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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。
With hexamethyldisilazane (HMDS) as a silylating reagent, trimethylsilyl hydroxyethyl cellulose was synthesized. The structure of the product was characterized by infrared spectroscopy and nuclear magnetic resonance. The effects of reaction temperature, reaction time and cosolvent on the silylation rate of hydroxyethyl cellulose were studied. The results showed that when the molar ratio of TMCS (trimethylchlorosilane) / OH was 0.2, the volume ratio of toluene / DMSO as cosolvent was 2: 3, the reaction temperature was 60 ℃ and the reaction time was 24 h, the molar ratio of HMDS / OH When 2, the resulting trimethylsilyl hydroxyethyl cellulose silylation rate of up to 83.2%. A method for the determination of the silylation rate by gas chromatography was established.