酐交换法制备甲基丙烯酸酐的研究  

Synthesis of methacrylic anhydride by transanhydrization

作　　者：王亚鑫 谢晖[1] 黄莉[1] 杨远正 WANG Yaxin;Xie Hui;Huang Li;Yang Yuanzheng(College of Chemical Engineering,Nanjing Tech University,Nanjing 211800,China)

机构地区：[1]南京工业大学化工学院

出　　处：《南京工业大学学报（自然科学版）》2019年第6期761-766,共6页Journal of Nanjing Tech University(Natural Science Edition)

摘　　要：以甲基丙烯酸和乙酸酐为原料,采用精馏装置,通过酐交换反应,合成了甲基丙烯酸酐。对合成反应中主要条件进行了实验研究,并对产物进行了红外光谱(FT-IR)、核磁共振氢谱(1 H NMR)分析。确定了最佳反应条件:在对苯二酚、吩噻嗪和氮氧自由基哌啶醇的复合阻聚体系下,n(甲基丙烯酸)∶n(乙酸酐)为1.9∶1,反应温度85~125℃,反应时间为4.5 h,回流比为1~2,压力为3.99 kPa。该工艺条件下,产品中甲基丙烯酸酐质量分数为95.09%,收率为89.11%。Methacrylic anhydride was synthesized by transanhydrization with methacrylic acid and acetic anhydride in the reactive distillation tower,and the products were identified by Fourier transform infrared spectroscopy(FT-IR)and nuclear magnetic resonance hydrogen spectrum(1H NMR).The main reactive conditions were investigated with the following optimal conditions:the purity of the product of 95.09%and the yield of methacrylic anhydride of 89.11%under the molar ratio of methacrylic acid to acetic anhydride of 1.9∶1,reaction temperature of 85~125℃,reaction time of 4.5 h,reflux ratio of 1—2 and pressure of 3.99 kPa in hydroquinone,phenothiazine and 4-hydroxy-2,2,6,6-tetramethyl-piperidinooxy mixed polymerization system.

关 键 词：甲基丙烯酸 乙酸酐 酐交换 

分 类 号：TQ225.23[化学工程—有机化工]