聚乙二醇与二氯亚砜反应合成氯代聚乙二醇过程研究Synthesis of Chloro-Terminated Polyethylene Glycol via Reaction of Polyethylene Glycol and Thionyl Chloride
王宜涛,张舜光,甄彬,侯凯湖
摘要(Abstract):
以吡啶为缚酸剂,二氯亚砜为氯化试剂对不同聚合度的聚乙二醇(PEG)进行端羟基取代,研究了反应过程中缚酸剂用量、反应温度、时间和聚乙二醇聚合度等条件对PEG转化率和氯代聚乙二醇(PEGCl)收率的影响;采用羟值测定、傅里叶变换红外光谱、核磁共振氢谱等技术对PEGCl的结构进行了分析。结果表明,在二氯亚砜、吡啶和聚乙二醇摩尔比为6:6:1时,PEG基本全部转化;在反应温度35~45℃,PEGCl的收率较高;随着反应时间延长,PEG转化率逐渐提高,但若反应时间过长则生成较多副产物,使PEGCl收率降低;当聚乙二醇聚合度较高时,氯化反应速率更快。经分析红外光谱和核磁共振氢谱表征可知,所得产物纯度较高。
关键词(KeyWords): 氯代反应;聚乙二醇;二氯亚砜;缚酸剂
基金项目(Foundation):
作者(Author): 王宜涛,张舜光,甄彬,侯凯湖
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