New industrial method for producing vitamin D3 by taking wool fat as raw material

A vitamin and saponification technology, applied in the direction of organic chemistry, can solve the problems of uneconomical cost, lack of industrialization, low yield and purity, etc., and achieve the effects of strong industrial operability, reducing reagent consumption and simplifying the process

Active Publication Date: 2019-05-17
AKTIN CHEM INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Many studies on how to separate and extract cholesterol from lanolin have been done a long time ago at home and abroad, but there are various problems, such as low yield and purity, pollutin...

Method used

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  • New industrial method for producing vitamin D3 by taking wool fat as raw material
  • New industrial method for producing vitamin D3 by taking wool fat as raw material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Embodiment 1 lanolin saponification

[0030] Add 50 kg of lanolin into the reaction kettle, then add 500 L (about 420 kg) of 80% methanol and 10 kg of sodium hydroxide, and saponify under reflux for 8 hours. Cool naturally after saponification, and filter; the filtrate supplements the consumed sodium hydroxide 3kg and uses it mechanically as the next saponification solution.

[0031] Or: Concentrate the above-mentioned filtrate under reduced pressure to about 50L to precipitate a large amount of sodium lanolate, remove the sodium lanolate by filtration, add 3Kg of sodium hydroxide to the filtrate, and use it as the next saponification solution.

Embodiment 2

[0032] Embodiment 2 Crystallization removes lanolin

[0033] Dry the filter cake obtained in Example 1 to obtain 15 kg, dissolve it with 75-150 kg of petroleum acetone (volume ratio 1:1), cool and crystallize to produce lanolin alcohol, filter, and concentrate the filtrate to dryness under reduced pressure to enter the next step for processing , and the filter cake was dried to obtain 4Kg of lanolin alcohol.

Embodiment 3

[0034] Example 3 Crystallization to remove lanosterol to obtain crude cholesterol

[0035] Add 50 times of weight methanol to the filtrate concentrate in Example 2 to separate out lanosterol, filter and dry to obtain about 4Kg of lanosterol solid; Lanosterol is monitored and detected by thin-layer chromatography until the filtrate only has a single spot of cholesterol and is concentrated to dryness to obtain 7 kg of crude cholesterol.

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PUM

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Abstract

The invention provides a new industrial method for producing vitamin D3 by taking wool fat as a raw material. The new industrial method comprises the following steps: carrying out saponification and primary purification on the wool fat in a low alcohol solution, thus obtaining a cholesterol crude product; directly carrying out acetylation on the cholesterol crude product, thus obtaining high-purity cholesterol acetate; then sequentially carrying out oxidizing, hydrazone forming, hydrazone removing, hydrolyzing, illuminating and the like, thus obtaining the vitamin D3. A production technology disclosed by the invention is efficient, green and environment-friendly, is high in product yield and is suitable for industrial production, and the manufacturing cost of the vitamin D3 is greatly reduced; a saponification technology is ingenious in filtrate treatment, has no generation of waste liquid and waste and is more beneficial for environment protection.

Description

technical field [0001] The present invention relates to a vitamin D 3 The industrialized production method belongs to the field of chemical drug preparation. Background technique [0002] Vitamin D 3 Also known as cholecalciferol, CAS number: 67-97-0, white powder, chemical name 9,10-cyclocholesta-5,7,10(19)-triene-3β-ol, molecular formula C 27 h 44 O, with a molecular weight of 384.64 and a melting point of 84-85°C, is easily oxidized in the air, has good heat resistance, but is easily decomposed when exposed to light, easily soluble in chloroform, easily soluble in ethanol, ether, cyclohexane and acetone, insoluble In water, in the human body, it is transformed from epidermal 7-dehydrocholesterol by light. Vitamin D 3 It is an essential substance for normal growth and reproduction of humans and animals, and it is also an active form with the highest biological metabolism rate among vitamin D. when vitamin D 3 Converted to activated vitamin D in the liver and kidneys...

Claims

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Application Information

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IPC IPC(8): C07C401/00
Inventor 付书清谢相林罗宗昂张林吴宪君
Owner AKTIN CHEM INC
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