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L-Menthol crystallization crystal form improvement method

A levomenthol and crystallization technology, applied in the field of crystallization technology of plant active ingredients, can solve problems such as taking a long time, and achieve the effects of shortening crystallization time, improving purity, and increasing diameter and length

Inactive Publication Date: 2016-02-24
安徽爱迪香料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Crystallization is the process of nuclei generation and crystal growth. The formation of crystal nuclei requires a certain amount of energy, while the growth of crystals takes a certain amount of time. Since the size of the crystal depends on the comparison between the nuclei generation rate and the crystal growth rate relationship, so the traditional crystallization takes a long time

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  • L-Menthol crystallization crystal form improvement method

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Embodiment 1

[0025] This embodiment relates to a method for improving the crystal form of L-menthol, comprising the following steps:

[0026] Step (1): Deploy peppermint oil until the content of L-menthol is 79%-85%;

[0027] Step (2): Take the above-mentioned part of peppermint oil into a glass container, and then place the glass container containing peppermint oil directly into a numerically controlled ultrasonic oscillator for ultrasonic treatment. The ultrasonic frequency is 5KHZ, the ultrasonic time is 10h, and the temperature is controlled at 0°C. , get velvet crystals;

[0028] Step (3): Add the remaining peppermint oil in step (1) into the crystallization container, and slowly introduce air into the bottom of the container at a rate of 0.5m- 3 / min, and the temperature is gradually lowered at a rate of 0.2°C / h. After cooling down to 8°C, symmetrically place electromagnets on both sides of the outer wall of the crystallization container with a magnetic field strength of 0.05T, and...

Embodiment 2

[0030] This embodiment relates to a method for improving the crystal form of L-menthol, comprising the following steps:

[0031] Step (1): Deploy peppermint oil until the content of L-menthol is 79%-85%;

[0032] Step (2): Take the above-mentioned part of peppermint oil into a glass container, and then place the glass container containing peppermint oil directly into a numerically controlled ultrasonic oscillator for ultrasonic treatment. The ultrasonic frequency is 40KHZ, the ultrasonic time is 72h, and the temperature is controlled at 10°C , get velvet crystals;

[0033] Step (3): Add the remaining peppermint oil in step (1) into the crystallization container, and slowly introduce air into the bottom of the container at a rate of 30m- 3 / min, and the temperature is gradually lowered at a rate of 1.0°C / h. After cooling down to 8°C, symmetrically place electromagnets on both sides of the outer wall of the crystallization container with a magnetic field strength of 1T, and ad...

Embodiment 3

[0035] This embodiment relates to a method for improving the crystal form of L-menthol, comprising the following steps:

[0036] Step (1): Deploy peppermint oil until the content of L-menthol is 79%-85%;

[0037] Step (2): Take the above-mentioned part of peppermint oil into a glass container, and then place the glass container containing peppermint oil directly into a numerically controlled ultrasonic oscillator for ultrasonic treatment. The ultrasonic frequency is 25KHZ, the ultrasonic time is 48h, and the temperature is controlled at 8°C , get velvet crystals;

[0038] Step (3): Add the remaining peppermint oil in step (1) into the crystallization container, and slowly introduce air into the bottom of the container at a rate of 3m- 3 / min, and the temperature is gradually lowered at a rate of 0.5°C / h. After cooling down to 8°C, symmetrically place electromagnets on both sides of the outer wall of the crystallization container with a magnetic field strength of 0.6T, and ad...

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Abstract

The present invention discloses a L-menthol crystallization crystal form improvement method comprising the following steps: step (1), blending mint oil until the L-menthol content is 79%-85%; step (2), take some of the mint oil into a container, and then putting the glass container containing the mint oil directly into a numerical control ultrasonic vibrating instrument for ultrasonic treatment to obtain velvet-like crystals; and step (3), taking the remaining mint oil into a crystallization vessel, slowly introducing air at the bottom of the crystallization vessel, cooling in gradient to a certain temperature, treating the crystallization vessel with an applied magnetic field, meanwhile adding the velvet-like crystals in the step (2), continuing for crystallization a period of time. Compared with the conventional crystallization method, the L-menthol crystallization crystal form improvement method can significantly increase the diameter and length of the L-menthol crystals, meanwhile the L-menthol crystallization crystal form improvement method also shortens the crystallization time of the L-menthol, gas chromatography detection results show that the purity of the L-menthol is also improved.

Description

technical field [0001] The invention relates to a crystallization process of plant active ingredients, in particular to a method for improving the crystal form of L-menthol. Background technique [0002] L-menthol is a white needle-like crystal extracted from the leaves and stems of peppermint. It is the main component of peppermint oil. It has a special cool aroma, with a pungent taste at the beginning and a cool after taste. It is widely used in food and daily chemical industries. [0003] The traditional production of L-menthol is made from peppermint crude oil through steam distillation, freezing and crystallization. Usually, the content of L-menthol produced by this method is about 95%, which can meet the requirements of food, daily chemical and other industries. In the production and sales process of levomenthol, in addition to the purity index, the crystal form of the product is another important index. The thick-looking L-menthol crystals are prismatic and produce a...

Claims

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Application Information

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IPC IPC(8): C07C29/78C07C35/12
CPCC07C29/78C07B2200/13C07C35/12
Inventor 刘锐锋郑俊峰文汉周仁术何光英刘中印汪燕
Owner 安徽爱迪香料有限公司