Method for preparing fish oil ethyl ester by microwave esterification and purifying ethyl eicosapentaenoate

A technology of fatty acid ethyl ester and fish oil, which is applied in the preparation of carboxylic acid esters, chemical instruments and methods, and the preparation of organic compounds. It can solve the problems of small processing capacity, achieve large processing capacity, fast speed, and avoid heavy metal ions or toxic The effect of the use of organic solvents

Inactive Publication Date: 2013-02-06
TIANJIN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the maximum injection volume of this method is only 2.5ml, and the processing volume is small

Method used

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  • Method for preparing fish oil ethyl ester by microwave esterification and purifying ethyl eicosapentaenoate
  • Method for preparing fish oil ethyl ester by microwave esterification and purifying ethyl eicosapentaenoate

Examples

Experimental program
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Effect test

Embodiment 1

[0027] The raw material used in this example is a certain crude fish oil glyceride, and the acid value measured by the national standard GB-T5530-2005 method is 12.38mgKOH / g.

[0028] 1) Pre-esterification of fish oil: figure 1 500g of fish oil, 10g of concentrated sulfuric acid, and 500g of absolute ethanol were added to a round-bottomed flask, the round-bottomed flask was placed in a microwave reaction chamber, the microwave power was set to 300W, and the mechanical stirring was refluxed for 20 minutes; The pre-esterified product was washed with water until neutral, and excess ethanol and water were distilled under reduced pressure.

[0029] About 510 g of the pre-esterification product was obtained, and the acid value of the above-mentioned pre-esterification product was measured by the national standard GB-T5530-2005 method: S=1.38mgKOH / g.

[0030] 2) transesterification of fish oil: figure 1 , take 10g KOH and 500g absolute ethanol to make a solution, add it into a roun...

Embodiment 2

[0038] This example adopts the crude fish oil glyceride in embodiment 1 as raw material.

[0039] 1) Pre-esterification of fish oil: Take 500g of fish oil, 5g of concentrated sulfuric acid, and 200g of absolute ethanol into a round-bottomed flask, place the round-bottomed flask in a microwave reaction chamber, set the microwave power to 800W, mechanically stir and reflux for 10 minutes; the reaction is complete Finally, the pre-esterified product was washed with hot distilled water until neutral, and excess ethanol and water were distilled under reduced pressure. The acid value of the pre-esterified product was 0.96 mgKOH / g.

[0040] 2) Transesterification of fish oil: Take 2.5g KOH and 200g absolute ethanol to make a solution, add it into a round-bottomed flask containing 500g of pre-esterified fish oil, place the round-bottomed flask in a microwave reaction chamber, and set the microwave power to 500W, stir and reflux for 15 minutes. After the reaction was completed, the p...

Embodiment 3

[0044] The raw material used in this example is a certain crude fish oil glyceride, and the acid value is 9.68mgKOH / g after determination.

[0045] 1) Pre-esterification of fish oil: Take 500g of fish oil, 2.5g of concentrated sulfuric acid, and 150g of absolute ethanol into a round-bottomed flask, place the round-bottomed flask in a microwave reaction chamber, set the microwave power to 500W, and mechanically stir and reflux for 30 minutes; After completion, the pre-esterified product is washed with hot distilled water until neutral, and excess ethanol and water are distilled under reduced pressure. The acid value of the pre-esterified product was 1.06 mgKOH / g.

[0046] 2) Transesterification of fish oil: Take 5g KOH and 150g absolute ethanol to make a solution, add it into a round-bottomed flask containing 500g of pre-esterified fish oil, place the round-bottomed flask in a microwave reaction chamber, and set the microwave power to 800W , stirred and refluxed for 5 minutes....

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Abstract

The invention relates to a method for preparing fish oil ethyl ester by microwave esterification and purifying ethyl eicosapentaenoate, which comprises the following steps: adding fish oil, absolute ethanol and catalyst concentrated sulfuric acid into a reaction vessel, and heating under reflux in a microwave reactor to convert free fatty acid into fatty acid ethyl ester; after the reaction is carried out for 10-30 minutes, removing excessive solvent and catalyst from the product, and drying to obtain the fish oil fatty acid glyceride of which the acid value is smaller than 2; preparing the pre-esterified fish oil, absolute ethanol and catalyst KOH into a KOH-ethanol solution, adding the KOH-ethanol solution into the reaction vessel, and heating under reflux in the microwave reactor to carry out the ester exchange process; and after the reaction is carried out for 5-15 minutes, stratifying the product by standing or centrifuging, removing the understratum glycerol, removing the excessive ethanol and catalyst, and drying to obtain the ethyl eicosapentaenoate. The invention adopts two-stage vacuum rectification: light components with lower boiling point than ethyl EPA (eicosapentaenoate) are removed in the primary rectification tower; and the component subjected to light component removal enters a secondary rectification tower to separate the ethyl EPA from ethyl DHA, thereby obtaining the ethyl EPA with the purity of higher than 97%.

Description

technical field [0001] The invention relates to a method for separating and purifying omega-3 series polyunsaturated fatty acids from crude fish oil by using microwave technology and high vacuum rectification technology, especially microwave esterification to prepare fish oil fatty acid ethyl ester and eicosapentaenoic acid ethyl ester Purification method. Background technique [0002] Polyunsaturated fatty acid (polyunsaturated fatty acid, PUFA) refers to a straight-chain fatty acid with 2 or more unsaturated double bonds and 16 to 22 carbon atoms in its molecular structure. According to the position of the first double bond from the methyl end, it can be divided into ω-3, ω-6, ω-7, ω-9 series. EPA (Eicosapentaenoic acid), scientific name all-cis-5,8,11,14,17-eicosapentaenoic acid, DHA (Docosahexaenoic acid), scientific name all-cis-4,7,10,13,16,19-di Docosahexaenoic acid, they are the two most important essential fatty acids for the human body in the omega-3 series of po...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C11C3/04C11C3/10C07C69/587C07C67/54
Inventor 丁辉程楠
Owner TIANJIN UNIV
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