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Method for purifying vitamin A isomer in vitamin A mother liquor

A purification method and vitamin technology, applied in liquid solution solvent extraction, organic chemistry, etc., can solve the problems of difficult separation, high price of organic solvents, high toxicity, etc., and achieve the effect of high purity, cheap and easy-to-obtain solvents, and low toxicity

Active Publication Date: 2014-07-23
SHANGYU NHU BIOCHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The organic solvent used in this extraction system is expensive, highly toxic and difficult to separate

Method used

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  • Method for purifying vitamin A isomer in vitamin A mother liquor
  • Method for purifying vitamin A isomer in vitamin A mother liquor
  • Method for purifying vitamin A isomer in vitamin A mother liquor

Examples

Experimental program
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Effect test

Embodiment 1

[0040] The highly polar solvent in this embodiment is all methanol, and the low polar solvent is all ether, according to figure 1 As shown in the flow process, 1000g of VA crude mother liquor (the sum of the total trans VA and 13 cis VA content is 45.12%) is dissolved in 500mL of low polarity solvent solution, and the formed material 1 enters from the middle of the normal extraction tower evenly within 4h In the normal extraction tower, the extraction agent 3 is a highly polar solvent, which enters the normal extraction tower from the top inlet of the normal extraction tower, and the low polarity solvent enters the normal extraction tower from the bottom inlet of the normal extraction tower. The polar solvent is full, and the high polar solvent is controlled: the volume ratio of material 1: low polar solvent is 20:1:4, and the temperature of the normal extraction tower is -10°C. After the extraction is completed, the heavy component phase 5 is decompressed under reduced pressur...

Embodiment 2

[0043] The highly polar solvent is acetonitrile, the low polar solvent petroleum ether, the temperature of the normal extraction tower is 20°C, and the other conditions are the same as in Example 1. After the extraction is completed, the light component phase 10 is removed under reduced pressure from the low polar solvent , to obtain 507.45g of stripping essence, content 81.35%, molar yield 91.49%.

Embodiment 3

[0045] The highly polar solvent is 10% (v / v) aqueous methanol, the low polar solvent toluene, and the temperature of the positive extraction tower is 50° C., and the others are the same as in Example 1. After the extraction is completed, the phase containing light components 10 is under reduced pressure. The low-polarity solvent was removed to obtain 520.05 g of the back-extracted fine product, with a content of 82.35% and a molar yield of 97.16%.

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Abstract

The invention discloses a method for purifying a vitamin A isomer in a vitamin A mother liquor. The purification method comprises the following steps: continuously entering the vitamin A mother liquor into a positive extraction tower; extracting and washing to remove non-polar impurities by a low-polarity solvent; entering the obtained heavy phase to a reverse extraction tower after solvent removal; extracting and washing by using a high-polarity mixed solvent of one or more alcohols and water to remove the polar impurities, and carrying out solvent removal on the obtained light phase to obtain the high-content vitamin A refined mother liquor. By adopting the method, the vitamin A refined mother liquor is high in content and yield, environment-friendly and energy-saving, and the solvent can be recycled.

Description

technical field [0001] The invention relates to a method for purifying substances, in particular to a method for continuously extracting and purifying isomer 13 cis and all-trans in vitamin A mother liquor. Background technique [0002] Vitamin A isomers, including (all-E)-3,7-dimethyl-9-(2,6,6-trimethyl-1-enyl)-2.4.6.8-nonatetraenyl-1 -Alcohol acetate (abbreviated as all-trans VA) and (Z-8 type) 3,7-dimethyl-9-(2,6,6-trimethyl-1-enyl)-2.3.6.8-nonanetetra En-1-ol acetate (referred to as 13 cis VA) two substances, the structural formula is as follows: [0003] All reverse VA: [0004] [0005] 13 cis VA: [0006] [0007] In the process of synthesizing vitamin A, after the obtained VA crude oil is dissolved with an appropriate amount of absolute ethanol, the mother liquor after low-temperature crystallization (hereinafter referred to as vitamin A mother liquor) contains two isomers of all-trans VA and 13 cis VA. Among them, isomer 13 cis VA can be transformed into a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C403/08B01D11/04
Inventor 方玉明黄国东吕国锋赵立峰王陶囡王成龙
Owner SHANGYU NHU BIOCHEM IND