Abstract
Abstract The synthesis of 3-picoline from the liquid-phase condensation of acrolein and ammonium acetate under atmospheric pressure was conducted by first dissolving ammonium acetate in a C 2 C 6 carboxyl acid medium in the presence of solid acid catalyst, and then, feeding gradually a solution of acrolein in a C 2 C 6 carboxyl acid solvent. It was found that the employment of acetic acid, among various carboxyl acids tested, as both the reaction medium and solvent of acrolein, was most favorable, due to the obvious promotion to the formation of 3-picolind in liquid phase and retarding to the side reaction of acrolein polymerization in gas phase. The SO 4 2− /ZrO 2 -FeZSM-5 catalyst possesses the largest acid acidity and thus exhibited the largest yield of 3-picoline, among various solid acid catalysts. By employing the SO 4 2− /ZrO 2 -FeZSM-5 catalyst and acetic acid as both the reaction medium and solvent of acrolein, the influencing factors, including reaction temperature, molar ratio of ammonium acetate/acrolein/acetic acid, concentration and feeding rate of acrolein solution as well as usage of catalyst, were systematically investigated. The results indicated that an as high as 60% yield of 3-picoline could be achieved from a batch with molar ratio composition acrolein/ammonium acetate/acetic acid = 0.025/0.125/1.8, under the conditions of reaction temperature = 130 °C, concentration of acrolein solution = 14 wt%, feeding speed of acrolein solution = 12 mL/h and catalyst usage = 0.7 g/g (acrolein).
Published Version
Talk to us
Join us for a 30 min session where you can share your feedback and ask us any queries you have
Schedule a call