.A., Bachheti, R.K. & Tadesse, M.G. Preparation and characterization of carboxylated cellulose nanocrystals from Oxytenanthera abyssinica (Ethiopian lowland bamboo) cellulose via citric acid anhydrous hydrolysis catalyzed by sulfuric acid. Biomass Conv. Bioref. (2023). https://doi.org/10.1007/s13399-022-03718-0

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