摘要
运用甲苯回流法制备了3-缩水甘油基丙基硅胶键合相,并通过正交实验及单因素实验,探讨了物料配比、反应温度、反应时间等条件对键合相形成的影响规律。结果表明：KH-560含量的适当增加、反应温度的升高、反应时间的延长均能促进键合相的形成。同时还发现反应温度过高、反应时间过长会导致KH-560的分解。适合硅胶和KH-560键合的反应条件是：硅胶︰KH-560=1︰2（质量比）;反应温度65~80℃;反应时间48~72 h。该条件可避免KH-560的分解。最后通过元素分析法所得氢含量与理论计算氢含量的比较,得出KH-560分子上只有1个甲氧基参与了键合反应。
The bonded phase,3-glycidoxypropyl silica gel,was prepared by the method of toluene reflux.The reaction conditions,including material ratio,reaction temperature and reaction time on the formation of bonded phase,were investigated through orthogonal test and one-factor test.The results indicated that the proper increasing of the content of KH-560,the reaction temperature and reaction time could promote the formation of bonded phase.But the results also showed that the overhigh reaction temperature and the overlong reaction time will cause the dissociation of KH-560.The suitable reaction conditions for the formation of silica gel and KH-560 bonded was：silica gel：KH-560 = 1：2（mass ratio）;reaction temperature 65—80 ℃;reaction time 48—72 h.The decomposition of KH-560 can be avoided under this condition.Finally,compared with the hydrogen content between elemental analysis and theoretical calculation,it could be identified that there was only one methoxy group of the KH-560 molecule involved in the bonded reaction.
出处
《化工进展》
EI
CAS
CSCD
北大核心
2012年第6期1263-1268,1273,共7页
Chemical Industry and Engineering Progress
