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Preparation method of a variety specifications of dementholized peppermint oil and menthol by combined azeotropic distillation and vacuum distillation technology

A technology of vacuum distillation and mint oil, which is applied in the preparation of hydroxyl compounds, organic compounds, essential oils/fragrances, etc., can solve the problems of large fraction loss, influence of vegetable oil aroma, high distillation temperature, etc., to ensure quality and reduce loss effect

Active Publication Date: 2018-05-18
ANHUI FENGLE PERFUME
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The problems existing in the traditional process cannot be ignored. First, the loss of the previous fraction is relatively large. Second, vacuum distillation requires high vacuum degree of equipment, high distillation temperature, and the aroma of vegetable oil is affected. Third, the separation effect is low and it is not convenient for special specifications. Preparation of vegetable oil

Method used

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  • Preparation method of a variety specifications of dementholized peppermint oil and menthol by combined azeotropic distillation and vacuum distillation technology
  • Preparation method of a variety specifications of dementholized peppermint oil and menthol by combined azeotropic distillation and vacuum distillation technology
  • Preparation method of a variety specifications of dementholized peppermint oil and menthol by combined azeotropic distillation and vacuum distillation technology

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Get 400g of peppermint hair oil, after adding 200g of entrainer water, carry out azeotropic rectification under the conditions of -0.06MPa in the height of packing column 1.0m, reflux ratio 3:1, vacuum degree, separate the cut before, detect, when cut When the content of olefins in the medium is ≤1%, stop. Oil and water are separated, and the oil phase is to be treated. The oil phase of the above-mentioned fraction before removal was obtained by rectification under reduced pressure under the conditions of packing column height 1.0m, reflux ratio 3:1, vacuum degree -0.096MPa, and detection, when the L-menthol content in the fraction was ≥50 %, stop. Add 150 g of water to the oil phase, and steam distillation under normal pressure to obtain the rear fraction.

[0022] The content of each fraction separated by azeotropic combined vacuum distillation technology:

[0023]

[0024] Deployment of peppermint oil (specification 1) selection amount:

[0025]

[0026] De...

Embodiment 2

[0034] Get 720g of peppermint hair oil, after adding 300g of entrainer water, carry out azeotropic rectification under the condition of packing column height 1.0m, reflux ratio 3:1, and vacuum degree of -0.08MPa, separate the fraction before separation, detect, when fraction When the content of olefins in the medium is ≤1%, stop. Oil and water are separated, and the oil phase is to be treated. The oil phase of the above-mentioned fraction before removal was obtained by rectification under reduced pressure under the conditions of packing column height 1.0m, reflux ratio 3:1, vacuum degree -0.096MPa, and detection, when the L-menthol content in the fraction was ≥50 %, stop. Add 200 g of water to the oil phase, and steam distillation under normal pressure to obtain the rear fraction.

[0035] The content of each fraction separated by azeotropic combined vacuum distillation technology:

[0036]

[0037]

[0038] Deployment of peppermint oil (specification 3) selection amo...

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Abstract

The invention provides a preparation method of a variety specifications of dementholized peppermint oil and menthol by combined azeotropic distillation and vacuum distillation technology. The method comprises the following steps that (1), azeotropic distillation to remove front distillate: peppermint trichomes oil is taken, after azeotropic agent water is added, azeotropic distillation is carriedout, front distillate is separated and detected, when olefin content in the front distillate is less than 1%, the azeotropic distillation is stopped; oil and water separation is carried out, oil phasewaits for treatment; (2), vacuum distillation to obtain post distillate: the above front distillate removed oil phase is subjected to vacuum distillation to obtain post distillate, the post distillate is detected, when the content of L-menthol is more than 50% in the distillate, the vacuum distillation is stopped; (3), atmospheric vapor distillation. The method reduces the loss of the front distillate, at the same time, the aroma of the front distillate can withstand 150 DEG C without being damaged by high temperature, the quality of dementholized peppermint oil is well guaranteed. And a variety specifications of dementholized peppermint oil can be prepared by the method, at the same time, the high content of menthol in the redundant post distillate can also be applied to the physical crystallization process to produce high purity natural menthol crystals.

Description

technical field [0001] The invention relates to the technical field of natural peppermint processing, in particular to a method for preparing various specifications of mint oil and menthol by azeotropic vacuum distillation technology. Background technique [0002] Peppermint is a plant of the Labiatae family. Peppermint crude oil can be obtained by extracting mint stems and leaves through methods such as steam distillation. One of the main components is menthol, which is an important spice substance. The mint crude oil is frozen, and part of the menthol is separated out, which is commonly called crude brain, and the mother liquor is called hair oil. The hair oil is distilled, blended, filtered and packaged to form a finished product of mint oil; [0003] The traditional menthol processing method is relatively simple. Menthol powder or rough brain is melted, dehydrated, filtered, and blended with peppermint oil to form a batching oil. After filtering, it is sent to a crystall...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/80C07C35/12C11B9/02
CPCC07C29/80C11B9/022C11B9/027C07C35/12
Inventor 朱俊峰赵国平王广强孙清华胡军张翼轸吴妍张玉莲赵以梅刘军赵彬
Owner ANHUI FENGLE PERFUME
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