摘要
用熔融酯化方法制备了丙烯酸高级酯 ,研究了单体量比、催化剂、阻聚剂、反应时间、反应温度等因素对该酯化反应的影响。确定用该法制备丙烯酸高级酯的适宜工艺为 :n(丙烯酸 )∶n(十八醇 ) =1 2∶1 0 ,m(对甲苯磺酸 )∶m(总单体 ) =1 0∶10 0 0 ,m(对苯二酚 )∶m(总单体 ) =0 5∶10 0 0 ,采用分段升温方法 ,于 110～ 140℃回流条件下反应 6h ,高级酯相对单体总质量的收率可达 90 %以上。测定了丙烯酸高级酯的熔点、沸点和元素组成 。
The melt esterification of acrylic acid and octadecyl alcohol without solvent was carried out.Effects of monomer ratio,amount of catalyst and inhibitor,reaction temperature and time on the reaction were investigated.Optimum reaction conditions were determined:molar ratio of acrylic acid to octadecyl alcohol 1 2∶1 0 ( n/n ),toluene p sulfonic acid as catalyst 1 0%( w/w ),hydroqinone as inhibitor 0 5%( w/w ),reflux time 6 hours at 110 -140 ℃ in stepwise heating.The yield was over 90%.The product was identified by melting point,boiling point,elementary analysis,IR spectra and H NMR spectra.Experimental results show that the physical characteristics and structural detail of octadecyl acrylate from melt esterification are in good agreement with that from normal method of esterification in solvent.This new preparation method has high efficiency and reliability with only small amount of catalyst and inhibitor.
出处
《精细化工》
EI
CAS
CSCD
北大核心
2002年第1期45-47,54,共4页
Fine Chemicals
