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Method of separating alpha ethyl linolenate by cuprous chloride complexation adsorption

A technology of ethyl linolenate and complexation adsorption, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylic acid esters, etc., can solve the problems of loss of complexation, high price, difficulty in large-scale production, etc., and achieve Good separation effect and high product purity

Inactive Publication Date: 2005-08-10
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The separation effect of Ag+ complex adsorption method is good, and the product purity is high. The disadvantage is that Ag+ is expensive and difficult to produce on a large scale. At the same time, silver nitrate has poor stability and is easily reduced to amorphous silver and loses complexation.
Supercritical extraction is a method of separation by adjusting the temperature and pressure to control the solubility of each component in the supercritical fluid in the raw material. It can separate fatty acids with different carbon numbers, but it can separate fatty acids with the same carbon number but different double bond numbers. Fatty acid separation effect is not good

Method used

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  • Method of separating alpha ethyl linolenate by cuprous chloride complexation adsorption
  • Method of separating alpha ethyl linolenate by cuprous chloride complexation adsorption

Examples

Experimental program
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Effect test

Embodiment 1

[0019] Take Al with a specific surface area of ​​127.85m2 / g 2 o 3 50g, the molecular weight of CuCl is 99, the density is 4.14, by (s is the specific surface of the carrier, M is the molecular weight of CuCl, d is the density of CuCl, N is Avogadro's constant) the formula counts embodiment 2 and can know that CuCl 9g, 9g CuCl and 50gAl 2 o 3 Mix well, and calcined at 350°C for 4h in a muffle furnace. After cooling to room temperature, weigh 50 g and load it into a 19 mm×3 cm adsorption column by wet method.

[0020] Mix linseed oil and ethanol at a ratio of 1:3 (molar ratio), and when the temperature reaches 50° C., add lipase accounting for 5% of the total weight of the reactants, and start stirring for 8 hours to obtain mixed fatty acid ethyl esters. Its fatty acid composition is shown in Table 1.

[0021] Dissolve 1ml of mixed fatty acid ethyl ester in 10ml of petroleum ether, add to the adsorption column, then add 90ml of petroleum ether to start elution, collect 10...

Embodiment 4

[0029] Mix 9g CuCl with 50g Al 2 o 3 Mix well, and calcined at 380°C for 2h in a muffle furnace. After cooling to room temperature, 50 g was weighed and packed into a column (19 mm×3 cm) by wet method.

[0030] Mix perilla oil and ethanol at a ratio of 1:3 (molar ratio), and when the temperature reaches 50° C., add lipase accounting for 5% of the total weight of the reactants, and start stirring for 8 hours to obtain mixed fatty acid ethyl esters. Its fatty acid composition is shown in Table 2.

[0031]Dissolve 1ml of mixed fatty acid ethyl ester in 10ml of n-hexane, add to the adsorption column, then add 90ml of n-hexane to start elution, collect 100ml of fractions, then add 100ml of n-hexane containing 1%, 2%, and 4% acetone Alkanes continued to elute until the sample completely flowed out of the adsorption column. One fraction was collected per 100ml, and a total of 4 fractions were collected, which were recorded as 1#, 2#, 3#, and 4#. No α-linolenic acid ethyl ester w...

Embodiment 5

[0039] Mix 9g CuCl with 50gAl 2 o 3 Mix well, and calcined at 350°C for 4h in a muffle furnace. After cooling to room temperature, weigh 50 g and load it into a 19 mm×3 cm adsorption column by wet method.

[0040] Dissolve 1ml of mixed fatty acid ethyl ester in 10ml of petroleum ether n-hexane mixed solvent (V:V=50:50), add to the adsorption column, then add 90ml of the above mixed solvent to start elution, and collect 100ml of fraction Then add 100ml of acetone-containing 1%, 2%, and 4% of the above-mentioned mixed solvents to continue eluting until the sample completely flows out of the adsorption column. No α-linolenic acid ethyl ester was detected in 1# fraction, α-linolenic acid ethyl ester accounted for 41.23% of all fatty acid ethyl esters in 2# fraction, α-linolenic acid ethyl ester accounted for all fatty acid ethyl esters in 3# fraction 76.25% of esters. The ethyl α-linolenic acid in fraction 4# accounted for 93.27% of all fatty acid ethyl esters.

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Abstract

A process for extracting high-purity alpha-ethyl linolenate from the mixed ethyl ester of fatty acid by using cuprous chloride for complexing and adsoptive separating includes alcoholyzing reaction between the plant oil rich in alpha-linoleic acid and alcohol, flowing the resultant through complexing-adsorbing column carrying Cu ions, and eluting with solvent. Its advantage is low cost.

Description

technical field [0001] The invention relates to a method for extracting and separating high-purity alpha-linolenic acid ethyl ester. Specifically, vegetable oil rich in α-linolenic acid is used as raw material to generate fatty acid ethyl ester through alcoholysis, and then the mixed fatty acid ethyl ester is separated by Cu+ complex adsorption column to produce high-purity α-linolenic acid ethyl ester. Background technique [0002] α-linolenic acid (18:3 n-3, abbreviated as ALA) is an n-3 polyunsaturated fatty acid, which has many important physiological functions: preventing cancer, inhibiting tumor cell metastasis, antithrombotic, reducing Blood fat, long-term use can also improve intelligence and so on. However, α-linolenic acid cannot be synthesized by the body itself and must be ingested from the outside world. [0003] In nature, natural vegetable oils such as linseed oil and perilla oil contain a large amount of α-linolenic acid, but it coexists with other fatty ac...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/56C07C69/24
Inventor 侯相林周印羲齐永琴村俊民
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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