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Myristic acid purification method

A purification method and technology of tetradecanoic acid, applied in the field of purification of tetradecanoic acid, can solve the problems of purity not exceeding 98.0%, unsatisfactory, incapable of rectifying removal, etc., and achieve the effects of environmental friendliness, simple operation and convenient product separation

Active Publication Date: 2013-04-03
李赛荣
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] The preparation process of myristic acid is to extract glyceryl myristate from plants, such as glyceride in nature in the form of cardamom oil (content 70%-80%), palm oil (content 1%-3%), Coconut oil (content 17%-20%) is saponified by 10% sodium hydroxide solution, and finally acidified with hydrochloric acid to obtain free myristic acid. The main impurities in the acid are dodecanoic acid, myristic acid and hexadecanoic acid. The boiling point and melting point of these three acids or their esters have little difference. When the content of myristic acid is not high, azeotropic acid will form , cannot be removed by rectification, so the purity of existing products does not exceed 98.0%, which cannot meet the needs of some products for high-quality myristic acid, such as the development and production of the antineoplastic drug miplatin

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0013] In a 5L flask, add 3.5L ethanol and 342g myristic acid, stir and dissolve, add 182ml of concentrated ammonia water with a density of 0.91g / ml, stir and react at room temperature for 0.5 hours, then cool to 0°C to crystallize, filter, and filter cake After washing with ethanol, the filter cake was vacuum-dried at 40°C to obtain 297.7 g of ammonium myristate, with a yield of 81.0%. Add the prepared ammonium myristate into a 5L flask, add 3L of water, stir evenly, adjust the pH to about 2 with hydrochloric acid, filter, wash the filter cake with water, and dry under vacuum at 30°C to obtain 258.7g of myristate. The yield is 93.4%, the chemical purity is 99.62%.

Embodiment 2

[0015] In a 5L flask, add 3.5L ethanol and 342g myristic acid, stir and dissolve, add 182ml of concentrated ammonia water with a density of 0.91g / ml, stir and react at room temperature for 0.5 hours, then cool to 0°C to crystallize, filter, and filter cake After washing with ethanol, the filter cake was vacuum-dried at 40°C to obtain 295.8 g of ammonium myristate, with a yield of 80.5%. Add the prepared ammonium myristate into a 5L flask, add 3L of water, stir evenly, adjust the pH to about 2 with hydrochloric acid, filter, wash the filter cake with water, and dry under vacuum at 30°C to obtain 259.9g of myristate. The yield is 94.4%, the chemical purity is 99.59%.

Embodiment 3

[0017] In a 5L flask, add 3.5L ethanol, 342g myristic acid, stir to dissolve, pass ammonia gas to saturation, stir and react at room temperature for 0.5 hours, cool to 0°C to crystallize, filter, wash the filter cake with ethanol, and wash the filter cake at 40 ℃ vacuum drying to obtain 300.2 g of ammonium myristate with a yield of 81.7%. Add the prepared ammonium myristate into a 5L flask, add 3L of water, stir evenly, adjust the pH to about 2 with concentrated hydrochloric acid, filter, wash the filter cake with water, and dry under vacuum at 30°C to obtain 260.4g of myristate. The yield is It was 93.2%. The chemical purity is 99.74%.

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Abstract

The invention discloses a myristic acid purification method which comprises the following steps: reacting myristic acid and ammonia in polar solvent to obtain ammonium myristate; and acidifying the ammonium myristate to obtain purified myristic acid. The method has the advantages of no use of toxic solvent, short route, simple operation process, high quality of obtained products, high yield and low cost, and is easy to realize industrial production.

Description

technical field [0001] The invention relates to a method for purifying myristic acid, in particular to a method for removing dodecanoic acid, myristic acid and palmitic acid from myristic acid. Background technique [0002] The preparation process of myristic acid is to extract glyceryl myristate from plants, such as glyceride in nature in the form of cardamom oil (content 70%-80%), palm oil (content 1%-3%), Coconut oil (content 17%-20%) is saponified by 10% sodium hydroxide solution, and finally acidified with hydrochloric acid to obtain free myristic acid. The main impurities in the acid are dodecanoic acid, myristic acid and hexadecanoic acid. The boiling point and melting point of these three acids or their esters have little difference. When the content of myristic acid is not high, azeotropic acid will form , cannot be removed by rectification, so the purity of the existing products does not exceed 98.0%, which cannot meet the needs of some products for high-quality m...

Claims

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Application Information

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IPC IPC(8): C07C51/487C07C53/126
Inventor 李赛荣尹霖
Owner 李赛荣
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