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An industrial production method for producing high-content natural vitamin E by hydrolysis reduction method

A technology of natural vitamins and production methods, which is applied in the field of production of high-content vitamin E, and can solve the problems of complex production equipment, large floor space, high equipment costs and operating costs

Active Publication Date: 2016-05-18
JIANGSU CONAT BIOLOGICAL PROD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] 2) The production equipment is complex, covers a large area, and requires a lot of labor. Each process step requires different equipment to complete
[0010] 3) The risk of environmental pollution is high. The esterification or saponification treatment process requires a large amount of sulfuric acid or sodium hydroxide, and the sewage treatment volume after extracting natural tocopherol is huge, so it needs to be equipped with high-demand sewage treatment equipment
[0011] 3) The concentration ratio and yield of the molecular distillation method are relatively high, but due to the high degree of vacuum in its operation, it is difficult for the equipment
However, the equipment cost and operating cost are high, and the content of glyceride and unsaturated fatty acid in the raw material is required to be low

Method used

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  • An industrial production method for producing high-content natural vitamin E by hydrolysis reduction method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] 50 kg of low-content natural mixed tocopherols (vitamin E), wherein the content of mixed tocopherols is 38.2%, add 5.5 kg of succinic anhydride, 10 kg of sodium hydroxide, and 150 kg of butanone, and esterify at 40 degrees Celsius for 6 hours; After the esterification is completed, butanone is distilled off under reduced pressure, and 250 kg of cyclohexane is added to wash with water, and 100 kg of water is added each time, washed three times until neutral, cooled to 15 degrees Celsius and left to crystallize for 12 hours; the crystalline solid is separated and dried to obtain Natural Tocopheryl Succinate. The content of natural tocopherol succinate is 93.6%.

[0041] After many times of the above operations, take 50 kg of natural tocopherol succinate (content 93.6%), 100 kg of ethanol, and 10 kg of 50% potassium hydroxide solution for hydrolysis. The hydrolysis temperature is 70 degrees Celsius and the hydrolysis time is 4 hours. After hydrolysis Add 100 kg of cyclohe...

Embodiment 2

[0043]50 kg of low-content natural mixed tocopherols (vitamin E), of which the content of mixed tocopherols is 18.5%, is added with 3 kg of succinic anhydride, 10 kg of potassium hydroxide, and 150 kg of acetone, and esterified at 65 degrees Celsius for 4 hours. After the esterification is completed, distill off the acetone and add 250 kg of petroleum ether to wash with water, adding 100 kg of water each time, washing three times until neutral. After the water was removed, the temperature was lowered to 10 degrees Celsius and left to stand for crystallization for 12 hours. The crystalline solid was separated and dried to obtain natural tocopherol succinate with a content of 92.6%.

[0044] After multiple times of the above operations, take 50 kg of natural tocopheryl succinate (92.6% content), 150 kg of methanol, and 10 kg of 50% sodium hydroxide solution for hydrolysis. The hydrolysis temperature is 60 degrees Celsius, and the hydrolysis time is 6 hours. After hydrolysis, 150...

Embodiment 3

[0046] Low-content natural mixed tocopherols (vitamin E) 50 kg, wherein the content of mixed tocopherols is 42.2%, add 5.8 kg of succinic anhydride, 15 kg of triethylamine, 150 kg of petroleum ether, carry out esterification at 65 degrees Celsius for 5 hours . After the esterification, the petroleum ether was removed by evaporation, and 250 kg of n-hexane was added to wash with water, and 100 kg of water was added each time, and washed three times until neutral. After the water is taken out, the temperature is lowered to 15 degrees Celsius for crystallization, and the natural tocopheryl succinate is obtained after separation, and its content is 92.5%.

[0047] After multiple times of the above operations, take 50 kg of natural tocopheryl succinate (92.5% content), 100 kg of methanol, and 10 kg of 50% sodium hydroxide solution for hydrolysis. The hydrolysis temperature is 65 degrees Celsius, and the hydrolysis time is 5 hours. After hydrolysis, add 150 kg of petroleum ether fo...

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Abstract

An industrialized production method for producing high-content natural vitamin E by utilizing a hydrolysis reduction process comprises: (1) dissolving low-content natural mixed tocopherols in proper amount of a solvent, adding succinic anhydride and performing esterification reaction under an alkaline condition, so as to generate corresponding natural tocopherol esters; (2) performing reduced-pressure distillation on the product obtained in the step (1) to remove the solvent, adding an extraction reagent and performing extraction, water washing, crystallization and separation, so as to obtain natural tocopherol succinate with high content; (3) hydrolyzing natural tocopherol succinate obtained in the step (2) under an alkaline condition, and reducing to generate natural tocopherols; and (4) performing extraction, water washing, separation and distillation on the natural tocopherols obtained through hydrolysis in the step (3), so as to obtain the natural vitamin E (mixed tocopherols) with the high content up to 90% or more.

Description

technical field [0001] The invention belongs to the technical field of chemical engineering, and in particular relates to an industrial production method for producing high-content vitamin E by using a hydrolysis reduction method. Background technique [0002] Natural vitamin E (VitaminE) is a fat-soluble vitamin, also known as tocopherol, is a commonly used medicine and health care product, and is one of the most important natural antioxidants. Soluble in organic solvents such as fat and ethanol, insoluble in water, stable to heat and acid, unstable to alkali, sensitive to oxygen, not sensitive to heat, but the activity of vitamin E is significantly reduced when fried. Tocopherol can promote the secretion of sex hormones, increase the vitality and quantity of sperm in men; increase the concentration of estrogen in women, improve fertility, prevent miscarriage, and can also be used to prevent and treat male infertility, burns, frostbite, capillary bleeding, menopausal syndro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D311/72
CPCC07D311/72
Inventor 陈其林郭春荣李同斌
Owner JIANGSU CONAT BIOLOGICAL PROD
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