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Vitamin D3 preparation method and device

A technology of vitamins and equipment, applied in the field of vitamins, can solve the problems of large ultraviolet absorption, many side reactions of polymerization, and no consideration of use, etc., and achieve the effect of high content, less side reactions of polymerization, and avoid deterioration

Active Publication Date: 2009-03-11
ZHEJIANG NHU CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

General alcohol solvents can basically meet the requirements of photochemical reaction, but the disadvantage is that the viscosity is too large and the solubility is too small
However, benzene ring solvents with low viscosity and high solubility are basically not considered to be used due to their large absorption of ultraviolet rays.
A single hydrocarbon solvent is too weak to cause free radical oxidation, resulting in too many polymerization side reactions

Method used

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  • Vitamin D3 preparation method and device
  • Vitamin D3 preparation method and device

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] As shown in the figure, the used equipment of aftertreatment process is made up of crystallization-filter 14 and tail gas condenser 15 connected in series with it, and described crystallization-filter 14 is made up of container body, a plurality of tubes 16 placed in the container body, Jacket 5 set on the container body and steam inlet valve 1 installed on the container body, nitrogen inlet valve 3, photochemical reaction liquid inlet valve 4, washing solvent inlet valve 6, 7-dehydrocholesterol inlet valve 7. The liquid outlet valve 10 and the filtrate outlet valve 11 are composed. The jacket 5 is equipped with a frozen brine return water 9 and a water inlet valve 8. The tail gas condenser 15 is also equipped with a frozen brine return water 12 and a water inlet valve 13. The above-mentioned filtrate discharge valve 11 is connected with a filtrate concentration tank, and the discharge valve 10 is directly connected with the photochemical reactor. The outer surface of t...

Embodiment 2

[0023] When post-processing the reaction liquid obtained by the photochemical reaction, open the crystallization-filter emptying port valve, open the tail gas condenser frozen brine return water 12, and the water inlet valve 13. Open the feed inlet valve and 4-way crystallization—put 1000Kg of transposed photochemical reaction liquid into the filter (including 700Kg of cyclohexane, 200Kg of ethanol, 56Kg of 7-dehydrocholesterol, vitamin D 3 crude oil 14Kg). After the feeding is completed, open the crystallization-filter jacket frozen brine return valve 2 and water inlet valve 8, and feed -20°C frozen brine into the crystallization-filter jacket to carry out freeze crystallization. When the temperature in the crystallization-filter reaches below -5°C, start counting, and the crystallization can end after about 5 hours.

[0024] After the crystallization is complete, close the tail gas condenser frozen brine water inlet 13 and return water valve 12. Open crystallization-the fi...

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Abstract

The invention discloses a method for preparing vitamin D3 and used equipment. In the prior method, a solvent must be replaced during the crystallization process of the post-treatment, and the heating time is long, which affect the content of a final product. A solvent used by the method in a photochemical reaction is a mixed solvent consisting of a high melting point solvent and a low melting point solvent; an obtained photochemical reaction liquid is subjected to freezing crystallization and filtering post-treatment after the photochemical reaction is finished; and crude vitamin D3 oil is obtained after filtrate is concentrated; after a filter cake is heated and dissolved, 7-dehydrocholesterol and the low melting point solvent which is concentrated from the filtrate are added to serve as raw materials for the photochemical reaction; the high melting point solvent is alcoholic solvents or hydrocarbon solvents with melting points of between 10 DEG C below zero and 10 DEG C, and the low melting point solvent is alcohol solvents with melting points less than or equal to 50 DEG C below zero. The vitamin D3 obtained by the method has high content and less polymerization side reactions, does not need to replace the solvent during the post-treatment process, and has good quality.

Description

technical field [0001] The invention relates to the field of vitamins, in particular to a vitamin D obtained by photochemical reaction of 7-dehydrocholesterol 3 The preparation method and the equipment used. Background technique [0002] Vitamin D 3 The synthesis of usually adopts dissolving 7-dehydrocholesterol in a suitable solvent and carrying out a photochemical reaction through a photochemical reactor. Due to the self-absorption effect of the 7-dehydrocholesterol solution, the solution concentration of the reaction cannot be too high (usually lower than 5% weight concentration); at the same time, too high a reaction concentration will cause an increase in the viscosity of the reaction solution, and the mass transfer effect will easily decline. Over-irradiation by-products are formed. Usually to get high vitamin D 3 The content must adopt low-concentration reaction solution, low-viscosity solvent, low conversion rate (no more than 40%), and sometimes needs to adopt t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C401/00
Inventor 张谦石程杨芝
Owner ZHEJIANG NHU CO LTD
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