活性聚丙烯酸丁酯的制备与表征  

Synthesis and Characterization of Living Poly(N-Butyl Acrylate)

作　　者：王伟侠 袁金凤[1] 袁立焕[2] 潘明旺[1] 

机构地区：[1]河北工业大学高分子科学与工程研究所,天津300130 [2]河北盛华化工有限公司,河北张家口075000

出　　处：《高分子材料科学与工程》2014年第5期177-181,共5页Polymer Materials Science & Engineering

基　　金：河北省自然科学基金资助项目(E2011202091)

摘　　要：采用单电子转移-活性自由基聚合(SET-LRP)法合成了活性聚丙烯酸丁酯(L-PBA),采用核磁共振谱仪对其分子结构进行了表征;通过改变单体/引发剂摩尔比,二次引发的单体/大分子引发剂摩尔比,以及多级引发3种途径验证了LPBA具有反应活性,并且发现L-PBA的相对分子质量可以进行控制;当采用L-PBA再次引发BA聚合时,可在较短时间内(3.5h)、单体/大分子引发剂摩尔比较高时(6665/1),获得较高单体转化率(31.3%),表明大分子引发剂比小分子引发剂活性高;凝胶渗透色谱结果还显示,多级引发所得L-PBA的相对分子质量分布,随单体/大分子引发剂摩尔比及引发级数的增加而变宽,当产物相对分子质量达到19万左右时产物相对分子质量分布出现双峰,原因与体系中活性种与休眠种间快速转换的失衡有关。Living poly(n-butyl acrylate) s[L-PBAs]were synthesized by single electron transfer-living radical polymerization[SET-LRP].1H-NMR was employed to characterize the structure of L-PBAs. By investigating various reaction parameters such as monomer/initiator and monomer/macroinitiator feed ratios and using multistep of living polymerization,the reactivity of L-PBAs was confirmed,and the L-PBAs with controllable average molecular weights were achieved. When the L-PBA was transformed into macroinitiator to re-initiate BA polymerization,relative high monomer conversion(31. 3%) was obtained with monomer/macroinitiator mole ratio of 6665/1 at 3. 5 h of polymerization time. The results reveal that the macroinitiators have higher reactivity than the first initiator. From GPC results,it is observed that the molecular weight distribution(MWD) of L-PBA prepared by multistep initiation becomes wider with increasing monomer/macroinitiator mole ratio and/or re-initiation step. As a result,MWD appeares double peaks when the molecular weight reaches 1. 9 × 105,which probably ascribes to an imbalance of fast exchange between active and dormant species.

关 键 词：聚丙烯酸丁酯 单电子转移-活性自由基聚合 相对分子质量 

分 类 号：TQ325.7[化学工程—合成树脂塑料工业]