Process for manufacturing high-purity alpha-ethyl linolenate

A technology for producing ethyl linolenate, which is applied in the chemical field, can solve problems such as instability of the free state and product loss, and achieve the effects of shortening the process time, increasing the yield, and making the process simple and practical

Active Publication Date: 2015-06-10
HENAN LINUO BIOCHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] a-Linolenic acid, chemical name: Allcis-9,12,15-octadecatrienoic acid (Allcis-9,12,15-Octadecatrienoic acid) symbol: 18:3Δ9, 12, 15 or 18:3n— 3. ω-3; a-linolenic acid is one of the necessary nutrients for people, which is of great significance to the health of the human body. It is lacking in the human body and needs to be supplemented by other means. Its preparations also have many medical therapeutic effects. In medicine , the food industry is used as an additive or health care product. The purity of a-linolenic acid is low in nature, and its content in perilla oil and linseed oil is as high as 50%. Since the free state of a-linolenic acid is unstable, it is esterified The form of a-linolenic acid ethyl ester is convenient for large-scale industrial application. At present, there are not many reports on the manufacturing process of a-linolenic acid ethyl ester. Anyang Chemical Industry Group Co., Ltd. announced the development in the patent application number: 200510107355.1 The manufacturing process of α-ethyl linolenic acid is a self-developed α-ethyl linolenic acid manufacturing process of its subsidiary Henan Linuo Biochemical Co., Ltd. The process flow is simply described as: perilla seed-pressing oil to obtain perilla oil —saponification—acidification—purification of α-linolenic acid—esterification—washing—dehydration—molecular distillation, and finally obtain ethyl α-linolenic acid. This technological process can obtain ethyl α-linolenic acid with a purity of more than 80%, but in practice There are the following problems in production: first, the fatty acid containing a-linolenic acid after washing needs to be purified before esterification, and the purification adopts the urine inclusion process, and part of the product a-linolenic acid will be lost during the purification process, making the final a-linolenic acid - The yield of ethyl linolenate is greatly affected, which is not conducive to maximizing the yield. Using this process, the initial 100kg of perilla oil can finally obtain about 10kg of a-linolenic acid ethyl ester. After various process optimization and lean management, it will reach 100kg The final a-linolenic acid ethyl ester obtained from perilla oil does not exceed 20kg; second, the purification of the target a-linolenic acid in the mixed fatty acids not only loses a lot of target substances, but also the purification process is complicated, requiring first heating, urine bag, The cooling and freezing process can only be completed, and the purification process is complicated, takes a long time and has a lot of loss, which is not conducive to the large-scale industrial production of a-linolenic acid ethyl ester. There is no effective solution to the above problems in various related technologies

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] A: Squeeze perilla oil: perilla seed is used as raw material to extract oil by cold-pressing oil technology to obtain perilla oil, and 100 kg of perilla oil obtained after filtering the solid impurities therein enters the next step;

[0023] B: Saponification: Add the perilla oil obtained in step A, deionized water, and enzyme catalyst lipolase100L into the container according to the ratio of 1:1:0.03 by weight, heat and stir, and control and maintain the pH of the material at a temperature of 45°C When the value is 7, react for 3 hours, and this process adopts the whole process of nitrogen protection;

[0024] C: Acidification: Slowly add sulfuric acid with a concentration of 15% to the material obtained after saponification in step B, stir and control the reaction temperature at 45°C, stop adding sulfuric acid when the material is less than 4, but continue when the pH value of the material rises to 4 or more Add sulfuric acid and repeat the above operations. When the...

Embodiment 2

[0032] Step E adopts multiple esterification process among the present embodiment, and other steps are identical with embodiment 1, specifically as follows:

[0033] A: Squeeze perilla oil: perilla seed is used as raw material to extract oil by cold-pressing oil technology to obtain perilla oil, and 100 kg of perilla oil obtained after filtering the solid impurities therein enters the next step;

[0034] B: Saponification: Add the perilla oil obtained in step A, deionized water, and enzyme catalyst lipolase100L into the container according to the ratio of 1:1:0.03 by weight, heat and stir, and control and maintain the pH of the material at a temperature of 45°C When the value is 7, react for 3 hours, and this process adopts the whole process of nitrogen protection;

[0035] C: Acidification: Slowly add sulfuric acid with a concentration of 15% to the material obtained after saponification in step B, stir and control the reaction temperature at 45°C, stop adding sulfuric acid ...

Embodiment 3

[0043] A: Squeeze perilla oil: perilla seed is used as raw material to extract oil by cold-pressing oil technology to obtain perilla oil, and 100 kg of perilla oil obtained after filtering the solid impurities therein enters the next step;

[0044] B: Saponification: Add the perilla oil obtained in step A, deionized water, and enzyme catalyst lipolase100L into the container according to the ratio of 1:1:0.03 by weight, heat and stir, and control and maintain the pH of the material at a temperature of 45°C When the value is 7, react for 3 hours, and this process adopts the whole process of nitrogen protection;

[0045] C: Acidification: Slowly add sulfuric acid with a concentration of 10% into the material obtained after saponification in step B, stir and control the reaction temperature at 45°C, stop adding sulfuric acid when the material is less than 4, but continue when the pH value of the material rises to above 4 Add sulfuric acid and repeat the above operations. When the...

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Abstract

The invention discloses a process for manufacturing high-purity alpha-ethyl linolenate, and belongs to the field of chemistry. The process comprises esterification reaction; the raw material comprises perilla oil; the perilla oil is saponified, acidified and washed to obtain fatty acid containing alpha-linolenic acid; the esterification reaction is directly carried out by adopting the fatty acid containing alpha-linolenic acid obtained by washing; the alpha-ethyl linolenate in the product is subjected to urea encapsulated purification after esterification; fatty acid ethyl ester of the alpha-ethyl linolenate, 95% ethanol and urea are added to a reactor according to a weight ratio of 1:(1-5):(1-5) during urea encapsulated purification, the mixture is heated to 80-100 DEG C and refluxed for 30-60min, then cooling and purification are carried out stage by stage, and the finished product is obtained by dehydration and molecular distillation. The process greatly simplifies the manufacturing process of the alpha-ethyl linolenate, and improves the yield.

Description

technical field [0001] The invention relates to a process for producing ethyl α-linolenate, in particular to a process for producing high-purity ethyl α-linolenate, and belongs to the field of chemistry. Background technique [0002] a-Linolenic acid, chemical name: Allcis-9,12,15-octadecatrienoic acid (Allcis-9,12,15-Octadecatrienoic acid) symbol: 18:3Δ9, 12, 15 or 18:3n— 3. ω-3; a-linolenic acid is one of the necessary nutrients for people, which is of great significance to the health of the human body. It is lacking in the human body and needs to be supplemented by other means. Its preparations also have many medical therapeutic effects. In medicine , the food industry is used as an additive or health care product. The purity of a-linolenic acid is low in nature, and its content in perilla oil and linseed oil is as high as 50%. Since the free state of a-linolenic acid is unstable, it is esterified The form of a-linolenic acid ethyl ester is convenient for large-scale ind...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/587C07C67/08C07C67/48
CPCC07C67/08C07C67/48C07C69/587
Inventor 高恒荆民哲闫西壮贾志强许志伟李超常新星
Owner HENAN LINUO BIOCHEM CO LTD
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