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A kind of crystallization purification method of 7-dehydrocholesterol and its application in the production of vd3

A dehydrocholesterol and purification method technology, which is applied in the field of purification and preparation of 7-dehydrocholesterol, the raw material for vitamin D3 production, can solve the problems of increased viscosity of the photochemical reaction system, increased probability of "occlusion", and long operation cycle, etc., to achieve purification The process is mild and controllable, it is convenient for filtration and washing, and the effect of improving utilization efficiency

Active Publication Date: 2022-04-05
ZHEJIANG NHU CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] With the increase of the number of applications in the reaction system, the VD3 content in the solution will gradually increase. When it increases to a certain concentration, the above operation will easily lead to an increase in the probability of "mother liquid occlusion" of 7-dehydrocholesterol. The separated 7 -Dehydrocholesterol contains VD3 content up to 25% (wt). At the same time, the VD3 contained in this part will further photochemically react during the application process, resulting in unnecessary impurities, which will cause serious product loss and increase impurities. The content of the photochemical reaction system will increase after being applied for many times at the same time, which greatly affects the filtration efficiency and reaction process, and has the disadvantages of long operation cycle, many steps, and cumbersome separation operations.

Method used

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  • A kind of crystallization purification method of 7-dehydrocholesterol and its application in the production of vd3
  • A kind of crystallization purification method of 7-dehydrocholesterol and its application in the production of vd3
  • A kind of crystallization purification method of 7-dehydrocholesterol and its application in the production of vd3

Examples

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Effect test

Embodiment 1

[0053] 45g 7-dehydrocholesterol with a content of 96% was added to a mixed solvent of 1544g methanol (70wt%) and 661g (30wt%) n-hexane to obtain a 7-dehydrocholesterol solution with a mass fraction of 2%, and the photochemical reactor was turned on , control the temperature of the reactor to be 40 ° C, and use the metering pump to pass the configured 7-dehydrocholesterol solution into the photochemical reactor. After the reaction is completed, a solution of pre-vitamin D3 is obtained, and the solution is heated at 60 ° C and refluxed for 1 hour, and then concentrated And reclaim methanol and n-hexane mixed solvent, filter and separate to obtain 7-dehydrocholesterol crude product 40g (7-dehydrocholesterol content is 86%, vitamin D3 content is 8%), see the crystal photo image 3 .

[0054] Use 180 g of solvent dichloromethane to dissolve the above-mentioned crude 7-dehydrocholesterol, set the external temperature of the water bath at 25°C, and remove the solvent by reducing the ...

Embodiment 2

[0067] 45 g of 7-dehydrocholesterol with a content of 96% was added to 4455 g of methanol to obtain a 7-dehydrocholesterol solution with a mass fraction of 1%. The photochemical reactor was turned on, and the temperature of the reactor was controlled to be 40°C. The 7-dehydrocholesterol solution was passed into the photochemical reactor, and after the reaction was completed, a solution of pre-vitamin D3 was obtained, and the solution was heated to 60 ° C and refluxed for 1 hour, then concentrated and recovered methanol and n-hexane solvent, and 7-dehydrogenation was obtained by filtration and separation Crude cholesterol 30g (7-dehydrocholesterol content is 90%, vitamin D3 content is 6%).

[0068] Use solvent dichloromethane 180g to dissolve above-mentioned 7-dehydrocholesterol crude product, set 25 ℃ of water bath external temperature, reduce the pressure of 200mbar to evaporate the solvent, obtain amorphous 7-dehydrocholesterol powder; configure n-hexane / methanol (n-hexane). ...

Embodiment 3

[0070] 45g 7-dehydrocholesterol with a content of 96% was added to a mixed solvent of 1544g methanol (70wt%) and 661g (30wt%) n-hexane to obtain a 7-dehydrocholesterol solution with a mass fraction of 2%, and the photochemical reactor was turned on , control the temperature of the reactor to be 40 ° C, use the metering pump to pass the configured 7-dehydrocholesterol solution into the photochemical reactor, after the reaction is completed, obtain a solution of pre-vitamin D3, heat the solution to reflux for 1 hour, then concentrate and recover Methanol and n-hexane were mixed solvent, and the concentrated product was filtered and separated to obtain 40 g of crude 7-dehydrocholesterol (the content of 7-dehydrocholesterol was 86%, and the content of vitamin D3 was 8%).

[0071] Use solvent dichloromethane 180g to dissolve above-mentioned 7-dehydrocholesterol crude product, set 25 ℃ of water bath external temperature, reduce the pressure of 200mbar to evaporate the solvent, obtain...

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Abstract

The invention discloses a method for crystallization and purification of 7-dehydrocholesterol and its application in the production of VD3. The method for crystallization and purification comprises the following steps: (1) dissolving crude 7-dehydrocholesterol in a halogenated hydrocarbon solvent, The solvent is then removed to obtain amorphous 7-dehydrocholesterol powder; (2) the 7-dehydrocholesterol powder obtained in step (1) undergoes crystal transformation in a mixed solvent system composed of a polar solvent and a non-polar solvent Form 7-dehydrocholesterol with a crystal form, and after the crystallization is completed, the pure product of 7-dehydrocholesterol is obtained through post-processing; the polar solvent is an alcohol solvent; the non-polar solvent is a hydrocarbon solvent. The method can improve the inclusion and entrainment problem of VD3 in the separation process of 7-dehydrocholesterol, thereby increasing the yield of VD3.

Description

technical field [0001] The invention belongs to the field of fine chemicals, and in particular relates to a process for purifying and preparing 7-dehydrocholesterol, a raw material for vitamin D3 (VD3) production, and its application. Background technique [0002] 7-Dehydrocholesterol (7-DHC for short) is an important intermediate for the synthesis of vitamin D3. It is isolated and extracted from raw materials such as pig skin and lanolin. It can also be obtained by acylation, oxidation, hydrazone, dehydration, and saponification of cholesterol. , and vitamin D3 is a kind of vitamin D, also known as cholecalciferol, vitamin D3 can improve the body's absorption of calcium and phosphorus, promote growth and bone calcification, saturate plasma calcium and plasma phosphorus, and can also repair high blood pressure, Cardiovascular damage such as diabetes. [0003] Prior art For the recovery and purification of 7-dehydrocholesterol, the methods of concentration and low-temperatur...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J9/00C07C401/00
CPCC07J9/00C07C401/00C07C2601/14C07C2602/24
Inventor 陈钢陈发吴文彬温昊李洋童丽刘宗京袁月黄玉兰
Owner ZHEJIANG NHU CO LTD
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