磺化分子筛固定床合成1-萘乙酸甲酯的研究

SYNTHESIS OF METHYL 1-NAPHTHYLACETATELAURATE CATALYZED BY SULFONATED MOLECULAR SIEVE IN FIXED BED

实验以甲醇与1-萘乙酸先预酯化,再将预酯化液在262-磺化分子筛固定床反应器中高温酯化工艺合成1-萘乙酸甲酯。考察了高温酯化反应的影响因素。最佳高温酯化条件为:预酯化液的酸值(KOH)为60mg/g,甲醇与1-萘乙酸的质量比为0.5,反应温度为95℃,反应物流量为0.9mL/min,总酯化率达99.0%以上。催化剂循环使用11次,表现出优良的催化活性和稳定性。与传统工艺相比无需中和、水洗、萃取等步骤便可得到高纯度的产品。

Esterification of 1-naphthylacetic acid with methanol was carried out first. Then such fore- esterifieation liquid was used as raw materials for the synthesis of methyl 1-naphthylacetate by high temperature esterification catalyzed by 262-sulfonated molecular sieve in fixed bed reactor. Factors af- fecting the high temperature esterification were investigated. The optimum conditions were found as follows： mass ratio of methyl alcohol to 1-naphthylacetic acid 0.5,flow rate of reactant 0.9 mL/min, reaction temperature 95 ℃, reaction time 1 h. Under the optimum conditions, the esterification yield could reach above 99%. The catalysts were reused for 11 times with 99%of the esterification yield, demonstrating the high catalytic performance and stability of the catalysts. Compared with the tradi- tional process, this method produces high purity methyl 1-naphthylacetate without the tedious steps like neutralization, washing, extraction and so on.