Separation and purification method for Omega-3 fatty acid ethyl ester from fish oil

A technology for separation and purification of fatty acid ethyl esters, applied in chemical instruments and methods, preparation of carboxylic acid esters, preparation of organic compounds, etc. The effect of low production efficiency, simple operation and less discharge of three wastes

Active Publication Date: 2016-03-09
ZHEJIANG MEDICINE CO LTD XINCHANG PHAMACEUTICAL FACTORY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the small amount of raw materials dissolved in non-polar solvents (that is, the concentration of the raw material solution can only be within 200g / L), the amount of raw materials in the reactor during the reaction is small, the production efficiency is low, and the product cost is high.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Omega-3 fatty acid ethyl ester purity (GC area normalization method, the same below) is 56% fish oil raw material, add N,N-dimethylformamide to dissolve, and prepare a 200g / L raw material solution. Using n-hexane as detergent and N,N-dimethylformamide as extractant, the flow ratio of raw material solution, detergent and extractant is 0.5:1.0:0.5, and multi-stage countercurrent extraction is carried out at 20°C. Collect the distillate from the washing section, add n-hexane equal to the volume of the distillate, stir and mix evenly, then add 2% saline solution equal to the volume of the distillate, carefully mix evenly, let stand, and after layering, the upper layer is obtained Clear liquid, rotary steaming removes normal hexane, obtains oily product, and the purity of total omega-3 fatty acid ethyl ester is 97.2%, and yield is 92.4%.

Embodiment 2

[0029] Omega-3 fatty acid ethyl ester purity is 56% fish oil raw material, add dimethyl sulfoxide to dissolve, be mixed with the raw material liquid of 300g / L. Use n-heptane as detergent and dimethyl sulfoxide as extractant. The flow ratio of raw material liquid, detergent and extractant is 0.5:1.0:1.0. Under the condition of 25°C, perform multi-stage countercurrent extraction and collect the washing section Distillate, add 0.5 times the amount of distillate volume of n-heptane, stir and mix evenly, then add 2% saline solution equal to the volume of the distillate, carefully mix evenly, let stand, after layering, get the supernatant liquid, and the n-heptane was removed by rotary evaporation to obtain an oily product, the purity of the total omega-3 fatty acid ethyl ester was 96.1%, and the yield was 91.6%.

Embodiment 3

[0031] Omega-3 fatty acid ethyl ester purity is 66% fish oil raw material, add methanol to dissolve, be mixed with the raw material liquid of 350g / L. Petroleum ether is used as detergent, methanol is used as extractant, the flow ratio of raw material liquid, detergent, and extractant is 1.0:1.0:0.5, multi-stage countercurrent extraction is carried out at 30°C, the distillate in the washing section is collected, and spin The solvent was evaporated to obtain an oily product, the purity of the total omega-3 fatty acid ethyl ester was 96.6%, and the yield was 90.5%.

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Abstract

The present invention discloses a separation method for high-content omega-3 fatty acid ethyl ester from ethyl ester type crude fish oil. According to a method in the prior art, the dissolved amount of a raw material in a non-polar solvent is small, so that the charge amount of the raw material in a reaction is small, the production efficiency is low, and the production cost is high. According to the method of the present invention, a polar solvent is used as a raw material solvent, a non-polar solvent is used as a detergent, and a solvent that is the same as the raw material solution is used as an extractant in an extraction section; and according to a liquid-liquid extraction principle, by adopting multistage countercurrent technology, high-purity omega-3 fatty acid ethyl ester is prepared and purified from fish oil with different purity levels of omega-3 fatty acid ethyl ester. The method disclosed by the present invention is simple in operation, small in three-waste discharge and easy for industrial production.

Description

technical field [0001] The invention relates to the technical field of chemical separation, in particular to a high-content omega-3 fatty acid ethyl ester (mainly including eicosapentaenoic acid ethyl ester and docosahexaenoic acid) separated from ethyl ester type crude fish oil ethyl ester) method. Background technique [0002] Omega-3, also written as omega-3 and omega-3, is a group of polyunsaturated fatty acids, which are commonly found in deep-sea fish, seal oil and certain plants, and are very beneficial to human health. In terms of chemical structure, omega-3 is a long chain composed of carbon and hydrogen atoms connected to each other, with 3 to 6 unsaturated bonds (ie double bonds) in between. Because the first unsaturated bond is located on the third carbon atom at the end of the methyl group, it is named omega-3 fatty acid. [0003] Omega-3 fatty acid ethyl esters mainly include octadecatrienoic acid ethyl ester (C18:3), stearidonic acid ethyl ester (C18:4), eic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/587C07C67/58
Inventor 张磊鑫余欢
Owner ZHEJIANG MEDICINE CO LTD XINCHANG PHAMACEUTICAL FACTORY
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