Department of Biotechnology and Bioengineering, Huaqiao University, Xiamen 361021, PR China.
Carbohydr Polym. 2013 Jun 5;95(1):332-7. doi: 10.1016/j.carbpol.2013.03.003. Epub 2013 Mar 13.
An improved process for production of cellulose sulfate (CS) was developed by using sulfuric acid/ethanol solution as sulfonating agent and Na2SO4 as water absorbent. The FTIR, SEM and TG analysis were used to characterize the CS prepared. The total degree of substitution and viscosity of the product solution (2%, w/v) were ranging from 0.28 to 0.77 and from 115 to 907 mPa s, respectively, by changing the process parameters such as the amount of Na2SO4, the reaction time, the temperature, the sulfuric acid/alcohol ratio and liquid/solid ratio. The results indicated that the product with DS (0.28-0.77) and η2% (115-907) mPa s could be produced by using this improved process and more cellulose sulfate could be produced when cellulose was sulfonated for 3-4 h at -2 °C in sulfuric acid/ethanol (1.4-1.6) solution with addition of 0.8 g Na2SO4. The (13)C NMR indicated that the sulfate group of CS produced using sulfuric acid/ethanol solution was at C6 position.
采用硫酸/乙醇溶液作为磺化剂、硫酸钠作为水吸收剂,开发了一种改进的纤维素硫酸酯(CS)生产工艺。通过改变工艺参数,如硫酸钠用量、反应时间、温度、硫酸/醇比和液固比,对所制备的 CS 进行 FTIR、SEM 和 TG 分析。结果表明,该方法可以制备取代度为 0.28-0.77、2%(w/v)溶液黏度为 115-907 mPa·s 的产物。当纤维素在硫酸/乙醇(1.4-1.6)溶液中于-2℃下磺化 3-4 h,加入 0.8 g 硫酸钠时,可得到取代度为 0.28-0.77、2%(w/v)溶液黏度为 115-907 mPa·s 的更多纤维素硫酸酯。13C NMR 表明,用硫酸/乙醇溶液制备的 CS 的硫酸根基团位于 C6 位。