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: 2012-07-04
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
  • Vitamin D3 preparation method and device

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] As shown in the figure, the equipment used in the post-treatment process is composed of a crystallization-filter 14 and a tail gas condenser 15 connected in series with it. The crystallization-filter 14 is composed of a container body, a plurality of tubes 16 placed in the container body, Jacket 5 on the container body and steam inlet valve 1, nitrogen inlet valve 3, photochemical reaction liquid inlet valve 4, washing solvent inlet valve 6, 7-dehydrocholesterol feeding inlet valve installed on the container body 7. The outlet valve 10 and the filtrate outlet valve 11 are composed. The jacket 5 is equipped with a chilled brine backwater 9, an inlet valve 8, and the tail gas condenser 15 is also equipped with a chilled brine backwater 12 and an inlet valve 13. The aforementioned filtrate discharge valve 11 is connected to a filtrate concentration kettle, and the discharge valve 10 is directly connected to the photochemical reactor. The outer surface of the tube 16 is wrap...

Embodiment 2

[0023] When the reaction liquid obtained from the photochemical reaction is subjected to post-treatment, the crystallization-filter drain valve is opened, the frozen brine return water 12 of the tail gas condenser, and the water inlet valve 13 are opened. Open the feed port valve 4 and put 1000Kg of the photochemical reaction liquid (which contains 700Kg of cyclohexane, 200Kg of ethanol, 56Kg of 7-dehydrocholesterol, 56Kg of 7-dehydrocholesterol, and vitamin D) into the crystallization-filter. 3 Crude oil 14Kg). After the feed is completed, open the crystallization-filter jacket frozen brine return valve 2 and the water inlet valve 8, and pass the -20°C frozen brine into the crystallization-filter jacket for frozen crystallization. When the temperature in the crystallization-filter reaches below -5°C, start timing, and the crystallization can end after about 5 hours.

[0024] After the crystallization is completed, turn off the chilled brine inlet 13 and the return valve 12 of th...

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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 equipment used. Background technique [0002] Vitamin D 3 The synthesis of 7-dehydrocholesterol is usually used to dissolve 7-dehydrocholesterol in a suitable solvent, and carry out the photochemical reaction through a photochemical reactor. Due to the self-absorption effect of the 7-dehydrocholesterol solution, the concentration of the reaction solution cannot be too high (usually less than 5% by weight); at the same time, a too high reaction concentration will increase the viscosity of the reaction solution and reduce the mass transfer effect. Formed by-products of irradiation. Usually get high vitamin D 3 The content must be a low-concentration reaction solution, a low-viscosity solvent, and a low conversion rate (not more than 40%). Sometimes a temperature slightly lower than the boiling po...

Claims

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Application Information

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