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Method for preparing menthane carboxamide by taking L-menthol as raw material

A technology of L-menthol and menthylamide, applied in the field of preparing menthylamide, can solve the problems of high production cost and high safety risk, and achieve the effects of small safety risk, simple operation and management, and saving production cost

Pending Publication Date: 2020-08-04
HENAN HUALONG SPICE
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] The purpose of the present invention is to provide a method for preparing menthyl amide with L-menthol as raw material, so as to solve the technical problems of high safety risk and high production cost of the existing industrial synthesis process route of menthyl amide

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  • Method for preparing menthane carboxamide by taking L-menthol as raw material
  • Method for preparing menthane carboxamide by taking L-menthol as raw material
  • Method for preparing menthane carboxamide by taking L-menthol as raw material

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preparation example Construction

[0028] The present invention provides a kind of method that takes L-menthol as raw material to prepare menthyl amide, and the preparation method comprises the following steps:

[0029] Step (1): Levomenthol and ZnCl 2 / HCl saturated solution for chlorination reaction, after the reaction, the upper oily matter is subjected to post-treatment to obtain chloromenthane, and the waste acid water in the lower layer is collected and subjected to vacuum distillation to remove H in the acid water 2 O and HCl, recovery of ZnCl 2 , the vacuum distillation is completed, and the recovered ZnCl 2 Add reagent concentrated HCl to reconstitute ZnCl 2 / HCl saturated solution, put in L-menthol and carry out the chlorination reaction again, and so on and on, realize the multiple application of waste acid water in the chlorination reaction, and the chloromenthane obtained by the reaction is used as the raw material for the next step reaction;

[0030] Step (2): Add magnesium chips, initiator, an...

Embodiment 1

[0056] The preparation method of menthyl amide (waste acid water is applied)

[0057] (1) Preparation of chloromenthane (used waste acid water)

[0058] Put the waste acid water produced after the chlorination reaction of the control group (waste acid water does not apply mechanically) into a reactor with a distillation device, heat the reactor for vacuum distillation, and control the temperature of the vacuum distillation at 80-130°C. During the distillation process, the distillation temperature must be strictly controlled. If the temperature is too high and the distillation time is too long, the zinc chloride will easily deteriorate and form basic zinc chloride, and the higher the temperature, the more serious the corrosion of the equipment caused by acid water. The vacuum degree is -0.08~-0.096Mpa, the time of vacuum distillation is 10-31h, the waste acid in the waste acid water is distilled, and zinc chloride is recovered. After the distillation, concentrated hydrochloric ...

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Abstract

The invention relates to a method for preparing menthane carboxamide by taking L-menthol as a raw material. The menthane carboxamide is prepared through the processes of chlorination, a Grignard reaction, acidification, acylating chlorination, amidation, distillation, recrystallization and the like in sequence. The process route is mature, has the advantages of operation management simplicity andsecurity risk reduction, during a chlorination process, lower-layer waste acid water is collected and reduced pressure distillation is carried out; H2O and HCl in the acid water are removed; recoveryof ZnCl2 is realized, reduced pressure distillation completion is realized, and a reagent, namely concentrated HCl, is added into the recovered ZnCl2; a ZnCl2 / HCl saturated solution is prepared again,the L-menthol is added for chlorination reaction again, the steps are repeated, the waste acid water in the chlorination reaction can be repeatedly used, the production cost is saved, the wastewatertreatment cost is reduced, and the economic benefit is improved.

Description

technical field [0001] The invention belongs to the technical field of cooling agents, in particular to a method for preparing menthylamide from L-menthol. Background technique [0002] Menthol is the main component of peppermint and peppermint essential oils. Naturally occurring menthol has 8 isomers because it contains 3 chiral centers. Among them, L-menthol has a cooling effect and is widely used in food, medicine, and daily chemicals. , Tobacco and other industries have been widely used. But, because the fragrance of levomenthol has obvious bitter taste, weak cooling effect and short action time, strong volatility, high temperature resistance, slightly soluble in water and other shortcomings, the application of levomenthol is greatly limited. In order to overcome these shortcomings of levomenthol, various novel cooling agents obtained by modifying the molecular structure of levomenthol arise at the historic moment. For example: menthyl acetate, menthyl lactate, menthon...

Claims

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Application Information

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IPC IPC(8): C07C231/02C07C233/59C07C17/16C07C23/10
CPCC07C17/16C07C51/15C07C51/60C07C231/02C07C2601/14C07B2200/07C07C23/10C07C61/08C07C233/59
Inventor 赵军侠李鹏毅姚彦涛文教刚王利霞马红磊冯亚萍栾淑静李刚
Owner HENAN HUALONG SPICE
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