Device and method for purifying delta-decalactone by vacuum batch distillation

Abstract

The invention discloses a device and a method for purifying delta-decalactone by vacuum batch distillation, wherein the device comprises a tower kettle, a tower body, a vertical condenser, a falling film evaporator, a horizontal condenser and a vacuum reception tank; and the method comprises the steps of throwing delta-decalactone crude products in the tower kettle and uniformly mixing the crude products; under normal temperature, pulling the vacuum in the tower kettle to 100Pa and starting to heat; when the temperature of the tower kettle is 130-140 DEG C, extracting low-boiling point light components represented by pentyl cyclopentanone with a reflux ratio of 3-6; and when the temperature of the tower kettle is 160-180 DEG C, extracting the delta-decalactone with qualified purity with a reflux ratio of 2-9. According to the invention, after using the falling film evaporator, the height of the tower body is reduced, the heating time of the product is short, the thermal decomposition probability is greatly decreased and the purity of the product can be up to over 98wt%.

Description

technical field [0001] The invention relates to separation and purification technology of butyl-decalactone, in particular to a device and method for purifying butyl-decalactone by batch distillation under reduced pressure. Background technique [0002] Butydecalactone has a milky aroma and is widely used in food flavors. Buty-decalactone can be synthesized by biological and chemical methods, but it is difficult to realize the industrialization of biological methods, so at this stage, butyrolactone is mainly synthesized by chemical methods. [0003] At present, the separation and purification of butyl-decalactone is mainly carried out by a batch kettle type fractionation tower. This method is simple to operate and requires less equipment investment; however, this method has low evaporation efficiency and the material stays at high temperature for a long time. This kind of fractionation tower is easy to cause the material with high heat sensitivity to decompose at high tempe...

AI Technical Summary

Problems solved by technology

Buty-decalactone can be synthesized by biological and chemical methods, but it is difficult to realize the industrialization of biological methods, so at this stage, butyrolactone is mainly synthesized by chemical methods

[0003] At present, the separation and purification of butyl-decalactone is mainly carried out by batch kettle type fractionation tower. This method is simple to operate and requires less equipment investment; but this method has low evaporation efficiency and long residence time of materials at high temperature.

For materials with high heat sensitivity, this kind of fractionation tower is easy to cause their decomposition at high temperature, and it is difficult to separate qualified products.

[0004] The normal pressure boiling point of butyl decanolactone is 289 degrees Celsius, and it is easy to cause decomposition by fractional distillation with the above-mentioned equipment

In the purification of butyldecalactone, the low-boiling impurities represented by pentylcyclopentanone and the high-boiling substances produced in the oxidation process are mainly removed. The current fractional distillation method has a purity of only about 96wt%.

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