微波辐射合成聚乳酸及其聚乙二醇共聚物的研究  

Microwave-irradiated Preparation of Poly(D,L-lactide acid)and Poly(D,L-lactide acid)-co-poly(ethylene glycol)Copolymer

作　　者：舒静[1] 李丽丽[1] 赵昱博 SHU Jing;LI Lili;ZHAO Yubo(College of Chemistry and Chemical Engineering,Northeast Petroleum University,Daqing 163318,China;DaQing Shiyan High School,Daqing 163318,China)

机构地区：[1]东北石油大学化学化工学院,黑龙江大庆163318 [2]大庆实验中学,黑龙江大庆163318

出　　处：《塑料工业》2022年第4期42-46,共5页China Plastics Industry

基　　金：中国博士后科学基金资助项目(20070410878);黑龙江省博士后落户基金资助项目(LBH-Q09193)。

摘　　要：通过微波辐射在常压、无惰性气体保护条件下合成了聚乳酸及其共聚物。考察了辅助加热介质的种类、引发剂用量、微波功率和辐射时间以及共聚单体聚乙烯醇(PEG)的用量等条件和参数,对真空和常压下的产物分子量进行了对比,测定了均聚物和共聚物的拉伸强度和断裂伸长率,对产物结构采用傅立叶红外光谱(FTIR)和核磁共振氢谱(^(1)H NMR)进行了确认和分析,采用差示扫描量热仪(DSC)测定了产物的玻璃化转变温度(T_(g))。结果表明,采用微波辐射的方式,可以在450 W功率下,仅需18 min和40 min就可制备得到分子量超过20万的乳酸均聚物和共聚物,且无须真空或惰性气体保护。与传统加热法相比,反应时间大大缩短,操作简单,能耗小,能大幅度地降低生产成本。FTIR和^(1)H NMR的表征结果验证了均聚物和共聚物的结构。DSC分析结果显示,随着PEG的加入使产物的T_(g)下降。产物的力学性能测试表明,聚乙烯醇的引入,可以调控材料的强度和韧性,对拓展材料的应用具有积极的意义。Poly(D,L-lactide)acid(PLA)and poly(D,L-lactide)-co-poly(ethylene glycol)copolymer(PELA)were prepared by microwave-irradiation under atmospheric pressure without inert gas.The conditions and parameters of assisted heating-medium,initiator concentration,microwave power level,reaction time and poly(ethylene glycol)(PEG)concentration were discussed.The molecular weight of products prepared under high vacuum and atmospheric pressure were compared.The tensile strength and elongation at break of homopolymer and copolymer were determined.The structure of product were analyzed by Fourier transform infrared spectroscopy(FTIR)and nuclear magnetic resonance(^(1)H NMR).The glass transition temperature(T_(g))of the product was determined by differential scanning calorimeter(DSC).The results show that PLA and PELA with viscosity average molecular weight(Mη)of 2.49×10^(5) and 2.22×10^(5) are obtained at 450 W respectively for 18 min and 40 min without the protection of inert gas.Comparing with conventional thermal method,this method has advantages of rapid polymerization rate,simple process,low energy exhaust and low cost.The structure of PLA and PELA are verified by FTIR and ^(1)H NMR.The results of DSC indicate that T_(g) decreases with the contents of PEG increasing.The strength and toughness of polymer could be controlled by PEG.It has positive significance to expand the application of materials.

关 键 词：微波 聚乳酸 聚乙烯醇 共聚物 常压 

分 类 号：TQ316.313[化学工程—高聚物工业]