Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Production process of high-purity alpha-ethyl linolenate

A technology of ethyl linolenic acid and production process, applied in the field of chemistry, can solve the problems of unstable free state, loss and the like, and achieve the effects of increasing the output of target product, increasing the yield, and shortening the esterification reaction time

Active Publication Date: 2015-06-10
HENAN LINUO BIOCHEM CO LTD
View PDF4 Cites 4 Cited by
  • 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 α-ethyl linolenate is convenient for large-scale industrial application. There are not many reports on the production process of α-ethyl linolenate. Anyang Chemical Industry Group Co., Ltd. announced the development in the patent application number: 200510107355.1 The production process of a-linolenic acid ethyl ester is a production process of a-linolenic acid ethyl ester self-developed by 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: one is that the fatty acid containing a-linolenic acid after washing needs to be purified before esterification, and part of the product a-linolenic acid will be lost in the purification process, so that the final yield of ethyl a-linolenic acid It 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. Ethyl linolenate should not exceed 20kg; secondly, in order to make the esterification reaction complete, the esterification needs to be cooled to a certain extent to release the product, and then the temperature is raised to continue the esterification. Generally, two or more esterifications are used in production. The reaction time is at least 16 hours, and the esterification reaction takes a long time

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 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;

[0025] B: saponification: 100kg perilla oil obtained in step A and deionized water, enzyme catalyst lipolase100L are added in the container according to the ratio of 1:1:0.9 by weight, heated and stirred, at a temperature of 50°C, controlled to maintain the temperature of the material React for about 2 hours at a pH value of 7, and adjust the time appropriately in conjunction with taking samples to analyze the acid value, and end when the acid value reaches 120-210mgKOH / g. This process is protected by nitrogen throughout the process;

[0026] C: Acidification: Slowly add sulfuric acid with a mass concentration of 20% to the material obtained after saponification in Step B and stir and control the reaction temperature at 40°C. Stop adding s...

Embodiment 2

[0035] Steps A-G are the same as in Example 1, and the H urine inclusion extraction process is divided into two steps H1 and H2, specifically:

[0036] H1: Urea complexation: add 100kg of fatty acid ethyl ester containing a-linolenic acid ethyl ester obtained in step G, 95% ethanol, and urea into the reactor according to the weight ratio of 1:1.6:1.6, and control the temperature at 90°C , keep for 30min-60min, then cool down to room temperature;

[0037] H2: Freezing: The material obtained in step H1 is cooled in stages, the first stage is from room temperature to 0°C, the second stage is from 0°C to -5°C to -10°C, and the third stage is from -5°C to -10°C ℃ down to -10℃ to -20℃, the fourth stage from -10℃ to -20℃ to -20℃ to -30℃, the fifth stage from -20℃ to -30℃ to -30℃ to - 40°C, the sixth stage is from -30°C to -40°C to -40°C to -50°C, and each stage is kept for 30 minutes. After completion, the obtained material is filtered at 0°C to obtain liquid material, and hot water...

Embodiment 3

[0041] 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;

[0042] B: saponification: 100kg of perilla oil obtained in step A and deionized water, enzyme catalyst lipolase100L are added in the container according to the ratio of 1:0.8:1 by weight, heated and stirred, at a temperature of 40°C, controlled to maintain the temperature of the material React for about 2 hours at a pH value of 7, and adjust the time appropriately in conjunction with taking samples to analyze the acid value, and end when the acid value reaches 120-210mgKOH / g. This process is protected by nitrogen throughout the process;

[0043] C: Acidification: Slowly add sulfuric acid with a mass concentration of 10% to the material obtained after saponification in step B, stir and control the reaction temperature at 40°C, stop adding s...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention discloses a production process of high-purity alpha-ethyl linolenate, and belongs to the field of chemistry. The process is characterized in that esterification reaction is adopted, raw materials include 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 washed fatty acid containing the alpha-linolenic acid, the esterification reaction is carried out at one time and carried out in a reaction device, the reaction device is connected with a water distribution device, azeotrope of ethanol and water is simultaneously evaporated into the water distribution device during the esterification reaction in a period of time, and the urine enveloping purification is carried out for the alpha-ethyl linolenate in a product after the esterification reaction. By adopting the production process, the production process of the alpha-ethyl linolenate is simplified, the productivity is greatly improved, the production time is shortened, and the production efficiency is improved.

Description

technical field [0001] The invention relates to a production process of α-ethyl linolenate, in particular to a production process of high-purity α-ethyl linolenate, which 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 α-ethyl linolenate is convenient for large-scale industrial ...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/587C07C67/08C07C67/48
CPCC07C67/08C07C67/48C07C67/54C07C69/587
Inventor 高恒荆民哲闫西壮许志伟贾志强李超常新星
Owner HENAN LINUO BIOCHEM CO LTD
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com