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Menthol and peppermint oil purification process

A technology of peppermint oil and menthol, which is applied in the separation/purification of hydroxyl compounds, essential oils/flavors, and fat production, etc., can solve the problem of poor quality of broken small grains, unsatisfactory performance of crystal length and thickness, and differences in crystal shape, etc. problem to avoid errors

Active Publication Date: 2018-03-09
ANHUI YINFENG PHARMA
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Through chromatographic analysis, using mint crude oil containing a small amount of isomenthol (isomer of menthol) as raw material, adopting the above-mentioned scheme to carry out crystallization treatment, the content of isomenthol in the gained primary brain is higher; The seed crystal generation stage of crystallization usually needs to be realized by quenching, but the quality of the broken and small grains obtained by quenching is poor, which is not conducive to the growth of crystals in the later stage, and the crystal length and thickness are not ideal. However, due to the different content of total menthol and temperature control of the two freeze-thawed raw materials, there are differences in the shape of the crystals

Method used

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  • Menthol and peppermint oil purification process
  • Menthol and peppermint oil purification process
  • Menthol and peppermint oil purification process

Examples

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Embodiment 1

[0027] The embodiments are divided into Group A and Group B. The difference between the embodiments of Group A and the embodiments of Group B is that the origin of mint crude oil is different, and the composition is different:

[0028] The purification process of embodiment 1 is:

[0029] Embodiment 1 adopts the steps of melting, batching, dehydration, pressure filtration, brain drying, brain drying, freezing out, dehydration of hair oil and rectification steps mentioned in CN102775277A. Thermometer on the surface of the crystallization plate, and the cooling and heat preservation of the crystallization barrel is carried out alternately from the first day to the fifth day after the end of the crystallization oil feeding. From the sixth day to the 12th day, the temperature drops by 1.8°C every day when the cold salt water is turned on; from the thirteenth day to the 20th day, the temperature drops by 2.7°C every day when the cold salt water is turned on until the temperature dr...

Embodiment 2

[0041] The difference between embodiment 2 and embodiment 1 is: with the crystallization plate surface thermometer located at the lower end of the crystallization tank and built-in heat exchange pipeline, the cooling and heat preservation of the crystallization tank is carried out alternately from the first day to the fifth day after the crystallization oil feeding is completed, every day Turn on the cold brine to cool down to 25-28°C and keep it warm for 10 hours, then turn off the cold brine crystallization tank and keep it warm until the next day and turn on the cold brine again to cool down; from the sixth day to the twelfth day, the temperature drops by 2.3°C every day when the cold brine is normally on; the tenth From three days to the twentieth day, the cold brine was normally opened and the temperature dropped by 3.2°C every day until the temperature dropped to 0°C and then kept warm.

Embodiment 3

[0042] The difference between embodiment 3 and embodiment 1 is that: with the surface thermometer of the crystallization plate located at the lower end of the crystallization tank and with a built-in heat exchange pipeline, the cooling and heat preservation of the crystallization tank is carried out alternately from the first day to the fifth day after the end of the crystallization oil feeding, every day Turn on the cold brine to cool down to 25-28°C and keep it warm for 9 hours, then close the cold brine crystallization tank and keep it warm until the next day and turn on the cold brine again to cool down; from the sixth day to the twelfth day, the temperature of the cold brine will drop by 2°C every day; From three days to the twentieth day, the cold brine was normally opened and the temperature dropped by 3°C every day until the temperature dropped to 0°C and then kept warm. Among them, from the sixth day to the twelfth day, 1°C will be dropped at 8:00 am and 17:00 pm respe...

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Abstract

The invention discloses a menthol and peppermint oil purification process which comprises the procedures of raw material heating and melting, primary dehydrating under decompression, dispensing, primary filtering, crystallization, solid-liquid separation, menthol drying, rectification and the like. In the first to fifth days after crystal oil feeding, cooling and heat preservation of a crystallization vat are alternately performed, cold brine cooling is started every day to reach 25-28 DEG C, heat preservation is performed for 8-10 hours, cold brine cooling is stopped, the crystallization vatis subjected to heat preservation to the second day, and cold brine cooling is started again. In the sixth to twelfth days, cold brine is normally open, and the temperature is reduced by 1.8 to 2.3 DEG C every day. In the thirteenth to twentieth days, the cold brine is normally open, the temperature is reduced by 2.7 to 3.2 DEG C every day, and heat preservation is performed until the temperatureis reduced to 0 DEG C. The content of isomenthol in menthol melting oil crystallized by the slow cooling process is lower than 0.5%, menthol crystals are higher in purity, and the obtained crystals are sturdy and uniform in length, thickness and shape.

Description

technical field [0001] The invention relates to the technical field of natural medicine purification, in particular to a purification process of menthol and mint oil. Background technique [0002] Menthol, also known as menthol, is colorless needle-like crystals or granules. Menthol oil refers to the volatile oil of peppermint that removes most of the menthol through cold analysis. After component analysis, it contains terpenes, limonene, menthone, menthol, pulegol and menthyl acetate. Esters etc. The raw materials for the production of menthol and peppermint oil are peppermint crude oil. The steps of separating menthol from mint crude oil in the prior art are as disclosed in CN 103274901 A, which includes steps such as melting, dehydration, batching, impurity removal, rectification and crystallization, brain drying, brain drying, packaging and storage, etc. And the purification of mint oil is as described in the content disclosed in CN106619807A, obtained by freeze-out se...

Claims

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Application Information

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IPC IPC(8): C07C29/78C07C35/12C11B9/02
CPCC07C29/78C11B9/022C11B9/027C07C35/12
Inventor 常松何祥郑广强吴章栓马春光侯广晋桑传才
Owner ANHUI YINFENG PHARMA
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