串联式微通道反应器中制备壬醛、9-氧代-壬酸甲酯的反应研究

Preparation of nonanal and methyl 9-oxononanoate in a tandem microchannel reactor

采用微通道反应器对壬醛(N)、9-氧代-壬酸甲酯(M)进行连续化反应的研究。以油酸甲酯(MO)为原料,搭建模块化微通道反应器,对环氧油酸甲酯(EMO)的制备及EMO裂解制备N/M的反应进行串联,在双氧水体系中,分别以浓硫酸和磷钨酸为催化剂,实现EMO和N/M的连续化生产。考察了温度、催化剂用量、停留时间及水油两相进料比(体积比)对反应的影响。得到最优反应条件:MO环氧化反应温度为70℃,硫酸用量为12%(质量分数),停留时间为10 min,水油进料比为4:1;EMO裂解反应温度为60℃,磷钨酸(PTA)用量为9%(占水相质量分数),停留时间为9 min,水油进料比为4:1。在上述条件下,EMO收率为84.99%,N/M收率为72.89%。与间歇反应相比,其具有停留时间短、反应温度低、目标产物可模块化连续化生产等优点。

The continuous reactions of nonanal(N)and methyl 9-oxononanoate(M)were investigated using a microchannel reactor.A modular microchannel reactor was designed and built for the preparation of methyl epoxy oleate(EMO)and N/M in tandem with methyl oleate(MO)as the raw material.The continuous production of EMO and N/M was achieved in the hydrogen peroxide system using concentrated sulfuric acid and phosphotungstic acid(PTA)as catalysts,respectively.Effects of temperature,catalyst dosage,residence time and water-oil feed ratio on the reactions were investigated.The optimal reaction conditions were obtained as follows:MO epoxidation reaction at 70,12%sulfuric acid dosage(mass ratio of the aqueous phase),10℃min and 4:1 water-oil feed ratio,and EMO cracking reaction at 60,9%PTA dosage(mass ratio of the℃aqueous phase),9 min and 4:1 water-oil feed ratio.Under the above conditions,the EMO yield is 84.99%and the N/M yield is 72.89%.Compared with batch reaction,it has advantages of short residence time,low reaction temperature,and products can be produced modularly and continuously.