The possibility of synthesizing nitrocellulose (NC) from an easily renewable non-woody feedstock, Miscanthus, is demonstrated herein. Nitration of Miscanthus cellulose with commercial mixed acid was found to afford high-quality NC: 11.85 % nitrogen content, 18 cP viscosity of 2 % NCacetone solution, 97 % solubility in alcohol-ester mixture, and 0.11 % ash content. The Miscanthus NC structure and fibers were characterized by analytical techniques such as SEM, IR spectroscopy, TGA/DTG, and 13 C NMR spectroscopy. The Miscanthus NC is comparable in quality to basic NC types used for the manufacture of films, membranes, lacquers, nail polish, liquid bandage, artificial silk and skin.
Bacterial nanocellulose (BNC) whose biosynthesis fully conforms to green chemistry principles arouses much interest of specialists in technical chemistry and materials science because of its specific properties, such as nanostructure, purity, thermal stability, reactivity, high crystallinity, etc. The functionalization of the BNC surface remains a priority research area of polymers. The present study was aimed at scaled production of an enlarged BNC sample and at synthesizing cellulose nitrate (CN) therefrom. Cyclic biosynthesis of BNC was run in a semisynthetic glucose medium of 10−72 L in volume by using the Medusomyces gisevii Sa-12 symbiont. The most representative BNC sample weighing 6800 g and having an α-cellulose content of 99% and a polymerization degree of 4000 was nitrated. The nitration of freeze-dried BNC was performed with sulfuric-nitric mixed acid. BNC was examined by scanning electron microscopy (SEM) and infrared spectroscopy (IR), and CN was explored to a fuller extent by SEM, IR, thermogravimetric analysis/differential scanning analysis (TGA/DTA) and 13C nuclear magnetic resonance (NMR) spectroscopy. The three-cycle biosynthesis of BNC with an increasing volume of the nutrient medium from 10 to 72 L was successfully scaled up in nonsterile conditions to afford 9432 g of BNC gel-films. CNs with a nitrogen content of 10.96% and a viscosity of 916 cP were synthesized. It was found by the SEM technique that the CN preserved the 3D reticulate structure of initial BNC fibers a marginal thickening of the nanofibers themselves. Different analytical techniques reliably proved the resultant nitration product to be CN. When dissolved in acetone, the CN was found to form a clear high-viscosity organogel whose further studies will broaden application fields of the modified BNC.
Pretreatment of biomass is a key step in the production of valuable products, including high-tech bacterial cellulose. The efficiency of five different pretreatment methods of Miscanthus and oat hulls for enzymatic hydrolysis and subsequent synthesis of bacterial cellulose (BC) was evaluated herein: Hydrothermobaric treatment, single-stage treatments with dilute HNO3 or dilute NaOH solution, and two-stage combined treatment with dilute HNO3 and NaOH solutions in direct and reverse order. The performance of enzymatic hydrolysis of pretreatment products was found to increase by a factor of 4−7. All the resultant hydrolyzates were composed chiefly of glucose, as the xylose percentage in total reducing sugars (RS) was 1−9%. The test synthesis of BC demonstrated good quality of nutrient media prepared from all the enzymatic hydrolyzates, except the hydrothermobaric treatment hydrolyzate. For biosynthesis of BC, single-stage pretreatments with either dilute HNO3 or dilute NaOH are advised due their simplicity and the high performance of enzymatic hydrolysis of pretreatment products (RS yield 79.7−83.4%).
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