Low-Concentration Chemical Pretreatment of Lignocellulose Biomass Derived from Hemp Hurds, Agricultural Waste: Comparative Characterisation of Various Pretreatment Methods

Hemp hurds (HHs), a lignocellulosic agricultural waste, have the potential for bioconversion into bio-based products. However, the matrix structure of biomass comprising cellulose, hemicellulose, and lignin makes cellulose inaccessible. Pre-treatment is essential for accessing cellulose by removing lignin, hemicellulose, and extractives. This study compares lignocellulose structure modification of HH using low-concentration chemical pretreatment methods, including organosolvent, 60% ethanol (EtOH), 3% hydrogen peroxide with 3% ammonia (H₂O₂/NH₃), and 2% sodium hydroxide (NaOH) with sonication. X-ray diffractor (XRD) analysis, using Segal method as a guide, showed that post treatments, the crystallinity index increased from 39.26% in untreated HH to 65.80% for NaOH-treated hurds. Polysaccharide content decreased compared to HH, attributed to the combination of solubilisation of hemicellulose, degradation of amorphous carbohydrates, and loss of sample during treatment wash. Although there was a reduction in polysaccharide content compared to HH, NaOH treated HH showed the highest total carbohydrate content of 48.6% and the most disrupted surface structure, based on scanning electron microscope (SEM) images at 2000× magnification. Fourier-transform infrared spectrophotometer (FTIR) analysis indicated a reduction in lignin and hemicellulose peaks for NaOH and H₂O₂/NH₃ treatments, while thermogravimetric analyser (TGA) and derivative thermogravimetric analysis (DTG) results showed improved thermal stability for NaOH-treated samples. The ultrasound-assisted NaOH-treated sample had the most structural disruption in recovered solid fraction, based on comparative compositional and structural analyses. This gives a guide on the selection of pretreatment to pursue for HH processing.