Green process for producing vinyl beta-ionol

Abstract

The invention discloses a green process for producing vinyl beta-ionol. The green process includes: pumping a solvent into a microchannel reactor, discharging air in channels, and continuously pumpinga beta-ionone solution and a vinyl magnesium chloride solution into the microchannel reactor to perform Grignard reaction to obtain reaction liquid; subjecting the obtained reaction liquid to normal-temperature reduced pressure distillation to recycle the solvent, and allowing the solvent to return to the microchannel reactor used in the previous step; adding residues after the normal-temperaturereduced pressure distillation into water, stirring to perform hydrolysis reaction, and filtering to remove basic magnesium chloride solid to obtain filtrate; standing the filtrate for layering, and separating upper-layer oil phase to obtain the vinyl beta-ionol, wherein the lower-layer water phase returns to the hydrolysis reaction of the previous step. The green process is simple in process flow, low in cost and energy consumption, safe, environmentally friendly and capable of continuously producing the vinyl beta-ionol.

Description

technical field [0001] The invention provides a green process for producing vinyl β-ionol, specifically pumping the THF solution of β-ionone and vinyl magnesium chloride into a microchannel reactor for Grignard reaction to prepare vinyl β-ionol Methods. Background technique [0002] Vinyl β-ionol is an important intermediate for the production of vitamin A and its derivatives, and its preparation methods mainly include two methods: acetylenation-hydrogenation reaction and Grignard reaction. [0003] Alkynylation-hydrogenation reaction method first dissolves β-ionone in liquid ammonia and passes it through acetylene to react to generate ethynyl β-ionol, and then uses Lindella catalyst to selectively hydrogenate to prepare vinyl β-ionol. This method needs to use three extremely dangerous raw materials of liquid ammonia, acetylene and hydrogen, which has great safety risks and extremely high requirements on production equipment. At the same time, the hydrogenation selectivity ...

AI Technical Summary

Problems solved by technology

[0005] 1. The Grignard reaction requires an anhydrous and oxygen-free environment, and the reaction is a strong exothermic reaction, which requires strict control of the reaction temperature and requires high production equipment;

[0006] 2. Excessive amount of Grignard reagent requires subsequent quenching, resulting in waste of raw materials and high cost;

[0007] 3. It is necessary to add an additional quencher, and part of THF is dissolved in the water phase during the subsequent extraction process, resulting in the loss of THF and a large amount of waste water;

[0009] 5. It is a batch reaction with low production efficiency

This patented technology can effectively control the safety of the Grignard reaction and realize continuous production, but there are still problems such as excessive Grignard reagents need to be quenched, low yield, and THF recovery and treatment.

Images