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A kind of preparation method of L-menthol spherical crystal

A technology of spherical crystals and menthol, applied in the field of preparation of L-menthol spherical crystals, can solve the problems of easy agglomeration, good fluidity and high bulk density, and achieves the Effect

Active Publication Date: 2022-03-01
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In order to overcome the defects of the existing L-menthol products, the present invention provides a method for changing the crystal form of L-menthol by using liquid-liquid phase separation to prepare a crystal product of spherical L-menthol, which solves the problem that the product is easy to crystallize. The problem of lumps, at the same time, the product particles are compact, the bulk density is high, and the fluidity is good

Method used

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  • A kind of preparation method of L-menthol spherical crystal
  • A kind of preparation method of L-menthol spherical crystal
  • A kind of preparation method of L-menthol spherical crystal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) Prepare 150 mL of a 0.01 g / mL L-menthol-water mixed solution at 40°C, stir until liquid-liquid phase separation occurs and L-menthol droplets are evenly distributed in the water;

[0031] (2) Cool the solution to 1°C at a cooling rate of 50°C / 10min, maintain a stirring rate of 600rpm until crystallization, and add 0.05% of surfactant sodium stearate (based on the quality of the L-menthol-water mixed solution) to continue Stir for 0.5h to make the crystals coalesce into a compact sphere;

[0032] (3) After vacuum filtration, washing with water, and drying at normal pressure at 10° C. for 12 hours, L-menthol spherical crystals were obtained.

[0033] The XRD pattern of the product is shown in figure 1 , it can be seen that the product is a stable crystal; the average particle size of spherical particles is 50 microns, and the tap density is 0.45g / cm 3 , the angle of repose is 29°.

Embodiment 2

[0035] (1) Prepare 150 mL of a 0.10 g / mL L-menthol-water mixed solution at 45°C, stir until the liquid-liquid phase separation occurs and the L-menthol droplets are evenly distributed in the water;

[0036] (2) Cool the solution to 5°C at a cooling rate of 40°C / 10min, maintain a stirring rate of 500rpm until crystallization, and add 0.20% of the surfactant sodium hexametaphosphate (based on the quality of the L-menthol-water mixed solution). Continue to stir for 2 hours to make the crystals coalesce into compact spheres;

[0037] (3) After vacuum filtration, washing with water, and drying at normal pressure at 20° C. for 24 hours, spherical L-menthol crystals were obtained.

[0038] The XRD pattern of the product is shown in figure 1 , it can be seen that the product is a stable crystal; the average particle size of spherical particles is 100 microns, and the tap density is 0.52g / cm 3 , the angle of repose is 31°.

Embodiment 3

[0040] (1) Prepare 150 mL of a 0.15 g / mL L-menthol-water mixed solution at 50°C, stir until the liquid-liquid phase separation occurs and the L-menthol droplets are evenly distributed in the water;

[0041](2) The cooling rate of the solution is 40°C / 10min to 10°C, and the stirring rate is maintained at 400rpm to crystallization, and 0.30% of the surfactant sodium dodecylbenzenesulfonate (based on the quality of the L-menthol-water mixed solution) is added ). Continue stirring for 3 hours to make the crystals coalesce into compact spheres;

[0042] (3) After vacuum filtration, washing with water, and drying at 30° C. under normal pressure for 36 hours, spherical crystals of L-menthol were obtained.

[0043] The XRD pattern of the product is shown in figure 1 , it can be seen that the product is a stable crystal; the average particle size of spherical particles is 250 microns, and the tap density is 0.55g / cm 3 , the angle of repose is 31°.

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Abstract

The invention discloses a preparation method of L-menthol spherical crystals. At 40-60°C, prepare an L-menthol-water mixed solution with an L-menthol concentration of 0.01-0.20g / mL; keep stirring until the liquid-liquid phase separation occurs in the solution; cool the solution to 1-20°C, and continue Stir until crystals appear; add 0.05% to 0.55% surfactant by mass fraction and keep stirring for 0.5 to 5 hours to make the crystals coalesce into balls; filter, wash and dry to obtain L-menthol spherical crystals. The solvent in the crystallization process only involves water, which is green and environmentally friendly, and the process is simple; the particle size of spherical crystals can be adjusted by stirring speed, and the average particle size of the product is between 50 and 300 microns; the crystal particles are round, with high fluidity and compactness The density is 0.45~0.55g / cm 3 ; The product has no tendency to agglomerate and form agglomerates, and can be stored for a long time.

Description

technical field [0001] The invention belongs to the technical field of chemical engineering industry crystallization, and in particular relates to a preparation method of L-menthol spherical crystals. Background technique [0002] L-menthol (CAS: 2216-51-5), the main component of peppermint oil, also known as L-menthol, natural menthol, menthol (L-rotary), etc., the English name is L-Menthol, molecular formula C 10 h 20 O, molecular weight 156.27, usually white needle-like crystals, with a cool mint aroma. Menthol is mostly extracted from plants. It is slightly soluble in water and easily soluble in alcohol, chloroform, ether, glacial acetic acid, liquid paraffin and petroleum ether. L-menthol has a special fragrance, spicy and cool feeling, and it is widely used in the food industry, daily fine chemical industry and pharmaceutical fields. For example, it is used as a flavoring agent for toothpaste, perfume, beverages and candies; it is used as a stimulant in medicine, ac...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C29/78C07C35/12
CPCC07C29/78C07C2601/14C07B2200/13C07C35/12
Inventor 龚俊波孙萌萌汤伟伟陈明洋侯宝红
Owner TIANJIN UNIV
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