表面含苄基磺酸基的介孔分子筛MCM-41-B-S催化合成多缩乙二醇双丙烯酸酯

Catalytic Synthesis of Di-tri-ethylene Glycol Diacrylate on Mesoporous MCM-41 Functionalized with Benzylsulfonic Acid Groups

以表面含有苄基磺酸基的介孔分子筛(MCM-41-B-S)为催化剂,采用直接酯化法合成了二(三)乙二醇双丙烯酸酯,探讨了各反应条件对反应的影响。结果表明,合成一缩乙二醇双丙烯酸酯(DEGDA)的反应温度在110～115℃,丙烯酸(AA)与二乙二醇(DEG)的摩尔比为2.1∶1,催化剂用量为AA质量的1.5%,带水剂甲苯用量为反应总质量的20%,阻聚剂对苯二酚的用量为AA质量的0.8%和回流时间为90min的优化条件下,DEGDA总收率可达94%以上,纯度大于98%。且产品外观质量好,催化剂易与产物分离,纯化工艺简单,产品产率高于均相强酸做催化剂的产率。并用X-射线衍射(XRD)、红外光谱(IR)、差示扫描量热(DSC)和Hammett指示剂对催化剂的结构和酸强度进行了表征和测定。

Di-tri-ethylene glycol diacrylate was prepared from acrylic acid（AA） and di-tri-ethylene glycol through direct esterification catalyzed by benzylsulfonic acid functionalized MCM-41 molecular sieve（MCM-41-S-B）.The effects of reaction condtions were investigated.It was found that MCM-41-S-B as catalyst was superior to sulphuric acid and other protonic acids in the esterification of AA with di-tri-ethylene glycol.The results showed that under the optimum conditions of molar ratio of 2.1∶1 of AA to diethylene glycol（DEG）,mass ratio of 1.5% of catalyst to AA,total mass ratio of 0.8% of polymerization inhibitor hydroquinone to AA,total mass ratio of 20% of water-entrainer toluene to reactant,reaction time of 90 min,and reaction temperature of 110~115℃,the yield of DEGDA reached 94.1%.The structure and acid strength of MCM-41-S-B catalyst were characterized by XRD,IR spectroscopy,DSC and Hammett indicator method.