Malays. J. Anal. Sci. Volume 29 Number 5 (2025): 1350

Research Article

Tailoring nanocellulose properties from spent coffee grounds via controlled sulphuric acid hydrolysis

Sabiha Hanim Saleh,^1,2 Nur Risha Umaira Shaiful Bahri,¹ Norizan Ahmat,³ Shariff Ibrahim,^1,2 and Noraini Hamzah,^1,2*

¹School of Chemistry and Environment, Faculty of Applied Sciences, Universiti Teknologi MARA, 40450 Shah Alam, Selangor, Malaysia

²Industrial Waste Conversion Technology Research Group, Faculty of Applied Sciences, Universiti Teknologi MARA, 40450 Shah Alam, Selangor, Malaysia

³Centre of Foundation Studies, Universiti Teknologi MARA, Cawangan Selangor, Kampus Dengkil, 43800 Dengkil, Selangor, Malaysia

^*Corresponding author: pnoraini@uitm.edu.my

Received: 19 September 2024; Revised: 22 August 2025; Accepted: 25 August 2025; Published: 16 October 2025

Abstract

Spent coffee grounds (SCG) are an abundant agricultural residue rich in cellulose, which can be converted into nanocellulose (NC), a renewable, biodegradable material with high crystallinity and strength. However, extracting NC requires careful control of process conditions to maximise yield while preserving structural integrity. In this study, the effect of sulphuric acid (H₂SO₄) concentration on NC production from SCG cellulose was systematically investigated. Cellulose was first obtained via alkaline treatment and delignification, followed by acid hydrolysis at four H₂SO₄ concentrations (45, 50, 55, and 60 wt%) under controlled temperature, reaction time, and fibre-to-acid ratio. The yield of NC increased from 66.69 ± 0.81% at 45 wt% to 78.58 ± 1.90% at 60 wt%, with the crystallinity index rising from 54% in cellulose to above 90% at 50–55 wt%. The optimal condition was identified at 55 wt% H₂SO₄, achieving 77.24 ± 2.03% yield and 93% crystallinity while maintaining the NC structure. Thermal analysis showed reduced stability in NC compared to cellulose due to sulphate group incorporation. These results demonstrate that precise control of acid concentration is essential for producing high-quality NC from SCG for sustainable material applications.

Keywords: cellulose, nanocellulose, spent coffee grounds, sulphuric acid

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