新型阳离子光固化活性单体3,3′-[1,4-丁基双(氧基亚甲基)]-双-(3-乙基)氧杂环丁烷的合成  

Study on the Synthesis of 3,3′-[1,4-Butanediylbis(oxymethylene)] bis[(3-ethyl)oxetane] for the Novel Cationic Curing Monomer

作　　者：万时策 黄笔武[1] 杜志鹏[1] 雍涛[1] 韩文娟[1] 

机构地区：[1]南昌大学材料科学与工程学院,江西南昌330031

出　　处：《影像科学与光化学》2016年第2期181-189,共9页Imaging Science and Photochemistry

基　　金：国家自然科学基金资助项目(51563017)

摘　　要：以3-乙基-3-羟甲基氧杂环丁烷(OXT101)和1,4-二溴丁烷为原料,四正丁基溴化铵为相转移催化剂,在碱性条件下合成了一种新型阳离子光固化活性单体3,3′-[1,4-丁基双(氧基亚甲基)]-双-(3-乙基)氧杂环丁烷。研究表明,其合成最佳工艺条件为:当1,4-二溴丁烷用量为0.2mol时,1,4-二溴丁烷与3-乙基-3-羟甲基氧杂环丁烷摩尔比为1∶2.5,四正丁基溴化铵2g,KOH提供碱环境,用量为1.0mol,0℃下反应时间24h。在此条件下,产率达49.3%。同时,对合成的活性单体的固化机理及其稀释性能进行了研究,结果表明新型活性单体的固化机理为阳离子开环聚合,稀释性能可与目前市场上常用的阳离子活性单体媲美,具有一定的工业实用价值。A novel cationic curing reactive monomer, 3,3＇-1-1,4-butanediylbis （oxymethylene） ] bis [- （ 3-ethyl）- oxetane], was synthesized with 3-ethyl-3-hydroxymethyl oxetane and 1,4-dibromobutane as raw materials, tera-n-butylammonium bromide as phase-transfer catalysts in the alkaline conditions. The optimum conditions were set as the amount of 1,4-dibromobutane was 0. 2 mol, the molar ratio of 1,4-dibromobutane and 3-ethyl-3- hydroxylmethyl oxetane was 1 ： 2. 5, the amount of tera-n-butylammonium bromide was 2 g, the alkaline condition offered by 1.0 mol potassium hydroxide and the reaction time was 24 hours at 0 ℃. Under such conditions, the yield of 3, 3＇-[- 1, 4-butanediylbis-（ oxymethylene）-] bis [ （3-ethyl） oxetane ] was obtained as 49.3%. Meanwhile, the curable mechanism and the property of dilution of the novel cationic reactive monomer were studied. The result showed that, the curing mechanism of the novel monomer is attributed to the cationic ring-open polymerization and it has the similar dilute compared with commercial common monomers.

关 键 词：阳离子活性单体 3 3′-[1 4-丁基双(氧基亚甲基)]-双-(3-乙基)氧杂环丁烷 紫外光固化 

分 类 号：TQ637[化学工程—精细化工]