端羟基聚环氧氯丙烷醚的合成及表征  

Synthesis and Characterization of Polyepichlorohydrin with Terminal Hydroxyl

作　　者：孙兆任[1] 顾尧[1] 孙冬冬[1] 

机构地区：[1]青岛科技大学橡塑材料与工程教育部重点实验室,山东青岛266042

出　　处：《含能材料》2010年第1期24-28,共5页Chinese Journal of Energetic Materials

基　　金：国家自然科学基金资助(批准号:20874054)

摘　　要：采用乳液双金属氰化物络合物代替Lewis酸类作为催化剂,使环氧氯丙烷(ECH)开环聚合,制得相对分子质量较高及分子质量分布较窄的聚环氧氯丙烷(PECH),这种PECH可用于高质量的含能叠氮粘合剂中。研究了影响ECH聚合的一些关键因素,包括引发剂的类型及用量,单体的加料方式及催化剂用量等。实验结果表明,PECH的官能度随引发剂的种类而变。而增加催化剂用量及提高反应温度,则可增大PECH的相对分子质量。另外,连续地逐滴加入单体比一次性加入单体较优。当以双酚A为引发剂,催化剂用量为生成PECH量的0.05%,反应温度为128℃时,PECH的收率可大于95%,所得PECH的官能度为2～3,PECH的结构由IR、1HNMR及GPC确认。Using emulsion double metal cyanide （EDMC） complex instead of Lewis acids etc as catalyst the hydroxyl terminated polyepichlorohydrin （PECH） with high relative molecular mass （g4w ） and narrow distribution was synthesized by ring-opening polymerization of epichlorohydrin （ECH）. The PECH obtained can be used to prepare energetic azide binders with top quality. The key factors influencing the ECH＇s polymerization were studied, including initiators, addition method of monomer, dosage of catalysts,and reaction time. Results show that the functionality of PECH varies as types of initiators. The increase of catalyst dosage and the rise of reaction temperature result in higher Mw of PECH. To add the monomer droprise continuosly could be helpful to improve the polymerization. The yield of PECH reaches more than 95% on the conditions listed below： bisphenol A as initiator, catalyst dosage of 0.05% （based on resulting PECH mass） ,reaction temperature of 128 ℃. The Mw of PECH can be adjusted by varying the molar ratio of monomer to initiator. The functionality of the synthesized PECH was calculated based on f= （OH value/ MW）/56100 and found to be of 2 -3. The PECH structure was identified by FTIR,^1H NMR,and GPC.

关 键 词：高分子化学 环氧氯丙烷 开环聚合 双金属氰化物 

分 类 号：TQ433[化学工程]