分子筛催化合成正构长链烷基酚

SYNTHESIS OF n-ALKYLPHENOL OVER ZEOLITE CATALYST

以月桂酸和苯甲醚为原料,分别采用HY、USY、Hβ和HZSM-5分子筛作催化剂,经Friedel-Crafts酰基化反应、黄鸣龙还原以及醚裂解3个步骤,得到对位正构十二烷基酚,各步产物通过萃取、减压蒸馏、重结晶、柱色谱等方法分离并提纯,采用核磁共振氢谱对产物进行了结构鉴定,探讨了不同分子筛催化剂、溶剂、反应物配比、反应时间等条件对烷基酚产率的影响。根据上述反应路线和反应条件,分别以正辛酸、正癸酸、正十四酸、正十六酸为原料与苯甲醚反应,也合成出了对应的对位正构长链烷基酚。结果表明,HY分子筛催化剂可用于正构长链烷基酚的制备,该催化反应选择性为100%,苯甲醚转化率为86.3%,最终目标产物的产率可达到53.1%。

Para-n-dodecylphenol was synthesized from lauric acid and anisole over zeolite catalysts through Friedel-Crafts acylation, Huang Minlon reduction, and cleavage of ether bond. The resultants of each reaction were separated and purified by using extraction, distillation under reduced pressure, re-crystallization and column chromatography. The molecule structure of product was characterized by means of ^1H NMR. Some factors affecting the p-n-alkylphenols yield such as the catalyst, solvent, mole ratio of reactants, and reaction time, were discussed. According to this synthesis route of p-n-dodecylphenol, p-n-octylphenol, p-n-decylphenol, p-n-tetradecylphenol, and p-n-hexadecylphenol were also successfully synthesized by using caprylic acid, decanoic acid, dodecanoic acid, tetradecanoic acid, hexadecanoic acid as the raw materials reacting with anisole, respectively. The experimental results showed that this method was suitable for the synthesis of p-n-alkylphenol over HY catalyst, and anisole conversion and selectivity toward 1-（4-methoxy） phenyl-1-dodecanone were 86.3% and 100%, respectively. The goal product was successfully obtained with a yield of 53.1%.