Extraction, Isolation, and TEMPO-NaBr-NaClO Oxidation Modification of Cellulose from Coffee Grounds

This study investigates the extraction, isolation, and chemical modification of cellulose from coffee ground residues using TEMPO-NaBr-NaClO oxidation. These residues represent a promising renewable source of cellulose, which is obtained after the removal of impurities such as lignin (24%), hemicell...

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Main Authors: Mourad Ouhammou, Abdellah Mourak, Aziz Ait-Karra, Jaouad Abderrahim, Najat Elhadiri, Mostafa Mahrouz
Format: Article
Language:English
Published: MDPI AG 2025-04-01
Series:Biomass
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Online Access:https://www.mdpi.com/2673-8783/5/2/22
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author Mourad Ouhammou
Abdellah Mourak
Aziz Ait-Karra
Jaouad Abderrahim
Najat Elhadiri
Mostafa Mahrouz
author_facet Mourad Ouhammou
Abdellah Mourak
Aziz Ait-Karra
Jaouad Abderrahim
Najat Elhadiri
Mostafa Mahrouz
author_sort Mourad Ouhammou
collection DOAJ
description This study investigates the extraction, isolation, and chemical modification of cellulose from coffee ground residues using TEMPO-NaBr-NaClO oxidation. These residues represent a promising renewable source of cellulose, which is obtained after the removal of impurities such as lignin (24%), hemicellulose (42%), and other compounds. The TEMPO (2,2,6,6-tetramethylpiperidine-1-oxyl radical)-catalyzed oxidation selectively converts primary hydroxyl groups into carboxylate groups (-COOH) under mild conditions in aqueous media, achieving an oxidation yield of up to 67%. Structural and morphological analyses, including scanning electron microscopy (SEM), Fourier transform infrared (FTIR) spectroscopy, and X-ray diffraction (XRD), confirm the successful chemical modification of the cellulose. The results indicate a reduction in crystallinity index from native cellulose (80%) to oxidized cellulose (65%), reflecting partial disruption of the microfibril structure and the introduction of new chemical functionalities. FTIR analysis reveals the appearance of characteristic carboxylate bands, confirming the conversion of hydroxyl groups into carboxyl groups. Energy-dispersive X-ray (EDX) analysis further highlights a significant increase in oxygen content, indicating the efficiency of the oxidation process. The TEMPO-oxidized cellulose is water-soluble, enabling the production of valuable polyelectrolytes and intermediates. These chemical modifications improve the cellulose’s reactivity, broadening its potential applications in various fields, including biocomposites, sustainable packaging materials, and functional films. This work demonstrates the feasibility of utilizing coffee ground residues as a renewable, eco-friendly source of modified cellulose for high-value applications.
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spelling doaj-art-e99c20c41ff54da08c79d7b5010efb6f2025-06-25T13:30:48ZengMDPI AGBiomass2673-87832025-04-01522210.3390/biomass5020022Extraction, Isolation, and TEMPO-NaBr-NaClO Oxidation Modification of Cellulose from Coffee GroundsMourad Ouhammou0Abdellah Mourak1Aziz Ait-Karra2Jaouad Abderrahim3Najat Elhadiri4Mostafa Mahrouz5The Higher Institute of Nursing Professions and Health Techniques of Marrakech, Marrakech 40000, MoroccoLaboratory of Material Sciences and Process Optimization, Faculty of Sciences Semallaia, Cadi Ayyad University, BP 2390, Marrakech 40000, MoroccoLaboratory of Applied Chemistry and Biomass, Department of Chemistry, Faculty of Sciences Semlalia, Cadi Ayyad University, BP 2390, Marrakech 40000, MoroccoLaboratory of Material Sciences and Process Optimization, Faculty of Sciences Semallaia, Cadi Ayyad University, BP 2390, Marrakech 40000, MoroccoLaboratory of Material Sciences and Process Optimization, Faculty of Sciences Semallaia, Cadi Ayyad University, BP 2390, Marrakech 40000, MoroccoLaboratory of Material Sciences and Process Optimization, Faculty of Sciences Semallaia, Cadi Ayyad University, BP 2390, Marrakech 40000, MoroccoThis study investigates the extraction, isolation, and chemical modification of cellulose from coffee ground residues using TEMPO-NaBr-NaClO oxidation. These residues represent a promising renewable source of cellulose, which is obtained after the removal of impurities such as lignin (24%), hemicellulose (42%), and other compounds. The TEMPO (2,2,6,6-tetramethylpiperidine-1-oxyl radical)-catalyzed oxidation selectively converts primary hydroxyl groups into carboxylate groups (-COOH) under mild conditions in aqueous media, achieving an oxidation yield of up to 67%. Structural and morphological analyses, including scanning electron microscopy (SEM), Fourier transform infrared (FTIR) spectroscopy, and X-ray diffraction (XRD), confirm the successful chemical modification of the cellulose. The results indicate a reduction in crystallinity index from native cellulose (80%) to oxidized cellulose (65%), reflecting partial disruption of the microfibril structure and the introduction of new chemical functionalities. FTIR analysis reveals the appearance of characteristic carboxylate bands, confirming the conversion of hydroxyl groups into carboxyl groups. Energy-dispersive X-ray (EDX) analysis further highlights a significant increase in oxygen content, indicating the efficiency of the oxidation process. The TEMPO-oxidized cellulose is water-soluble, enabling the production of valuable polyelectrolytes and intermediates. These chemical modifications improve the cellulose’s reactivity, broadening its potential applications in various fields, including biocomposites, sustainable packaging materials, and functional films. This work demonstrates the feasibility of utilizing coffee ground residues as a renewable, eco-friendly source of modified cellulose for high-value applications.https://www.mdpi.com/2673-8783/5/2/22cellulose extractioncoffee groundsTEMPO-NaBr-NaClO oxidationcrystallinity indexwaste valorization
spellingShingle Mourad Ouhammou
Abdellah Mourak
Aziz Ait-Karra
Jaouad Abderrahim
Najat Elhadiri
Mostafa Mahrouz
Extraction, Isolation, and TEMPO-NaBr-NaClO Oxidation Modification of Cellulose from Coffee Grounds
Biomass
cellulose extraction
coffee grounds
TEMPO-NaBr-NaClO oxidation
crystallinity index
waste valorization
title Extraction, Isolation, and TEMPO-NaBr-NaClO Oxidation Modification of Cellulose from Coffee Grounds
title_full Extraction, Isolation, and TEMPO-NaBr-NaClO Oxidation Modification of Cellulose from Coffee Grounds
title_fullStr Extraction, Isolation, and TEMPO-NaBr-NaClO Oxidation Modification of Cellulose from Coffee Grounds
title_full_unstemmed Extraction, Isolation, and TEMPO-NaBr-NaClO Oxidation Modification of Cellulose from Coffee Grounds
title_short Extraction, Isolation, and TEMPO-NaBr-NaClO Oxidation Modification of Cellulose from Coffee Grounds
title_sort extraction isolation and tempo nabr naclo oxidation modification of cellulose from coffee grounds
topic cellulose extraction
coffee grounds
TEMPO-NaBr-NaClO oxidation
crystallinity index
waste valorization
url https://www.mdpi.com/2673-8783/5/2/22
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AT azizaitkarra extractionisolationandtemponabrnaclooxidationmodificationofcellulosefromcoffeegrounds
AT jaouadabderrahim extractionisolationandtemponabrnaclooxidationmodificationofcellulosefromcoffeegrounds
AT najatelhadiri extractionisolationandtemponabrnaclooxidationmodificationofcellulosefromcoffeegrounds
AT mostafamahrouz extractionisolationandtemponabrnaclooxidationmodificationofcellulosefromcoffeegrounds