摘要
采用在线调节缚酸剂的合成工艺,2,2′-亚乙基双(4,6-二叔丁基)苯酚(简称双酚H)、丙烯酸、氧氯化磷、三乙胺为反应原料,甲苯为溶剂,酯化反应合成2-[1-(2-羟基-3,5-二叔丁基苯基)-乙基]-4,6-二叔丁基苯基丙烯酸酯(简称MB)。正交实验考察了合成MB的适宜工艺条件,n(双酚H)∶n(丙烯酸)∶n(氧氯化磷)=1∶1.2∶0.75,反应温度85℃、反应时间120 min。在线控制反应系统的pH在8.0左右,抑制副反应发生;原料双酚H转化率90.5%;产品选择性97.6%;摩尔收率大于88.0%。熔点188.3-189.7℃,IR1、H1、3C、谱图数据解析,定性MB的结构式;液相色谱定量分析,产品MB的纯度大于98.5%。
Adopting on-line adjustment of acid accepter synthesis technology,Antioxidant 2-[1-（2-hydroxy-3,5-di-tert-butylphenyl）-ethyl]-4,6-di-tertbutyl phenyl acrylate（MB for short） was synthesized with 2,2′-ethyliden-bis-（4,6-di-tere-butyl-phenol）（biphenyl H for short）,acrylic acid and phosphorus oxychloride;the optimum ratio was 1∶1.2∶0.75,by reacting at 85℃ for 120min.In order to suppress the side reaction,adjust pH value at 8.0 for on-line control.Under these optimum conditions,the conversion of bisphenol H was 90.5%,the selectivity to MB was 97.6%,the molar yield of MB reached 88.0%.The melt pointing was 188.3-189.7℃;Structures were verified by IR,1H NMR and 13C NMR respectively and agree satisfactorily with MB.The purity of MB qualified by HPLC reached over 98.5%（wt）.
出处
《常州大学学报（自然科学版）》
CAS
2010年第3期27-30,共4页
Journal of Changzhou University：Natural Science Edition
