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Preparation method of high-purity menthol

A menthol, high-purity technology, applied in the field of high-purity menthol preparation, can solve the problems of low yield, inability to maintain natural characteristics, unfriendly environment, etc., and achieve the effect of improving product yield

Active Publication Date: 2020-12-08
HUANGSHAN TIANMU MINT PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present invention is in order to overcome that the menthol process route that the present synthetic method prepares is too long, and yield is low, needs to carry out chiral resolution, simultaneously because involves chemical reaction, A lot of waste is produced, it is not friendly to the environment, and at the same time, it cannot maintain the natural characteristics

Method used

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  • Preparation method of high-purity menthol
  • Preparation method of high-purity menthol

Examples

Experimental program
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Effect test

preparation example Construction

[0041] General embodiment: a kind of high-purity menthol preparation method comprises following preparation steps:

[0042] (1) Put mint crude oil at 40-50°C for 24-30h, and remove bottom moisture and impurities;

[0043] (2) Mix peppermint crude oil and ice oil at a mass ratio of 2:0.5-1, freeze out at -4~-10°C for 21-27 hours once, drain the oil to obtain primary oil and secondary oil, and then process the primary oil Heating to 55-60°C for melting, vacuum dehydration, and filtering through glass fiber filter paper to obtain naphtha;

[0044] (3) Mix Erbum oil and ice oil at a mass ratio of 1:1-1.5, freeze and freeze for a second time at -20 to -25°C for 50-60 hours, and drain the oil to obtain Erbum oil and hair oil; Heating the part of the brain to 55-60°C for heating and melting, vacuum dehydration, and filtering through glass fiber filter paper to obtain the dipepone oil;

[0045] (4) Mix 20-22 parts of virgin naphtha and 9-11 parts of digoxin, and add 8-9 parts of bak...

Embodiment 1

[0061] Embodiment 1: a kind of high-purity menthol preparation method comprises the following preparation steps:

[0062] (1) Put mint crude oil at 48° C. for 27 hours, and remove moisture and impurities at the bottom;

[0063] (2) Mix mint crude oil and ice oil at a mass ratio of 2:0.8, freeze out at -8°C for 25 hours once, drain the oil to obtain primary oil and secondary oil, then heat the primary oil to 58°C to melt and vacuum Dehydration, and filter through glass fiber filter paper, obtain early naphtha;

[0064] (3) Mix Erbum oil and ice oil at a mass ratio of 1:1.3, freeze out for 58 hours at -23°C for the second time, and drain the oil to obtain Erbum oil and hair oil; then heat Dimbum to 57°C for Heating and melting, vacuum dehydration, and filtering through glass fiber filter paper to obtain dipephalin;

[0065] (4) Mix 21 parts of naphtha and 10 parts of two parts of naphtha, add 8 parts of baked naphtha and 2 parts of melted oil, mix well at 57°C, and then carry ...

Embodiment 2

[0080] Embodiment 2: a kind of high-purity menthol preparation method comprises the following preparation steps:

[0081] (1) Place mint crude oil at 40°C for 30 hours, and remove bottom moisture and impurities;

[0082] (2) Mix mint crude oil and ice oil at a mass ratio of 2:0.5, freeze and freeze at -4°C for 21 hours once, and drain the oil to obtain primary and secondary oils, then heat the primary oil to 55°C to melt and vacuum Dehydration, and filter through glass fiber filter paper, obtain early naphtha;

[0083] (3) Mix Erbum oil and ice oil at a mass ratio of 1:1, freeze out for a second time at -20°C for 60 hours, and drain the oil to obtain Erbum oil and hair oil; then heat Dimbum to 55°C for Heating and melting, vacuum dehydration, and filtering through glass fiber filter paper to obtain dipephalin;

[0084] (4) Mix 20 parts of primary naphtha and 9 parts of digoxin, add 8 parts of roasted naphtha and 1 part of molten oil, mix well at 55°C, and then carry out cool...

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Abstract

The invention discloses a preparation method of high-purity menthol, and relates to the field of menthol preparation. The method comprises the following steps: 1)standing mint crude oil to remove bottom moisture and impurities; 2)mixing the mint crude oil with ice oil, carrying out primary freeze-out, draining the oil to obtain primary menthol and secondary oil, and then melting, dehydrating and filtering the primary menthol to obtain primary menthol oil; (3)mixing the secondary oil with ice oil, carrying out secondary freeze-out, and draining oil to obtain secondary menthol and crude oil; melting, dehydrating and filtering the secondary menthol to obtain secondary menthol oil; 4)mixing the primary menthol oil and the secondary menthol oil, adding the baked menthol oil and the molten oil for cooling crystallization, and separating to obtain wet menthol and ice oil; and(5)drying the menthol, cutting off the head part and the end part of the menthol, and airing the menthol to obtain thehigh-purity menthol. The high-purity menthol is prepared through multiple times of freeze-out and filtration, the natural characteristics of the high-purity menthol are maintained, and meanwhile, theproduct yield is greatly improved.

Description

technical field [0001] The invention relates to the field of menthol preparation, in particular to a method for preparing high-purity menthol. Background technique [0002] Natural menthol is colorless acicular, prismatic crystal or white crystalline powder. It is mainly derived from plants of the Labiatae family, and has the special aroma of mint. It can be used in medicine, flavors and fragrances, toothpaste, confectionery, cigarettes, cosmetics and other industries. agent, can also be used for medicine, be used for skin or mucous membrane, have the effect of cooling and relieving itching, at present, menthol can be prepared by synthetic method, but the menthol process route that synthetic method prepares is too long, and yield is low, needs to carry out Chiral separation, because it involves chemical reactions, produces more waste, is not friendly to the environment, and cannot maintain natural characteristics. [0003] For example, a kind of " a kind of refining method...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C35/12C07C29/74C07C29/78C07C29/76
CPCC07C29/74C07C29/78C07C29/76C07C2601/14C07C35/12
Inventor 方胜李友谊汪莉萍任移生
Owner HUANGSHAN TIANMU MINT PHARMA
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