Nanocellulose is a renewable and biocompatible nanomaterial that evokes much interest because of its versatility in various applications. This study reports the production of nanocellulose from Agave gigantea (AG) fiber using the chemical-ultrafine grinding treatment. Chemical treatment (alkalization and bleaching) removed non-cellulose components (hemicellulose and lignin), while ultrafine grinding reduced the size of cellulose microfibrils into nanocellulose. From the observation of Transmission Electron Microscopy, the average diameter of nanocellulose was 4.07 nm. The effect of chemical-ultrafine grinding on the morphology and properties of AG fiber was identified using chemical composition, Scanning Electron Microscopy, X-ray Diffraction, Fourier Transform Infrared, and Thermogravimetric Analysis. The bleaching treatment increased the crystal index by 48.3% compared to raw AG fiber, along with an increase in the cellulose content of 20.4%. The ultrafine grinding process caused a decrease in the crystal content of the AG fiber. The crystal index affected the thermal stability of the AG fiber. The TGA results showed that AG fiber treated with bleaching showed the highest thermal stability compared to AG fiber without treatment. The FTIR analysis showed that the presence of CH vibrations from the ether in the fiber. After chemical treatment, the peaks at 1605 and 1243 cm−1 disappeared, indicating the loss of lignin and hemicellulose functional groups in AG fiber. As a result, nanocellulose derived from AG fiber can be applied as reinforcement in environmentally friendly polymer biocomposites.
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