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Method for extracting vitamin E and phytosterin from cottonseed oil deodorizer distillate

A technology for deodorizing distillate and phytosterol, applied in chemical instruments and methods, organic compounds/hydrides/coordination complex catalysts, steroids, etc., can solve the problem of small processing capacity, serious equipment corrosion and high operating costs problems, to achieve the effect of mild reaction conditions, less corrosive equipment and less environmental pollution

Inactive Publication Date: 2010-02-10
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Some of the above processes use strong acid or strong base to catalyze esterification. Strong acid or strong base will seriously corrode the equipment, and produce acidic or alkaline wastewater, pollute the environment, and need post-treatment before discharge; some use lipase to catalyze esterification, although the reaction Mild conditions, no environmental pollution, but lipase is expensive, easy to inactivate, difficult to store
When separating, high vacuum distillation, molecular distillation or supercritical extraction are used. These methods have short process routes and less loss of vitamin E, but the equipment investment is large, the operating cost is high, and the processing capacity is relatively small.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Mix 200g of cottonseed oil deodorized distillate (containing vitamin E 8.03%, acid value 70mgKOH / g) with 400ml methanol, start to heat up to 60°C, feed inert gas, add 100g strong acid ion exchange resin 001×7, react 3h;

[0033] Filter out the catalyst by vacuum filtration;

[0034] Evaporate the filtrate under reduced pressure to remove methanol, water, etc.; the acid value of the esterified product after removing the solvent is 1.32mgKOH / g, and the preservation rate of vitamin E is above 94%;

[0035] According to the ratio of 1g: 3mL, the precipitated material and ethanol were made into a solution, and at 20°C, at a flow rate of 1BV / h, it passed through a strong basic anion exchange machine with a diameter of 25mm and a bed height of 500mm, which was filled with a model of 201×7 The adsorption column of the resin, and then wash the bed layer with ethanol until the effluent is transparent and clear, and collect the effluent;

[0036] Desorb with 5% acetic acid ethan...

Embodiment 2

[0039] Mix 200g of cottonseed oil deodorized distillate (containing vitamin E 8.03%, acid value 70mgKOH / g) with 600ml of methanol, start to heat up to 55°C, feed inert gas, add 80g of strong acid ion exchange resin NKC-9, and react 4h;

[0040] Filter out the catalyst by vacuum filtration;

[0041] Evaporate the filtrate under reduced pressure to remove methanol, water, etc.; the acid value of the esterified product after removing the solvent is 1.84mgKOH / g, and the preservation rate of vitamin E is more than 91%;

[0042] According to the ratio of 1g: 7mL, the desolubilized material and ethanol were made into a solution, and at 15°C, at a flow rate of 1.5BV / h, it passed through a strongly basic anion exchange machine with a diameter of 25mm and a bed height of 500mm. The adsorption bed of the resin, and then wash the bed layer with ethanol until the effluent is transparent and clear, and collect the effluent;

[0043] Desorb with 3% acetic acid ethanol solution at 30°C, elu...

Embodiment 3

[0046] Mix 200g of cottonseed oil deodorized distillate (containing vitamin E 8.03%, acid value 70mgKOH / g) with 800ml of methanol, start to heat up to 68°C, pass inert gas, add 50g of strong acid ion exchange resin D001, and react for 5h;

[0047] Filter out the catalyst by vacuum filtration;

[0048] Evaporate the filtrate under reduced pressure to remove methanol, water, etc.; the acid value of the esterified product after removing the solvent is 1.21mgKOH / g, and the preservation rate of vitamin E is more than 93%;

[0049] According to the ratio of 1g: 5mL, the precipitated material and ethanol are made into a solution, and at 20°C, at a flow rate of 0.5BV / h, it passes through an adsorption resin with a diameter of 25mm and a bed height of 500mm filled with an adsorption resin of the type S-8. bed, and then wash the bed with ethanol until the effluent is transparent and clear, and collect the effluent;

[0050] Use 5% acetic acid ethanol solution for desorption at 50°C, the ...

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Abstract

The invention discloses a method for extracting vitamin E and phytosterin from cottonseed oil deodorizer distillate, comprising the following steps that: methanol is added by taking cottonseed oil deodorizer distillate as raw material, reaction is proceeded by taking strong-acid cation exchange resin as catalyst so that free fatty acid in the raw material is converted into relative methyl ester; the catalyst is filtered; the filtrate is evaporated and is then formulated into mixed solution with ethanol after methanol and water are removed, after the mixed solution passes through an adsorptioncolumn filled with adsorbent, bed is washed with ethanol until the effluent solution is transparent and clear, and the effluent solution is collected; the adsorption column is eluted with acetic acidethanol solution, the eluant is collected and then subjected to reduced pressure evaporation, and vitamin E is acquired after the solvent is removed; the material of the effluent solution in which ethanol is removed by evaporation is dissolved in methanol, crystals are separated subsequent to temperature reduction and standing under stirring, and phytosterin crystals are acquired by filtering separation. The invention simplifies the steps for reaction and has the characteristics of small corrosiveness to equipment, no environmental pollution, simple operation and less equipment investment.

Description

technical field [0001] The invention relates to a method for extracting vitamin E and phytosterols, in particular to a method for extracting vitamin E and phytosterols from cottonseed oil deodorized distillates. Background technique [0002] The deodorized distillate of cottonseed oil contains fatty acids, glycerides, phytosterols, vitamin E and other components. [0003] Vitamin E (VitaminE), also known as tocopherol, is a fat-soluble vitamin. Is a lipid that stabilizes cells and reacts with peroxides to make them harmless to cells. Therefore, vitamin E is widely used in pharmaceutical products, which can be used to prevent diseases such as arteriosclerosis, cerebral hemorrhage, liver disease and diabetes. In addition, vitamin E can also be used in oil, food, cosmetics, and feed for livestock and poultry. There are two types of vitamin E: chemical synthetic products and natural products. Natural vitamin E is superior to chemically synthesized vitamin E in terms of physio...

Claims

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Application Information

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IPC IPC(8): C07D311/72C07J9/00B01J31/08
Inventor 郭翠梨张金钊雷鹏吴海艳
Owner TIANJIN UNIV
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