Comparative study on liquid versus gas phase hydrochloric acid hydrolysis for microcrystalline cellulose isolation from sugarcane bagasse.

Microcrystalline cellulose (MCC) was successfully synthesized from sugarcane bagasse using a rapid, low-temperature hydrochloric acid (HCl) gas treatment. The primary aim was to develop an energy-efficient "green" cellulose extraction process. Response surface methodology optimized the liquid-phase hydrolysis conditions to 3.3 % HCl at 117 °C for 127 min to obtain MCC with 350 degree of polymerization. An alternative gas-phase approach utilizing gaseous HCl diluted in hot 40 °C air was proposed to accelerate MCC production. The cellulose pulp was moistened to 15-18 % moisture content and then exposed to HCl gas, which was absorbed by the moisture in the cellulose fibers to generate a highly concentrated acidic solution that hydrolyzed the cellulose. The cellulose pulp was isolated from depithed bagasse through soda pulping, multistage bleaching and cold alkali purification. Hydrolysis was conducted by saturating the moist cellulose fibers with gaseous HCl mixed with hot air. Extensive analytical characterization using FT-IR, XRD, SEM, TGA, DSC, particle size, and porosity analyses verified comparable physicochemical attributes between MCC samples prepared via liquid and gas phase methods. The gas-produced MCC revealed 85% crystallinity, 71 Å crystallite dimensions, and thermally stable rod-shaped morphology with an average diameter below 200 μm. The similar material properties validate the proposed gas-based technique as an equally effective yet more energy-efficient alternative to conventional aqueous acid hydrolysis for fabricating highly pure MCC powders from lignocellulose. This sustainable approach enables the value-addition of sugarcane bagasse agro-industrial residue into cellulosic nanomaterials for wide-ranging industrial applications. In summary, the key achievements of this work are rapid MCC production under mild temperatures using HCl gas, optimization of liquid phase hydrolysis, successful demonstration of gas phase method, and extensive characterization verifying equivalence between both protocols. The gas methodology offers a greener cellulose extraction process from biomass.