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Method for refining pseudoionone through molecular distillation

A pseudo-ionone and molecular distillation technology is applied in the field of separating and refining pseudo-ionone by molecular distillation technology, which can solve the problems of easy oxidation, polymerization, impure product aroma and high production cost of pseudo-ionone, and achieve The effect of low production intensity, low production cost and short operation time

Active Publication Date: 2013-12-25
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, industrial production mainly uses intermittent vacuum distillation to purify pseudo-ionones. However, due to the long heating time of this method, pseudo-ionones are prone to oxidation and polymerization reactions, so the product aroma is impure and the production cost is high.

Method used

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  • Method for refining pseudoionone through molecular distillation
  • Method for refining pseudoionone through molecular distillation
  • Method for refining pseudoionone through molecular distillation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] The steps and conditions of a method for purifying pseudoionone by molecular distillation are as follows:

[0027] (1) Standing for stratification: pump the aldehyde-ketone condensation reaction product of 5kg of Litsea cubeba oil and acetone under alkaline conditions into a settling kettle kept at 20°C, and collect the upper organic phase after standing and settling for 10 minutes;

[0028] (2) First-level thin-film distillation dehydration and degassing: the collected upper organic phase is pumped into a first-level thin-film distillation column at a flow rate of 40ml / min for dehydration and degassing. The first-stage distillation heating temperature is 60℃, and the vacuum degree is 5×10 4 ~9×10 4 Pa, the film scraping speed is 100rpm, and the condensation temperature is 5℃;

[0029] (3)Secondary molecular distillation separation: the dehydrated and degassed liquid is pumped into the second molecular distiller at a flow rate of 40ml / min for distillation separation, and the l...

Embodiment 2

[0032] The steps and conditions of a method for purifying pseudoionone by molecular distillation are as follows:

[0033] (1) Standing for stratification: Pump the aldehyde-ketone condensation reaction product of 5 kg of Litsea cubeba oil and acetone under alkaline conditions into a settling kettle kept at 30°C. After standing and settling for 30 minutes, collect the upper organic phase;

[0034] (2) First-level thin-film distillation dehydration and degassing: The collected upper organic phase is smoothly pumped into the first-level thin-film distillation column at a flow rate of 40ml / min for dehydration and degassing. The heating temperature of the first-stage distillation is 80℃ and the vacuum degree is 7×10 4 Pa, the scraping speed is 200rpm, and the condensation temperature is 8℃;

[0035] (3)Secondary molecular distillation separation: pump the dehydrated and degassed liquid into the second molecular distiller at a flow rate of 40ml / min for distillation separation to obtain 1.2...

Embodiment 3

[0038] The steps and conditions of a method for purifying pseudoionone by molecular distillation are as follows:

[0039] (1) Standing for stratification: 5kg of aldehydes and ketone condensation reaction products of Litsea cubeba oil and acetone under alkaline conditions are pumped into a settling kettle kept at 50°C, and after standing and settling for 60 minutes, the upper organic phase is collected;

[0040] (2) First-level thin-film distillation dehydration and degassing: The collected upper organic phase is pumped into a first-level thin-film distillation column at a flow rate of 40ml / min for dehydration and degassing. The first-stage distillation heating temperature is 90℃ and the vacuum degree is 5×10 4 Pa, the film scraping speed is 300rpm, and the condensation temperature is 12℃;

[0041] (3)Secondary molecular distillation separation: pump the dehydrated and degassed liquid into the second molecular distiller at a flow rate of 40ml / min for distillation separation, and the ...

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Abstract

The invention discloses a method for refining pseudoionone through molecular distillation. The method comprises the steps as follows: (1) raw materials stand for layering, litsea citrate oil and acetone perform an aldehyde ketone condensation reaction under an alkaline condition, a product is pumped in a settlement kettle, the temperature of the settlement kettle is kept to range from 20 to 50 DEG C, standing and settling are carried out for 5 to 60 minutes, and a supernatant organic phase is collected; (2) in a primary film distillation dehydration degasification step, the collected supernatant organic phase is stably pumped in a primary film distillation column for dehydration and degasification; in a secondary molecular distillation separation step, dehydration degasification liquid is pumped in a secondary molecular distiller for distillation and separation, and light and heavy components are obtained; and (4) in a tertiary molecular distillation separation, the secondary molecular distillation heavy components are pumped in a tertiary molecular distiller for distillation separation to obtain light and heavy components, and the light components are pseudoionone. The method is an efficient separation method, can avoid the technological operation of a rectifying tower, can save the operation time at the same time, reduces the production intensity, and achieves continuous production; in addition, pseudoionone achieves high purity and pure aroma.

Description

Technical field [0001] The invention relates to a method for refining and separating pseudoionone, in particular to a method for separating and refining pseudoionone by molecular distillation technology. Background technique [0002] Pseudoionone, the chemical name is 6,10-dimethyl-undecanetrien-2-one, molecular formula C 13 H 20 O, molecular weight 192, is a light yellow liquid and an important intermediate for the production of ionone. Ionone has a strong aroma and is the blending base of all ionone flavors. It is widely used in the main flavor of high-purity floral flavors. At the same time, pseudoionone is also widely used in the pharmaceutical industry. It is the vitamin A and E of medicine. An important intermediate for the production of raw materials and β-carotene, is currently one of the pharmaceutical intermediates that my country mainly relies on imports. [0003] Pseudoionone is a high-boiling substance and is prone to decomposition or oxidation at high temperatures. A...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C49/203C07C45/82
Inventor 吕扬效金伟铮王飞
Owner SOUTH CHINA UNIV OF TECH
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