Properties of cellulose nitrates produced by nitration of bacterial cellulose using mixed sulfuric-nitric acids

P. A. Gorbatova, A. Korchagina, Yu. A. Gismatulina, N. Shavyrkina, V. Budaeva
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Abstract

   The study set out to investigate the chemical functionalization of bacterial cellulose as an alternative means of satisfying the high demand for nano-sized cellulose nitrates.   Using a Medusomyces gisevii Sa-12 symbiotic culture as a microbial producer, bacterial cellulose having a polymerization degree of 3950 was obtained on a synthetic glucose medium. Nitration was carried out using mixed sulfuric-nitric acids differing in their water content, followed by stabilization of the synthesized bacterial cellulose nitrates. Subject to a varying water content (14, 16 and 20 %) in the nitrating mixture, the obtained bacterial cellulose nitrates exhibited a nitrogen mass content of 8.68–11.56 %, a solubility in alcohol-ether mixture of 16.5–91.0 % and a viscosity of 32–255 mPa×s. The bacterial cellulose nitrate fibers were shown to have a nanoscale nature. Coupled thermogravimetric and differential thermal analyses revealed the bacterial cellulose nitrates to have a high chemical purity and energy content. FTIR spectroscopy confirmed the high quality of the bacterial cellulose based on the presence of basic functional groups characteristic of conventional cellulose: 3371, 2943, 1633, 1428, 1371, 1163, and 1112 cm-1. According to their infrared spectra, the detected basic functional groups corroborate that the synthesized products are low-substituted cellulose nitrate esters: 1660–1643, 1282-1276, 847–837, 752–749, and 691–690 cm-1. The relationship between the properties of the synthesized bacterial cellulose nitrates and the water mass content in mixed sulfuric-nitric acids is shown to have a complex nature.
使用混合硫酸-硝酸硝化细菌纤维素所产生的纤维素硝酸盐的性质
这项研究旨在研究细菌纤维素的化学功能化,以此作为满足对纳米级纤维素硝酸盐的高需求的替代方法。 使用吉赛酵母菌 Sa-12 共生培养物作为微生物生产者,在合成葡萄糖培养基上获得了聚合度为 3950 的细菌纤维素。使用含水量不同的混合硫酸-硝酸进行硝化,然后稳定合成的细菌纤维素硝酸盐。根据硝化混合物中不同的含水量(14%、16% 和 20%),得到的硝酸纤维素细菌的氮含量为 8.68-11.56%,在醇醚混合物中的溶解度为 16.5-91.0%,粘度为 32-255 mPa×s。研究表明,硝酸纤维素细菌纤维具有纳米级性质。热重分析和差热分析显示,细菌硝酸纤维素具有很高的化学纯度和能量含量。傅立叶变换红外光谱证实了细菌纤维素的高质量,因为它含有传统纤维素特有的基本官能团:3371、2943、1633、1428、1371、1163 和 1112 cm-1。根据它们的红外光谱,检测到的基本官能团证实了合成产物是低取代纤维素硝酸酯:1660-1643、1282-1276、847-837、752-749 和 691-690 cm-1。合成的细菌纤维素硝酸酯的性质与混合硫酸-硝酸中水质量含量之间的关系具有复杂性。
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