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A photoreaction device and its application in the preparation of hydroxocobalamin or its salt

A technology of photoreaction and hydroxocobalamin, applied in the preparation of hydroxocobalamin or its salt, in the field of photoreaction equipment, can solve the problems of loss of product yield, product quality decline, low reaction efficiency, etc., and achieve production efficiency improvement , energy-saving reaction, and high reaction efficiency

Active Publication Date: 2020-11-06
HEBEI HUARONG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This will lead to low reaction efficiency and reduced product quality.
In the refining process, in order to improve the product quality, it is necessary to carry out the layering operation, which will inevitably lose the yield of the product

Method used

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  • A photoreaction device and its application in the preparation of hydroxocobalamin or its salt
  • A photoreaction device and its application in the preparation of hydroxocobalamin or its salt
  • A photoreaction device and its application in the preparation of hydroxocobalamin or its salt

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Embodiment 1 Photoreaction equipment

[0039] see figure 1 , figure 2 , the photoreaction equipment of the present invention comprises illumination reaction device 2, circulating pump 3, mixing stirring device 1 and air filter 4, and described illumination reaction device 2 is made of shell case 2-1, strong light 2-2, reaction tank 2 -3 and aeration pipe 2-4, the cover of the shell box 2-1 is hinged with the box body, the front side of the box body is a detachable structure, and the side wall of the box body is a porous structure wall plate, in which A diffuse reflector 2-5 is installed on the inner wall, the strong light 2-2 is installed on the box cover, the reaction tank 2-3 is placed on the slide rail 2-7 at the bottom of the shell box, and the reaction tank 2-3 3 The slide block 2-6 fitted with the slide rail 2-7 is installed on the bottom surface, and the aeration tube 2-4 is located inside the reaction tank 2-3 and immersed in the reaction substance 5.

[004...

Embodiment 2

[0044] Embodiment 2: Adopt photoreaction equipment of the present invention to carry out the preparation of hydroxocobalamin or its salt

[0045] Dissolve 500 grams of methylcobalamin in 120 liters of deionized water, use hydrochloric acid to adjust its pH value to 3.5, place it in the reaction tank, open the circulation pump, open the discharge valve and the return valve of the pump, and pass through the opening of these two valves. Keep the liquid level in the reaction tank at 5-7 cm. After the liquid level is stable, turn on the energy-saving lamp, confirm that the illuminance in the reaction tank is above 30,000LUX, and open the air valve to allow the aeration tube to evenly aerate the entire reaction liquid level. During the reaction, 3M hydrochloric acid was used to maintain the pH value of the reaction solution at 3.0-4.0, and the reaction was confirmed by HPLC for 3 hours, and the methylcobalamin was less than 0.2%.

[0046] Adsorb the obtained reaction solution in a ...

Embodiment 3

[0047] Embodiment 3: Adopt photoreaction equipment of the present invention to carry out the preparation of hydroxocobalamin or its salt

[0048] Dissolve 1000 grams of adenosylcobalamin in 200 liters of deionized water, use glacial acetic acid to adjust its pH value to 3.8, place it in the reaction tank, turn on the circulation pump, open the discharge valve and the return valve of the pump, and control the two The opening of the valve maintains the liquid level in the reaction tank at 5-7 cm. After the liquid level is stable, turn on the energy-saving lamp, confirm that the illuminance in the reaction tank is above 30000 lux, and open the air valve to allow the aeration tube to evenly aerate the entire reaction liquid level. During the reaction, glacial acetic acid was used to maintain the pH value of the reaction solution at 3.0-4.0, and the reaction end point was confirmed by HPLC after 4 hours of reaction, and methylcobalamin was less than 0.2%.

[0049] Adsorb the obtai...

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Abstract

The invention relates to a light reaction device and applications in preparation of hydroxycobalamin or salts thereof. The light reaction device comprises a light reaction device, a circulating pump, a mixing and stirring device and an air filter. The light reaction device is composed of a housing box, a strong light, a reaction tank and an aerated pipe. The side walls of the box body of the housing box are wallboards with porous structures. Diffuse reflection plates are arranged at the inner sides of the side walls. The strong light is arranged on the box cover. The reaction tank is arranged at the bottom of the housing box. The aerated pipe is arranged inside the reaction tank and immersed in reactive substances. Through the light reaction device, the reaction conversion rates of methylcobalamin and cobamamide in an aqueous solution reach above 99%, the chromatographic purity of the generated hydroxycobalamin reaches above 98%, the product yield reaches above 98%, and the production efficiency is raised by above 5 times compared with that of a normal reactor.

Description

technical field [0001] The invention belongs to the technical field of organic chemical industry, and relates to a photoreaction device and its application in preparing hydroxocobalamin or its salt. Background technique [0002] Organic cobalamins such as methylcobalamin and adenosylcobalamin contain Co-C bonds in their molecules. Since Co atoms and C atoms have strong electron repelling effects, the chemical bonds are easily broken when exposed to light, and Co- After the C bond is broken, Co ions are oxidized immediately to generate hydroxocobalamin. Therefore, hydroxocobalamin and its salts can be prepared in the chemical and pharmaceutical industry according to this theory. [0003] At present, the main equipment used to produce hydroxocobalamin and its salts is a photoreactor. The Chinese Patent No. CN200520123882.7 "forced circulation photoreactor" discloses a device that uses cyanocobalamin to produce hydroxocobalamin through light. . Although it can ensure the cont...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J19/12C07H23/00C07H1/00
Inventor 陈学军李振东任静赵浪涛任洁付海云张京月王欢殷小江谭锟刘少卿贾伟娜马蕙赵宇
Owner HEBEI HUARONG PHARMA
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