季戊四醇二丙烯酸酯的合成.pdf

2013年第42卷第8期石油化工 PETROCHEMICAL TECHNOLOGY ·891· 季戊四醇二丙烯酸酯的合成祁元春,董擎之(华东理工大学材料科学与工程学院特种功能高分子材料及其相关技术教育部重点实验室,上海200237) [摘要]采用直接酯化法,以对甲苯磺酸为催化剂、对苯二酚/无水CuSO。为阻聚剂、甲苯为溶剂、丙烯酸和季戊四醇为原料合成了季戊四醇二丙烯酸酯(PEDA),考察了阻聚剂种类及用量、催化剂用量、原料配比和溶剂用量对酯化反应的影响,得出了最佳合成条件:以质量比为l:1的对苯二酚/%(占反应物总质量,下同),%,,甲苯用量为50%,反应温度120℃,反应时间4 h。在此条件下,粗产物收率为70%,PEDA收率为52%。将粗产物进行层析分离,通过HPLC,1H NMR,MS,FTIR等手段对粗产物中各组分进行定性、定量分析:定结果可知,PEDA的纯度由分离前的74%提高至U99%。[关键词]季戊四醇二丙烯酸酯;丙烯酸;季戊四醇;对甲苯磺酸;直接酯化法[文章编号]1000—8144(2013)08—0891—06 [中图分类号]TQ [文献标志码]A Synthesis ofPentaerythritol Diacrylate Oi Yuanchun,Dong Qingzhi (Key Laboratory forSpecially Functional Polymers and Related Technology ofMinistry ofEducation。College ofMaterials Science and Engineering,East China University ofScience and Technology,Shanghai 200237,China) [Abstract]Pentaerythritol diacrylate(PEDA)was synthesized by directesterification from acrylic acidand pentaerythritol with toluene-p—sulfonic acid asthecatalyst,hydroquinone/anhydrous copper sulfate astheinhibitor system and toluene asthesolvent。The effectsofinhibitors,catalyst dosage, mole ratioofacrylic acid topentaerythritol and solvent dosage on theesterification were studied. Under theoptimum conditions ofhydroquinone/anhydrous copper sulfatewith mass ratio1:1 posite inhibitor system %(based on thetotalmass ofthereactants,the same blow),toluene-p— sulfonic acid asth