聚乙二醇类单体的制备及其生物相容性测定

聚乙二醇类单体是合成功能性高分子材料的重要单体。直接酯化法是合成此类单体的主要方法,但利用该法所制备产物的双键保留率偏低。针对这一问题,本文以聚乙二醇单甲醚-200和丙烯酸为原料,在携水剂存在的同时,向反应体系中引入变色硅胶,提高了直接酯化法去除生成水的效率,制备出了高双键保留率、高产率的聚乙二醇单甲醚-200丙烯酸酯(MPEGA-200),并采用红外光谱、1H NMR对产物进行了表征,采用过氧化氢酶评价了产物的生物相容性。通过正交实验确定了最佳合成条件为:醇酸摩尔比1:2,催化剂对甲苯磺酸和阻聚剂对苯二酚加量均为2%,变色硅胶占醇酸总质量的12%,携水剂石油醚60~90加量为18%,反应温度120℃,反应时间6h。在此条件下,酯化率可达95.47%,MPEGA-200的双键保留率为95.45%,产率为87.68%。另外,本文还采用单因素法研究了各反应条件对酯化反应的影响规律。

Synthesis and Biotoxicity Evaluation of Polyethylene Glycol Monomer

Polyethylene glycol monomer is an important monomer for the synthesis of functional polymer materials.The direct esterification method is one of the main methods for synthesizing such monomers,but the product prepared by this method has a low double bond retention rate.To solve this problem,in this study,Polyethylene glycol monomethyl ether-200 acrylate(MPEGA-200)with high yield and high double bond retention was synthesized by direct esterification of methoxy polyethylene glycol(MPEG-200)with acrylic acid(AA),and by introducing color-changing silica gel into the reaction system based on the presence of a water-carrying agent to enhance the water removal efficiency.FT-IR and 1H NMR were used to characterize MPEGA-200,and the biocompatibility of MPEGA-200 was evaluated by catalase activity analysis.The optimal conditions for synthesizing MPEGA-200 were determined by orthogonal experiments.The results shown that the optimal conditions are:n(MPEG-200):n(AA)=1:2,the additions of inhibitor and catalyst were 2%(based on the total acid and alcohol mass),18%of petroleum ether and 12%of color-changing silica gel,the reaction time was 6h,and the esterification temperature was 120℃.Under the conditions,95.47%of esterification rate,95.45%of double bond retention and 87.68%of yield can be reached.In addition,the influences of various factors on esterification were studied by the single factor method.