摘要
以六甲基二硅胺烷(HMDS)作为硅烷化试剂,合成了三甲基硅基羟乙基纤维素。采用红外光谱及核磁共振对产物的结构进行了表征。研究了反应温度、反应时间、共溶剂等因素对羟乙基纤维素甲硅烷基化率的影响。结果表明,当TMCS(三甲基氯硅烷)/OH的摩尔比率为0.2,共溶剂甲苯/DMSO的体积比为2∶3,反应温度为60℃,反应时间为24h,HMDS/OH的摩尔比率为2时,所得三甲基硅羟乙基纤维素的甲硅烷基化率可达到83.2%。并建立了用气相色谱法测定甲硅烷基化率的方法。
Silylation of hydroxyethyl cellulose was produced by as using hexametyyldisilazane(HMDS) as silylation agent. The structure of product was characterized by IR spectrum and NMR spectrum. The effect of TMCS/OH ratio, co- solvent, reaction temperature, reaction time and HMDS/OH ratio on silytation yield was investigated. The results showed that silylation yield of hydroxyl cellulose reached to 83.2% when the molar ratio TMCS/OH was 0. 2 : 1, the volume ratio toluene/DMSO was 2 : 3, medium temperature was 60℃, reaction time was 24h, and the molar ratio HMDS/OH was 2 : 1. The gas chromatograph method for determination of silylation yield of hydroxyethyl cellulose was establised.
出处
《化工新型材料》
CAS
CSCD
北大核心
2008年第9期56-59,共4页
New Chemical Materials
基金
国家自然科学基金项目(20506008)