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.pdf

668
化学卌界
2012年
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
杨师棣,蕠秀琴
渭南师范学院化学与生命科学学院,陕西渭南714000)
摘要:以表面含有苄基磺酸基的介孔分子筛(MCM-41-BS)为催化剂,采用直接酯化法合成了
(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)与ニ乙ニ醇(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射线符射(XRD)、红外光谱(IR)、差示担描量热(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
关键词:多编乙二醇双丙烯酸酯;介孔分子筛;磺酸型MCM-41;催化合成
中图分类号:O623.624
文献标志码:A
文章编号:0367-6358(2012)11-90668-05
Catalytic Synthesis of Di-tri-ethylene Glycol Diacrylate on Mesoporous
MCM-41 Functionalized with Benzylsulfonic Acid Groups
YANG Shi-di, CAI Xiu-qin
(College of Chemistry and Life Science, Weinan Teachers University, Shaanxi Weinan 714000, China)
Abstract Di-tri-ethylene glycol diacrylate was prepared from acrylic acid(AA) and di-tri-ethylene glycol
hrough 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-ethyl-
ene glycol. The results showed that under the optimum conditions of molar ratio of 2.1: l of AA to dieth-
ylene glycol( DEG), mass ratio of 1. 5% of catalyst to AA, total mass ratio of O.8% of polymerization in
hibitor hydroquinone to AA, total mass ratio of 20% of water-entrainer toluene to reactant, reaction time
of 90 min, and reaction temperature of 110-115C, the yield of DEGDA reached 94. 1%. The structure
and acid strength of MCM-4L-S-B catalyst were characterized by XRD, IR spectroscopy, DSC and Hammett
indicator method
Key words: di-tri-ethylene glycol diacrylate; mesoporous molecular sieve; sulphonic acid functionalized
MCM-41; catalytic synthesis
(三)乙二醇双丙烯酸酯( DTEGDA)是重要的精细化工产品,它作为紫外光固化树脂的活性稀
收稿日期:2011-12-23
作者简介:杨师棣(1953-),男,陕西白水人,教授,主要从事有机合成方面的研究。Email:ysdzzl23@126.com