A kind of production of vitamin D with lanolin as raw material 3 new method of industrialization

A vitamin and saponification technology, applied in the direction of organic chemistry, can solve the problems of no industrialization, uneconomical economic cost, low yield and purity, etc., and achieve the effects of reducing reagent consumption, strong industrial operability, and simplified process

Active Publication Date: 2021-02-26
AKTIN CHEM INC
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  • Claims
  • Application Information

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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, polluting the environment, uneconomical economic costs, etc., so industrialization has not been implemented. , so it is very necessary to choose a suitable method to separate and extract cholesterol from lanolin

Method used

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  • A kind of production of vitamin D with lanolin as raw material <sub>3</sub> new method of industrialization
  • A kind of production of vitamin D with lanolin as raw material <sub>3</sub> new method of industrialization

Examples

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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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Abstract

The invention provides a method for producing vitamin D with lanolin as raw material 3 A new industrialized method, first saponification of lanolin in a lower alcohol solution, and preliminary purification to obtain crude cholesterol, which is directly acetylated to obtain high-purity cholesterol acetate, and then sequentially undergoes oxidation, hydrazone, dehydrazone, hydrolysis, and light irradiation vitamin D 3 . The production process of the present invention is efficient, green, environmentally friendly, and has high product yield, is suitable for industrial production, and greatly reduces vitamin D 3 The manufacturing cost is low; the saponification process filtrate is handled skillfully, no waste liquid and waste are produced, and it is more conducive to environmental 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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Patent Type & Authority Patents(China)
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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