硫酸/丙醇法制备高取代度纤维素硫酸钠  

Preparation of Cellulose Sulphate with High Substitution Using Concentrated Sulfuric Acid and Propanol

作　　者：方磊[1] 吴小立[2] 林东强[1] 姚善泾[1] 

机构地区：[1]浙江大学化学工程与生物工程学系,浙江杭州310027 [2]宁波港集团有限公司,浙江宁波315800

出　　处：《化学反应工程与工艺》2008年第6期541-544,共4页Chemical Reaction Engineering and Technology

基　　金：国家自然科学基金(20776129;20876139)

摘　　要：以浓硫酸和正丙醇的混合溶液为磺化剂,制备高取代度纤维素硫酸钠(NaCS)。考察了反应液配比、反应时间、反应温度以及液固比对 NaCS 取代度和分子量的影响。随着反应时间的延长,反应温度的提高,浓硫酸在反应液中比例的增加,NaCS 取代度呈现上升趋势,但增大到一定程度,由于副反应加剧以及纤维素的降解,NaCS 分子量下降。结果表明,在硫酸与正丙醇的物质的量之比为2.1,反应液与纤维素的液固质量比为45和反应温度0℃条件下,反应时间16 h,NaCS 取代度可接近1。将反应条件调节在适当的范围内,反应时间控制在2～16 h,可控制 NaCS 取代度在0.3～1.0,分子量在100～2 000 kD。Cellulose sulfate with high degree of substitution was prepared using the mixture of concentrated sulfuric acid and n-propanol as sulphonating agent. Some important factors, such as the ratio of concentrated sulfuric acid to n-propanol in the reactant mixture, reaction time, reaction temperature and ratio of reactant liquor to cellulose, which influenced the degree of substitution and molecular weight of cellulose sulfate, were investigated. It was found that with the increase of reaction time, reaction temperature and the molar ratio of concentrated sulfuric acid to n-propanol, the degree of substitution increased. The optimized conditions were obtained as follows： the molar ratio of concentrated sulfuric acid to n-propanol at 2.1, the mass ratio of reactant liquor to cellulose at 45, reaction temperature at 0 ℃ and reaction time 16 h. Under the optimized condition, the degree of substitution of cellulose sulfate could reach about 1.0. By applying the various preparation conditions （specially reaction time of 2-16 h）, the degree of substitution could be 0.3-1.0, and molecular weight could be 100-2 000 kD.

关 键 词：纤维素硫酸钠 浓硫酸 正丙醇 取代度 分子量 

分 类 号：TQ031[化学工程]