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1、第22卷第2期高校化学工程学报No.2Vol.222008年4月JournalofChemicalEngineeringofChineseUniversitiesApr.2008文章编号:1003-9015(2008)02-0299-06窄分子量分布的聚[甲基(3,3,3-三氟丙基)硅氧烷]的合成与表征1,211易玲敏,詹晓力,陈丰秋(1.浙江大学化学工程与生物工程学系,浙江杭州310027;2.浙江理工大学先进纺织材料与制备技术教育部重点实验室,浙江杭州310018)摘要:聚[甲基(3,3,3-三氟丙基)硅氧烷](PMT
2、FPS)具有非常优越的物理化学性能,是一种有着重要应用价值的有机硅′′′材料。研究以正丁基锂与1,3,5-三甲基-1,3,5-三(3,3,3-三氟丙基)环三硅氧烷(简称F3)反应所得硅醇锂为引发剂,在正己烷与THF的混合溶剂中,在较高的单体浓度下实现了F3的可控阴离子开环聚合,得到了窄分子量分布(1.03~1.08)的含氯苄端基的聚[甲基(3,3,3-三氟丙基)硅氧烷](PMTFPS-BzCl),聚合物得率在93%以上。结果显示,在F3的开环聚合过程中聚硅氧烷活性链的“反咬”与再分布副反应得到有效的抑制。关键词:聚甲基三氟
3、丙基硅氧烷;阴离子聚合;开环聚合;活性聚合;可控聚合中图分类号:O634.4;TQ316.341文献标识码:ASynthesisandCharacterizationofPoly[methyl(3,3,3-trifluoropropyl)siloxane]withNarrowMolecularWeightDistribution1,211YILing-min,ZHANXiao-li,CHENFeng-qiu(1.DepartmentofChemicalandBiochemicalEngineering,ZhejiangUn
4、iversity,Hangzhou310027,China;2.KeyLaboratoryofAdvancedTextileMaterialsandManufacturingTechnologyofMinistryofEducation,ZhejiangSci-TechUniversity,Hangzhou310018,China)Abstract:Poly[methyl(3,3,3-trifluoropropyl)siloxane](PMTFPS)isanimportantsiliconematerialwithgrea
5、tvalueduetoitssuperiorphysicalandchemicalproperties.Inthisstudy,usingthehigh-vacuumpolymerizationtechniqueandtheco-solventofhexaneandTHFat0℃,thecontrolledanionicring-openingpolymerization(ROP)of1,3,5-trimethyl-1,3,5-tris(3’,3’3’-trifluoropropyl)cyclotrisiloxane(F3
6、)wascarriedout,andthenthebenzylchloride-terminalpoly[methyl(3,3,3-trifluoropropyl)siloxane](PMTFPS-BzCl)wassynthesized.TheinitiatorusedfortheROPisthelithiumsilanolatewhichwasmadedirectlybythereactionofn-butyllithiumandF3inthereactoratroomtemperaturebeforepolymeriz
7、ation.Theobtainedpolymers,PMTFPS-BzCl,hasnarrowmolecularweightdistributionwithdistributionrangof1.03to1.08,anditsyieldismorethan93%.Itindicatesthat,usingtheproposedsynthesisprocess,the“back-biting”bythechainendsaswellastheredistributionreactionsbetweenthesiloxanec
8、hainswereefficientlysuppressedduringtheanionicROPofF3.Keywords:poly[methyl(3,3,3-trifluoropropyl)siloxane];anionicpolymerization;ring-openingpolymerizat