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Concentration method for low-content natural mixed tocopherol

A tocopherol, low-content technology, applied in the field of chemical engineering, can solve the problems of large sewage treatment volume, use of labor, complex production equipment, etc.

Inactive Publication Date: 2014-12-17
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
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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  • Concentration method for low-content natural mixed tocopherol

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] A method for concentrating low-content natural mixed tocopherols, comprising adding 50 g of natural mixed tocopherols with a mixed tocopherol content of 38.2%, 5.5 g of succinic anhydride, 10 g of sodium hydroxide and 10 g of butanone, and stirring at 40° C. for 6 hours; After the reaction was over, butanone was distilled off under reduced pressure, and 250g of cyclohexane was added to wash with water to neutrality, cooled to 10°C and allowed to stand for crystallization for 24 hours, the crystalline solid was separated and dried to obtain natural tocopherol succinate; take 50g of natural tocopherol Add 100g of ethanol and 10g of 50% potassium hydroxide solution to the succinate for hydrolysis. The hydrolysis temperature is 60°C and the hydrolysis time is 4 hours. After hydrolysis, 100g of cyclohexane is added to wash with water until neutral. After recovery of cyclohexane by pressure distillation, 40 g of mixed tocopherol concentrate with mixed tocopherol content greate...

Embodiment 2

[0036] A method for concentrating low-content natural mixed tocopherols, comprising 50 g of natural mixed tocopherols with a mixed tocopherol content of 18.5%, adding 3 g of succinic anhydride, 10 g of sodium hydroxide and 150 g of butanone, and stirring at 60° C. for 4 hours; After the end, the methyl ethyl ketone was distilled off under reduced pressure, and 250g cyclohexane was added to wash with water to neutrality, and the temperature was lowered to 13°C to stand for crystallization for 20 hours, and the crystalline solid was separated and dried to obtain natural tocopherol succinate; natural tocopherol succinic acid Add 150g of ethanol and 10g of 50% potassium hydroxide solution to 50g of ester for hydrolysis. The hydrolysis temperature is 65°C and the hydrolysis time is 5 hours. After hydrolysis, add 150g of cyclohexane to wash with water until neutral, and decompress the solvent layer after separation. After recovering cyclohexane by distillation, a mixed tocopherol con...

Embodiment 3

[0038] A method for concentrating low-content natural mixed tocopherols, comprising adding 50 g of natural mixed tocopherols with a mixed tocopherol content of 42.2%, 5.8 g of succinic anhydride, 15 g of sodium hydroxide and 150 methyl ethyl ketone, and stirring at 70° C. for 6 hours; After the reaction was over, butanone was distilled off under reduced pressure, and 250 g of cyclohexane was added to wash with water to neutrality, and the temperature was lowered to 15° C. to stand for crystallization for 24 hours. The crystalline solid was separated and dried to obtain natural tocopherol succinate; natural tocopherol succinate Add 100g of ethanol and 10g of 50% potassium hydroxide solution to 50g of ester for hydrolysis. The hydrolysis temperature is 70°C and the hydrolysis time is 6 hours. After hydrolysis, 150g of cyclohexane is added to wash with water until neutral. After recovery of cyclohexane by pressure distillation, a mixed tocopherol concentrate with a mixed tocophero...

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Abstract

The invention relates to a concentration method for low-content natural mixed tocopherol. The method comprises: adding succinic anhydride, sodium hydroxide and butanone into natural mixed tocopherols with the mixed tocopherols content of 10%-45%, and stirring at 40-70 DEG C for 3-6 h; after the reaction is finished, performing reduced-pressure distillation to remove butanone, adding cyclohexane, performing water washing to neutral, cooling to 10-15 DEG C, standing for crystallization for 12-24 h, performing solid separation on the crystal and drying to obtain natural tocopherol succinate; adding ethanol and a potassium hydroxide solution with the concentration of 50% into natural tocopherol succinate to perform hydrolysis, controlling the hydrolysis temperature to be 60-70 DEG C and the hydrolysis time to be 4-6 h, after hydrolysis, adding cyclohexane and performing water washing to neutral, separating and performing reduced-pressure distillation on the solvent layer to recover cyclohexane, so as to obtain the mixed tocopherol concentrated liquid with the mixed tocopherol content larger than 90%.

Description

technical field [0001] The invention belongs to the technical field of chemical engineering, and in particular relates to a method for concentrating low-content natural mixed tocopherols. Background technique [0002] Natural vitamin E (Vitamin E) is a fat-soluble vitamin, also known as tocopherol, a commonly used medicine and health care product, and 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 syndrome, Beauty and other aspects have a ver...

Claims

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Application Information

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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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