2,3-二甲基纤维素的制备与表征  

Preparation and Characterization of 2,3-Dimethyl Cellulose

作　　者：宫大军 陈卫平 李博 叶应庆 白岩 GONG Da-jun;CHEN Wei-ping;LI Bo;YE Ying-qing;BAI Yan(Kun Shan JingKun Chemistry Company,Kunshan 215300,China;China Petroleum GreatWall Drilling Kunshan Company,Kunshan 215300,China;JiangSu Engineering Research Center for Plant Polysaccharide Gums,Kunshan 215300,China)

机构地区：[1]昆山京昆油田化学科技有限公司,江苏昆山215300 [2]中国石油长城钻探工程有限公司昆山公司,江苏昆山215300 [3]江苏省多糖植物胶工程技术研究中心,江苏昆山215300

出　　处：《纤维素科学与技术》2023年第1期60-70,共11页Journal of Cellulose Science and Technology

摘　　要：以溶解的纤维素为原料,三苯氯甲烷作为定向取代试剂取代纤维素的6位羟基,制备6-三苯甲基纤维素。采用^(13)C-NMR、FT-IR对其进行了表征,结果表明三苯基氯甲烷实现了纤维素6位羟基完全取代。以6-三苯甲基纤维素作为原料,通过甲基化,脱除三苯甲基保护基团,制备了2,3-二甲基纤维素,采用13C-NMR、GC-MS、FT-IR等表征方法对样品进行了表征,并考察了反应温度与时间、甲基化试剂与糖结构单元摩尔比对2,3-二甲基-纤维素取代度的影响。结果表明,^(13)C-NMR、GC-MS两种表征方法表征2,3-二甲基-纤维素的取代分布具有较好的一致性,2,3-二甲基-纤维素取代度随着反应温度的升高、反应时间的延长、甲基化试剂与糖结构单元的摩尔比提升呈一定的递增关系。The performance of the polysaccharide compound relates to not only the degree of the substituent groups but also the position of the hydroxyls.The different location of the substituent groups can lead to the different intermolecular interactions between the hydrogen bonds of the polysaccharide compound.Therefore the performance of the polysaccharide compound can also be affected.Based on the relationship between the performance and the location of the substituent groups,2,3-dimethyl cellulose is prepared and is used as the research object to study the structure and the performance of the polysaccharide compound.In this paper,the dissolution conductions of the cellulose in the lithium chloride/N,N-dimethylacetamide is firstly studied and then the structure of the cellulose is characterized by ^(13)C-NMR.Using the dissoluted cellulose as the material,triphenyl methyl chloride as a directional replace reagent to replace the sixth hydroxy of the cellulose and 6-triphenyl cellulose is prepared.The structure of it is characterized by ^(13)C-NMR and FT-IR.The influence of the reaction temperature,the reaction time,the molar ratio of methylation reagent to the sugar structure on the substitution degree of the 2,3-dimethyl-cellulose are examined.The results showed that it has good consistency for the two methods of 13C-NMR and GC-MS to the substitution distribution of 2,3-dimethyl-cellulose.With the increase of the temperature,the longer of the reaction time,the increase mole ratio of the methylation reagent to the sugar structure,the substitution degree of 2,3-dimethyl-cellulose is also increased.

关 键 词：纤维素 定向取代 三苯基氯甲烷 甲基化 定向保护 脱保护 

分 类 号：TQ352.79[化学工程]