Continuous synthesis method of milk lactone perfume

Abstract

The invention belongs to the technical field of synthetic perfumes, and specifically relates to a continuous synthesis method of milk lactone perfume. The continuous synthesis method comprises the following steps: carrying out aldol reaction under the action of alkaline water, then carrying out hydrogenation reaction and Baeyer-Villiger oxidation, carrying out acidic continuous hydrolysis, and dehydrating the product to obtain the milk lactone perfume, wherein the aldol reaction comprises: uniformly mixing part of cyclohexanone serving as a base material with the alkaline water, heating the mixture, dropwise adding a mixture of the remaining cyclohexanone and n-butyraldehyde, stirring the materials while the mixture is dropwise added, continuously stirring after the dropwise adding is ended, and ending the heat-preserved reaction till the content of the n-butyraldehyde is less than 1 percent; allowing the solution to stand still, separating an oil layer, collecting a water layer for recycling and use; washing the collected oil layer with water, then transferring the oil layer into a distillation still for distillation to recycle excessive cyclohexanone for use; collecting a condensation product at the bottom of the distillation still. According to the continuous synthesis method, the yield of the aldol reaction is increased by adding the cyclohexanone in different ways; furthermore, under a reaction temperature condition of the continuous synthesis method, an aldol condensation product can be obtained in one step.

Description

technical field [0001] The invention belongs to the technical field of synthetic perfume, and in particular relates to a continuous synthesis method of milk lactone perfume. Background technique [0002] Milk lactone is a mixture of 5 or 6-decenoic acids, CAS No. 72881-27-7, English name: Milk lactone, 5(6)-decenoic acids mixture, is a fragrance product with milk fragrance. It is actually a kind of unsaturated fatty acid. This very small amount of unsaturated fatty acid can produce milk flavor, strong aroma and long-lasting fragrance. It is a safe edible flavor approved by the American Practical Flavor Manufacturers Association. , cream, cheese essence, chocolate and other important raw materials of food. In addition, milk lactone has a high boiling point and can be used in baked foods. It is not easily destroyed like the compound milk flavor, and its application prospect is very broad. [0003] Chinese patent CN1266841A uses n-butyraldehyde and cyclohexanone as raw materi...

AI Technical Summary

Problems solved by technology

[0003] Chinese patent CN1266841A uses n-butyraldehyde and cyclohexanone as raw materials, through alkaline condensation, selective hydrogenation, hydrogen peroxide ring expansion to lactone, and finally dehydration under acidic conditions to obtain 5(6)-decenoic acid, the When the reaction is in alkaline condensation, the reaction is slow, and the reaction yield is low, and the separation and purification process is cumbersome, resulting in the disadvantages of high cost, harsh reaction conditions, complicated operation, and low yield in the entire synthesis route.

This reaction is condensed by using a phase inversion catalyst at room temperature, and subsequent solvent dehydration is required, resulting in the disadvantages of high cost, harsh reaction conditions, complicated operation, and low yield in the entire synthetic route.

In the subsequent decarboxylation process, the patent reacts under strong acid conditions, which will produce a large amount of strong acid wastewater