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纸质出版日期:2008-10-20,
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魏志勇, 刘炼, 王沛, 高军, 齐民. 辛酸镁催化L-丙交酯与ε-己内酯共聚及其共聚物结构与性能研究[J]. 高分子学报, 2008,(10):947-954.
WEI Zhiyong, LIU Lian, WANG Pei, GAO Jun, QI Min. STUDIES ON COPOLYMERIZATION OF L-LACTIDE WITH ε-CAPROLATONE CATALYZED BY MAGNESIUM OCTOATE AND THE STRUCTURE AND PROPERTIES OF THE COPOLYMERS[J]. Acta Polymerica Sinica, 2008,(10):947-954.
魏志勇, 刘炼, 王沛, 高军, 齐民. 辛酸镁催化L-丙交酯与ε-己内酯共聚及其共聚物结构与性能研究[J]. 高分子学报, 2008,(10):947-954. DOI: 10.3724/SP.J.1105.2008.00947.
WEI Zhiyong, LIU Lian, WANG Pei, GAO Jun, QI Min. STUDIES ON COPOLYMERIZATION OF L-LACTIDE WITH ε-CAPROLATONE CATALYZED BY MAGNESIUM OCTOATE AND THE STRUCTURE AND PROPERTIES OF THE COPOLYMERS[J]. Acta Polymerica Sinica, 2008,(10):947-954. DOI: 10.3724/SP.J.1105.2008.00947.
以无毒性的辛酸镁为催化剂催化L-丙交酯和ε-己内酯本体开环共聚合,制备了一系列不同单体配比的共聚物.首先用1H-NMR跟踪了共聚合单体转化率,显示L-LA聚合速率显著快于ε-CL.用13C-NMR分析共聚物微观结构和计算单体单元平均序列长度(LLLe和LCe),表明聚合过程中酯交换反应导致单元序列结构重新分布.随着反应进行,LLLe急剧下降而LCe逐渐增加后稍有降低,游程数逐渐增大,共聚物无规度提高.反应初期主要是一级酯交换反应,二级酯交换反应导致的CLC序列结构在反应后期才观察到.由Fineman_Ross法计算出L-丙交酯和ε-己内酯的竞聚率分别为rLA=23和rCL=0.22,表明在聚合反应初期LLA单体优先插入聚合物增长链端,形成LL单元长嵌段结构.共聚物组成显著影响单元序列长度,各序列长度随相应单体加入量增加而增长.二级酯交换系数(TIICLC])随ε-CL含量增加而增大.对于整个组成范围内,根据竞聚率计算的LLLr值始终要大于聚合产物的LLLe,而LCr计算值小于或接近LCe实验值.因此,共聚物单元序列分布随共聚物投料比和反应时间而改变,趋向于无规分布.以DSC和XRD分析了共聚物热性能和结晶性,表明共聚物结晶性与单元序列长度密切相关.所有共聚物只有一个玻璃化转变温度Tg,符合无规共聚物的Fox方程,说明所得共聚物为无规共聚物,或者说包含有相容性嵌段成分的共聚物.
Poly(L-lactide-co-ε-caprolactone) P(LLA-co-CL) copolymers with various L-lactide/ε-caprolactone(L-LA/ε-CL) mole ratios were prepared by the ring opening copolymerization of L-LA andε-CL using nontoxic magnesium octoate as a catalyst in bulk.The time-conversion curves of L-LA and ε-CL copolymerization were recorded by1HNMR.The results showed significantly more rapid polymerization of LLA relative to ε-CL.The carbonyl carbon signals in 13C-NMR are most sensitive to the sequence distributions of the lactidyl and caproyl units and used for calculating their average block length (LLLe and LCe).Two modes of transesterification occurred during the copolymerization process and played an important role in the redistribution of comonomer sequences.With polymerization progress
LLLe decreased sharply andLCe increased at first and then decreased gradually
as a result
the run number (R) increased gradually and the extent of randomness enhanced.The CLC sequence formed by the second mode of transesterification was observed at the end of reaction.Then
the reactivity ratios of L-LA and ε-CL were measured to berLA=23 and rCL=0.22
respectively
using the FinemanRoss method.The results(rLA1 and rCL 1) imply that Llactide monomer added preferentially into the copolymer chain end in the first step of the reaction
resulting in the formation of long blocks of lactidyl unit in the polymer chain.The copolymer composition has a profound influence on the values ofLLLe and LCe.Both LLLe and LCe increased as the relative proportions of their respective monomers increased.The transesterification coefficient of the second mode of lactidyl units(TⅡ[CLC]) increased as the feed mole fraction of ε-CL increased.In terms of the overall feed compositions
the LLLr values calculated from the reactivity ratio exceeded the LLLe values determined from the product; however
the LCr values were identical or shorter than the LCe values.Therefore
the repeat unit sequence distribution of the copolymers was varied more or less toward a random sequence distribution by variation in the comonomer feed ratio and reaction time.The thermal properties and crystallization of the copolymers were investigated by DSC and XRD.The results showed that a close relationship between copolymer crystallinity and the length of the copolymer sequences.All copolymers of L-LA and ε-CL exhibited a single Tgsdetermined from the second heating scan.The experimental Tgswere in agreement with the calculated Tgsvalues from Fox equation.It can be concluded that the copolymers are random
or comprise a mixture of compatible block copolymers.
聚(L-丙交酯-co-ε-己内酯)辛酸镁竞聚率酯交换微观结构性能
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