抗氧剂2246单丙酸酯的合成及表征  

Synthesis and characterization of antioxidant 2246 mono propionate

作　　者：徐志华 吴开赟 王忠冬 

机构地区：[1]江苏飞亚化学工业有限责任公司,江苏南通226600

出　　处：《合成橡胶工业》2012年第6期445-448,共4页China Synthetic Rubber Industry

基　　金：江苏飞亚化学工业有限责任公司资助项目

摘　　要：以抗氧剂2246和丙酰氯为原料、三乙胺为缚酸剂进行单酚羟基酯化反应,合成了抗氧剂2246单丙酸酯,确定了最佳合成工艺条件,并通过液相色谱、傅里叶变换红外光谱及核磁共振氢谱对产物进行了表征。结果表明,最佳合成工艺条件为抗氧剂2246/丙酰氯/三乙胺(摩尔比)1∶1.2∶1.8、抗氧剂2246/石油醚(质量比)1∶3.3、于60℃滴加丙酰氯、反应温度80℃、保温反应5.0 h;此条件下反应具有较好的重复稳定性,产品最高收率达到88.51%,纯度为98.5%,熔点104～106℃。The 2-（2-hydroxy-5-methyl-3-tert-butyl-benzyl）-4-methyl-6-tert-butyl-phenyl propionate（antioxidant 2246 mono propionate） was synthesized by mono phenolic hydroxyl esterification reaction with antioxidant 2246 and propionyl chloride as raw materials,triethylamine as acid binding agent,the optimal reaction conditions were found,and the obtained product was characterized by liquid chromatography,Fourier transform infrared spectroscopy and 1H-nuclear magnetic resonance.The results showed that the optimal reaction conditions were as follows： n（antioxidant 2246）/n（propionyl chloride）/n（triethylamine） 1∶ 1.2∶ 1.8,mass ratio of antioxidant 2246 to petroleum ether 1∶ 3.3,temperature for dripfeeding propionyl chloride 60 ℃,reation temperature 80 ℃ and reaction time 5.0 h.Under these conditions,the maximum yield,purity and melting point of the product reached 88.51%,98.5% and 104-106 ℃ respectively,and the reaction had good repeatability and stability.

关 键 词：抗氧剂2246 丙酰氯 三乙胺 缚酸剂 酯化 抗氧剂2246单丙酸酯 微观结构 

分 类 号：TQ314.249[化学工程—高聚物工业]