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Preparation method and device for polyenoic acid and ester monomer thereof

A technology of polyenoic acid and monomer, which is applied in the field of preparation of polyenoic acid and its ester monomer, can solve problems such as uncoupled green pretreatment process, achieve efficient preparation, avoid pollution, and reduce pressure

Active Publication Date: 2014-05-21
THIRD INST OF OCEANOGRAPHY STATE OCEANIC ADMINISTATION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

4. The method for preparing high-purity polyene acid by supercritical carbon dioxide fluid chromatography provided by the existing patent, the pretreatment of raw materials has not been coupled with the green pretreatment process

Method used

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  • Preparation method and device for polyenoic acid and ester monomer thereof
  • Preparation method and device for polyenoic acid and ester monomer thereof

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preparation example Construction

[0047] A kind of preparation method and device thereof of polyenoic acid and its ester monomer described in the present invention, such as figure 1 , 2 as shown,

[0048] It includes short path distillation separation and supercritical carbon dioxide fluid chromatography separation.

[0049] 1. Separation by short path distillation

[0050] The short path distillation device of the present invention is as figure 1 As shown, the short-distance distillation experimental device system consists of a feed tank 11, a control valve 12, a motor 13, a film scraper 14, an internal cooling hydrazine 15, a distillation kettle 16, a heat transfer oil inlet 17, a cold hydrazine 18, a vacuum pump 19, and a collection bottle 110 , cold water inlet 111, cold water outlet 112, light phase collection valve 113, heavy phase collection valve 114, heat transfer oil outlet 115. The working principle of the short-path distillation system has been described in detail in many documents and works, and...

Embodiment 1

[0079] After ethyl esterification, the arachidonic acid crude oil is put into the short-path distillation feed tank, the vacuum pump and temperature controller are turned on, and the degassing, solvent removal, moisture and volatile components are carried out at a vacuum degree of 20Pa and a temperature of 90°C. 1 hour. Turn on the short-path distillation feed pump, set the heating temperature to 95°C and the condensation temperature to 10°C, and conduct short-path distillation under the condition of 0.1-0.15Pa, and receive the light phase components from the condensation end. The received light phase components are dissolved into a solution with a certain concentration with a solvent, and the supercritical carbon dioxide fluid is used to prepare a chromatographic device for separation and preparation.

[0080] Two high-purity silica gel chromatographic columns (diameter 10 mm, length 250 mm, packing particle size 5 μ) were used; the temperature of the cryostat was -10 ° C; th...

Embodiment 2

[0084] Put the arachidonic acid crude oil after methylation into the short-path distillation feed tank, turn on the vacuum pump and temperature controller, and carry out degassing, solvent, moisture and volatile components at a vacuum degree of 20Pa and a temperature of 80°C. 1 hour. Turn on the short-path distillation feed pump, set the heating temperature to 85°C, and the condensation temperature to 8°C, conduct short-path distillation under the condition of 0.1-0.15Pa, and receive the light phase components from the condensation end. The received light phase components are dissolved into a solution with a certain concentration with a solvent, and the supercritical carbon dioxide fluid is used to prepare a chromatographic device for separation and preparation.

[0085] One high-purity silica gel chromatographic column (diameter 20 mm, length 250 mm, packing particle size 5 μ) is used; the temperature of the cryostat is -5 ° C; the system back pressure is 9-14 MPa; the column...

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Abstract

The invention provides a preparation method and device for polyenoic acid and an ester monomer thereof. The polyenoic acid and the ester monomer thereof are prepared by combining a primary short-range distillation method without consumption of an organic solvent with a supercritical carbon dioxide fluid chromatography. The short-range distillation technology is used for pre-separating long-chain compounds, polar compounds and volatile compounds in the raw materials of the polyenoic acid and the ester thereof to relieve the pressure of supercritical carbon dioxide fluid chromatographic separation and avoid polluting a chromatographic column, so that the polyenoic acid and the ester monomer thereof can be more efficiently prepared; a supercritical carbon dioxide fluid chromatograph device which takes carbon dioxide at a supercritical state as a chromatographic separation mobile phase, and has constant temperature control, no pulse and very small system dead volume is used for separating compound monomer components. The preparation method and device can be used for high-purity separation preparation of the polyenoic acid and the ester monomer thereof in fish oil, microalgae oil, microorganism oil, plant oil and other bio-oil rough grease. The preparation method and device can be used for guaranteeing high purity of produced products and no solvent residues; and the method is economical, safe and effective.

Description

technical field [0001] The invention relates to a preparation method and device of polyenoic acid and its ester monomer. Background technique [0002] Polyenoic acids (PUFAs) are a class of fatty acids with important physiological functions. The human body cannot synthesize them, but they are essential to the human body just like vitamins and minerals. Insufficient intake can easily lead to heart, kidney, brain, eyes and other vital organ disorders . Supplementing insufficient polyenoic acid through exogenous sources plays an important role in enhancing the normal operation of human body functions. A variety of polyenoic acids have been used as nutritional fortifiers and various health-care functional factors in the nutritional fortification of infant food and the daily nutritional health care of adults, and even in the treatment of diseases. Polyenoic acid comes from plants, animals, microorganisms (including microalgae), and the primary raw materials extracted from t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/44C07C51/47C07C57/03C07C57/12C07C67/54C07C67/56C07C69/587C07C69/58B01D3/10B01D15/08
CPCB01D3/10B01D15/08C07C51/42C07C51/44C07C51/47C07C67/48C07C67/54C07C67/56C07C231/24C07C69/587C07C69/58C07C233/20C07C57/03C07C57/12Y02P20/54
Inventor 许晨许建中夏金梅林翌
Owner THIRD INST OF OCEANOGRAPHY STATE OCEANIC ADMINISTATION
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