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Process for extracting vitamin E from plant-oil debrominated distillate

A technology of deodorizing distillate and process method, applied in the field of extracting vitamin E, can solve the problems of incomplete methylation of fatty acid, loss of vitamin E, increased cost, etc., and achieves reduction of production cost, high transesterification rate and good quality Effect

Inactive Publication Date: 2003-05-21
武汉凯迪精细化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

If saponification and acidification steps are taken, the loss of vitamin E in the lye is serious, and acid and alkali are used as reactants, which consume a large amount and increase the cost
If saponification is not adopted, fatty acid methyl esterification will not be complete, which will affect the operation of subsequent processes

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030]Embodiment 1: Soybean oil deodorization distillate 5000g, containing VE8.07%, containing sterol 8.71%, acid value 110, add methanol 2L, concentrated sulfuric acid 105ml, react at reflux temperature 68 ℃ for 2 hours, then add 90 ℃ heat 5000g of water to terminate the reaction. Stir evenly, let stand to separate layers, separate the lower layer of water, methanol, and sulfuric acid phase, wash with water three times, and wash the oil phase with water until neutral. The oil phase was cooled to room temperature, vacuum filtered to obtain 445g of sterols, with a content of 62.7%, the filtrate was cooled to 4°C, and then vacuum filtered to obtain 160g of sterol filter cakes, with a content of 60.8%, and the filtrate entered the supercritical carbon dioxide fluid extraction system , extracted at 12.0Mp, column temperature 32~48 ℃, obtained fatty acid methyl ester 2350g by separator, obtained 2600g pigment mixture at the bottom of rectifying column, wherein contained natural vit...

Embodiment 2

[0031] Example 2. Soybean oil deodorization distillate 300Kg, containing 8.80% VE, containing 6.59% sterol, acid value 120, add methanol 150L, ​​concentrated sulfuric acid 6L, react at reflux temperature 68 ℃ for 2 hours, then add 90 ℃ 300Kg of hot water to terminate the reaction. Stir evenly, let stand to separate layers, separate the lower layer of water, methanol, and sulfuric acid phase, wash with water three times, and wash the oil phase with water until neutral. The oil phase was cooled to room temperature, vacuum filtered to obtain sterol 19.8, the sterol content was 65.23Kg, the filtrate was cooled to 4°C, and then vacuum filtered to obtain 7.34Kg sterol filter cake, and the filtrate entered the supercritical carbon dioxide fluid extraction system, at 12.0 Mp, extracted at a column temperature of 32-48°C, obtained 154Kg of fatty acid methyl esters from the separator, and 116.8Kg of pigment mixture at the bottom of the rectification column, which contained 20.20% of nat...

Embodiment 3

[0032] Example 3. Soybean oil deodorization distillate 500Kg, containing 5.61% VE, containing 4.76% sterol, acid value 140.1, add methanol 245L, concentrated sulfuric acid 10L, react at reflux temperature 68 ℃ for 2 hours, then add 90 ℃ 500g of hot water to terminate the reaction. Stir evenly, let stand to separate layers, separate the lower layer of water, methanol, and sulfuric acid phase, wash with water three times, and wash the oil phase with water until neutral. The oil phase was cooled to room temperature, vacuum filtered to obtain 24.2Kg of sterols, the filtrate was cooled to 4°C, and then vacuum filtered to obtain 9.44Kg of sterol filter cake, wherein the sterol content was 63.00%. The filtrate enters the supercritical carbon dioxide fluid extraction system, extracts at 12.0Mp, and the column temperature is 32-50°C, and obtains 299Kg of fatty acid methyl esters from the separator, wherein the VE content is 1.30%. Obtain 165Kg pigment mixture at the bottom of rectifyi...

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PUM

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Abstract

The method for extracting vitamin E from vegetable oil deodorized distillate includes the following steps: methyl esterification, water-washing, removing steroid, removing fatty acid methyl ester, cold separation and removing solid, distillation, specially, after twice method esterification and washing with water, making dehydration and ester exchange. The ester exchange is characterized by that the mixture after dehydration is transferred into reactor still, the catalyst and low-grade alcohol necessary for ester exchange reaction are addded, the added amount of alcohol is 10-15 times theoretical requirement amount, its reaction temp. is reflux temp. of alcohol, 65-68 deg.C, stirring time is 1-2 hr. after the reaction is completed the isosteric concentrate sulfuric acid is added to neutralize alkaline catalyst and the reaction is stopped.

Description

technical field [0001] The invention provides a process for extracting vitamin E from vegetable oil deodorization distillates, which belongs to the technical field of fine chemicals. Background technique [0002] The commonly used natural vitamin E extraction process is to use the deodorized distillate of vegetable oil as raw material, saponify it with alkali, acidify the soap with strong acid, and then methylate it. The solubility of phytosterols in fatty acid methyl esters varies greatly with temperature. Cold crystallization and filtration to remove phytosterols, vacuum distillation to remove fatty acid methyl esters, and finally molecular distillation or supercritical extraction to obtain concentrated vitamin E products. There is also direct methyl esterification without saponification first. If saponification and acidification steps are taken, the loss of vitamin E in the lye is serious, and acid and alkali are used as reactants, which consume a large amount and increa...

Claims

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Application Information

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IPC IPC(8): C07D311/72
Inventor 王先宝方涛何方刘长华刘树发曹义飞吴小刚
Owner 武汉凯迪精细化工有限公司
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