在单模聚焦微波辐射作用下,以辛酸亚锡为催化剂,炔丙醇为小分子引发剂引发L-丙交酯开环聚合合成了端炔基修饰的聚(L-丙交酯).通过正交实验考察了各种反应条件对产物产率的影响,得出最佳的聚合反应条件如下:反应温度110℃,微波功率45W,辐照时间45min,催化剂用量0.1%.在此基础上,通过改变n(L-丙交酯)∶n(炔丙醇)投料比合成了一系列端炔基修饰的聚(L-丙交酯),通过FT-IR、1 H NMR、DSC、XRD和GPC对其结构与性能进行了研究.结果表明,在微波作用下,快速、高效地合成了端炔基修饰的聚(L-丙交酯)目标产物,且产物的结构与性能可以通过改变n(L-丙交酯)∶n(炔丙醇)投料比在一定程度上进行调控,随着L-丙交酯投料量增大,产物的分子量逐渐增大,熔点逐渐升高.
参考文献
[1] | Joo-Eon Park;Mitsugu Todo .Development and characterization of reinforced poly(L-lactide)scaffolds for bone tissue engineering[J].Journal of Materials Science. Materials in Medicine,2011(5):1171-1182. |
[2] | 刘淑琼,肖秀峰,刘榕芳,林月红,钟章裕,焦简金.热致相分离制备聚乳酸纳米纤维支架[J].高等学校化学学报,2011(02):372-378. |
[3] | Parrish, B;Breitenkamp, RB;Emrick, T .PEG- and peptide-grafted aliphatic polyesters by click chemistry[J].Journal of the American Chemical Society,2005(20):7404-7410. |
[4] | Bryan Parrish;Todd Emrick .Aliphatic Polyesters with Pendant Cyclopentene Groups:Controlled Synthesis and Conversion to Polyester-graft-PEG Copolymers[J].Macromolecules,2004(16):5863-5865. |
[5] | Eliska Tresohlava;Stepan Popelka;Ludka Machova .Modification of Polylactide Surfaces with Lactide-Ethylene Oxide Functional Block Copolymers: Accessibility of Functional Groups[J].Biomacromolecules,2010(1):68-75. |
[6] | Vsevolod V.Rostovtsev;Luke G.Green;Valery V.Fokin;K.Barry Sharpless .A stepwise huisgen cycloaddition process:copper(I)-catalyzed regioselective"ligation" of azides and terminal alkynes[J].Angewandte Chemie International Edition,2002(14):2596-2599. |
[7] | Himo F.;Demko ZP.;Noodleman L.;Sharpless KB. .Mechanisms of tetrazole formation by addition of azide to nitriles[J].Journal of the American Chemical Society,2002(41):12210-12216. |
[8] | Hartmuth C. Kolb;K. Barry Sharpless .Click chemistry: diverse chemical function from a few good reactions[J].Angewandte Chemie International Edition,2001(11):2004-2021. |
[9] | Binder WH;Sachsenhofer R .'Click' chemistry in polymer and materials science[J].Macromolecular rapid communications: Publishing the newsletters of the European Polymer Federation,2007(1):15-54. |
[10] | Victoria D.Bock;Rossana Perciaccante;T.Paul Jansen;Henk Hiemstra;Jan H.van Maarseveen .Click Chemistry as a Route to Cyclic Tetrapeptide Analogues: Synthesis of cyclo-[Pro-Val-psi (triazole)-Pro-Tyr][J].Organic letters,2006(5):919-922. |
[11] | Noodleman L;Sharpless K B;Fokin V V et al.Copper (Ⅰ)-catalyzed synthesis of azoles DFT study predicts unprecedented reactivity and intermediates[J].Journal of the American Chemical Society,2005,127:210-216. |
[12] | 曾庆慧,罗丙红,杨媛,赵剑豪,周长忍.低温常压下高分子量左旋聚乳酸的微波合成及表征[J].功能材料,2007(06):972-975. |
[13] | Luo B H;Yang J;Zhao J H et al.Rapid synthesis and characterization of chitosan-g-poly (D,L-lactide) copoly mers using hydroxyethyl chitosan as macroinitiator under microwave irradiation[J].Journal of Applied Polymer Science,2012,125:E125-E131. |
[14] | 罗丙红,钟翠红,徐宠恩,焦延鹏,周长忍.单模聚焦微波辐射酶促合成PLA-PEG-PLA三嵌段共聚物[J].功能材料,2011(01):21-24,29. |
[15] | 何柱国,罗丙红,周长忍,程松,张奕,钟翠红.微波辅助壳聚糖接枝聚乳酸共聚物的合成及表征[J].应用化学,2009(10):1134-1138. |
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