Preparation method of alpha-linolenic acid with purity of 98%

A technology of linolenic acid and ethyl linolenate, which is applied in the preparation of carboxylic acid esters, organic compounds, carboxylic acid esters/lactones, etc., can solve the problem of low purity, low yield and unsaturated fatty acid components of unsaturated fatty acids Incomplete separation and other problems, to achieve the effect of sufficient sources, wide coverage, and increased separation efficiency

Active Publication Date: 2015-05-27
湖北华龙生物制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the single urea inclusion method also has shortcomings such as incomplete separation of unsaturated fatty acid components, low yield, and low purity of monopolyunsaturated fatty acids.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0017] 1. Preparation of fatty acid ethyl esters:

[0018] (1) Deacidification of Chinese tallow catalpa oil: take 200g of tallow tree catalpa oil, add 500ml of absolute ethanol, and stir in a water bath at 30°C for 10 minutes to extract. The upper layer is a milky white liquid, and the lower layer is a yellow oil. Oil 180g.

[0019] (2) Deacidified catalpa oil transesterification: Weigh 150g deacidified catalpa oil, 1.8g potassium hydroxide, 450ml absolute ethanol, completely dissolve potassium hydroxide in ethanol, mix with deacidified catalpa oil evenly, stir and reflux , the temperature rose to 70°C, and the reaction was carried out for 5h. After the reaction is over, recover ethanol, separate layers, release the lower layer, extract the upper layer with petroleum ether, add acetic acid solution to adjust the pH to 5, then wash with sodium chloride solution until neutral, dry, recover petroleum ether, and obtain 140 g of mixed fatty acid ethyl ester .

[0020] 2. Urea i...

example 2

[0036] 1. Preparation of fatty acid ethyl esters:

[0037] (1) Deacidification of tallow catalpa oil: Take 400g of industrial tallow catalpa oil, add 600ml of absolute ethanol, stir at 25°C for 20min, let stand to separate layers, and recover ethanol from the lower layer to obtain 370g of deacidified catalpa oil.

[0038] (2) Deacidified catalpa oil transesterification: Weigh 200g of deacidified catalpa oil, 2.0g of potassium hydroxide, and 500ml of absolute ethanol, completely dissolve potassium hydroxide in ethanol, mix with catalpa oil evenly, stir and reflux, and Raised to 80 ° C, the reaction 3h. All the other conditions are identical with example one, get mixed fatty acid ethyl ester 180g

[0039] 2. Urea inclusion:

[0040] (1) The first urea clathrate: Weigh 360g of urea and dissolve it in 1260g of 95% ethanol, then add 180g of mixed fatty acid ethyl ester obtained in the previous step at 80°C, after adding the sample, stir and reflux at 80°C for 30min. Heating was ...

example 3

[0052] Get α-linolenic acid ethyl ester 20g prepared by example one, process as follows:

[0053] Weigh 35 g of silver nitrate solid, and use 50% ethanol aqueous solution as solvent to prepare a 35% silver nitrate ethanol solution. Then 20 g of ethyl α-linolenic acid was prepared into a solution with a concentration of 0.4 g / ml using petroleum ether as a solvent, passed through N2, and stirred and complexed with 40% silver nitrate ethanol solution at 5° C. for 3 hours. After the complexation was completed, separate the liquids, add an equal volume of petroleum ether to the silver nitrate solution in the lower layer, desorb at 60° C. for 30 minutes, and then treat according to the method of Example 1 to obtain 5.9 g of ethyl α-linolenic acid with a content of 98.3%.

[0054] Take the α-ethyl linolenic acid obtained in the previous step, NaOH and 90% ethanol and mix them uniformly at a mass ratio of 1:0.2:4, carry out saponification reaction at 75°C for 5 hours under the protect...

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Abstract

The invention discloses a preparation method of alpha-linolenic acid with the purity of 98%. The preparation method is characterized by comprising the following steps: removing free fatty acid from Chinese tallow kernel oil, or siritch (linseed oil), purple perilla seed oil, eucommia seed oil, kiwi seed soil and the like in anhydrous ethanol to obtain mixed fatty glyceride; then performing base catalysis ester exchange to obtain mixed fatty acid ethyl ester; performing urea inclusion and complex salt complexing to obtain 90% alpha-linolenic acid; and finally performing metal ion complexing and dissociation to obtain alpha-linolenic acid with the purity of 98%. The preparation method disclosed by the invention is stable and reliable, simple, convenient and feasible to operate, simple in equipment and suitable for large-scale production.

Description

technical field [0001] The invention belongs to the technical field of preparation methods of linolenic acid, in particular to a preparation method of alpha-linolenic acid with a purity of 98%. Background technique [0002] Linoleic acid and linolenic acid have the effects of lowering blood fat, lowering cholesterol, lowering blood pressure and anti-cancer, and can also improve cardiovascular and cerebrovascular diseases and improve brain functions. Chinese tallow tree oil is mostly mixed fatty acids, such as: linolenic acid, linoleic acid, oleic acid and palmitic acid, etc. In order to obtain high-purity fatty acids, it is necessary to use certain methods to purify the mixed fatty acids of tallow tallow seed oil. [0003] The commonly used methods for purifying mixed fatty acids mainly include: silver ion complexation method, supercritical carbon dioxide distillation method, molecular distillation method, column chromatography method, adsorption separation method, lipase co...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C57/12C07C27/02C07C67/60C07C69/587
CPCC07C51/09C07C67/03C07C67/60C07C57/12C07C69/587
Inventor 董俊刘顺山刘成广余文权张凯林张惠芝明乐灿
Owner 湖北华龙生物制药有限公司
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