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Technology for preparing vitamin D3

A vitamin and process technology, applied in the field of preparation technology of pure vitamin D3, can solve the problems of low separation yield and difficult separation, and achieve the effects of simple process, high efficiency and low cost

Inactive Publication Date: 2013-01-02
ZHEJIANG GARDEN BIOCHEM HIGH TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] CN1709869A proposes to use column chromatography to separate vitamin D3 actinic oil, but usually tachysterol is contained in vitamin D3 actinic oil, and the ratio of tachysterol can account for 17%-20%. Since vitamin D3 and tachysterol are similar in nature, adopt The column chromatography method is difficult to separate the two, and the separation yield is low, and the average yield is no more than 30%.

Method used

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  • Technology for preparing vitamin D3

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Dissolve 1kg of 7-dehydrocholesterol with a content of 95% at a concentration of 3wt.% in 22L methanol + 11L n-hexane at 40°C to make a 7-dehydrocholesterol solution, and turn on the photochemical water cooler, nitrogen, and circulating water pump , High-pressure mercury lamp, turn on the magnetic pump to pass the 7-dehydrocholesterol solution into the photochemical reactor, control the reaction temperature to 40°C, carry out the photochemical reaction at a flow rate of 0.5L / min, collect the photochemical reaction solution to detect the conversion rate of 14%, and perform decompression Recover n-hexane and methanol, control the temperature at about 30°C to distill 80%, and centrifuge to obtain 0.75 kg of 7-dehydrocholesterol, which is used again. The filtrate is stirred and frozen at -10°C for 10 hours, and then filtered to obtain Contain the solution of a large amount of vitamin P3, the filtrate is all reclaimed, obtain the oily solid containing 75% vitamin P3, 5% vitam...

Embodiment 2

[0020] 750 grams of 7-dehydrocholesterol recovered from Example 1 + 250 grams of 95% fresh 7-DHC were dissolved in 22L methanol + 11L n-hexane at a temperature of 45°C at a concentration of 3% to prepare 7-dehydrocholesterol solution, turn on the photochemical water cooler, nitrogen, circulating water pump, and high-pressure mercury lamp, turn on the magnetic pump to pass the 7-dehydrocholesterol solution into the photochemical reactor, control the reaction temperature at 45°C, and carry out the photochemical reaction at a flow rate of 0.6L / min. For the reaction solution, first detect the conversion rate of 12%. After the detection, recover methanol and n-hexane. Control the temperature at about 30°C to recover 75% of methanol and n-hexane. After centrifugation, 0.7 kg of 7-dehydrocholesterol is obtained. Apply mechanically for the first time, the filtrate was frozen and crystallized at -10°C for 8 hours, and then filtered to obtain a solution containing a large amount of vitam...

Embodiment 3

[0022] 750 grams of 7-dehydrocholesterol recovered from Example 2 + 250 grams of 95% fresh 7-DHC were dissolved in 22L methanol + 11L n-hexane at a temperature of 45°C at a concentration of 3% to prepare 7-dehydrocholesterol solution, turn on the photochemical water cooler, nitrogen, circulating water pump, and high-pressure mercury lamp, turn on the magnetic pump to pass the 7-dehydrocholesterol solution into the photochemical reactor, control the reaction temperature at 45°C, and carry out the photochemical reaction at a flow rate of 0.6L / min. For the reaction solution, first detect the conversion rate of 12%. After the detection, recover methanol and n-hexane. Control the temperature at about 30°C to recover 75% of methanol and n-hexane. After centrifugation, 0.7 kg of 7-dehydrocholesterol is obtained. For the first time, the filtrate was frozen and crystallized at -10°C for 8 hours, and then filtered to obtain a solution containing a large amount of vitamin P3. The filtrate...

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Abstract

The invention discloses a technology for preparing vitamin D3. The technology comprises the following steps of: (1) preparing a 1wt%-3wt% 7-dehydrocholesterol solution, and passing the 7-dehydrocholesterol solution through a photochemical reactor filled with nitrogen for carrying out photochemical reaction, wherein the reaction temperature is controlled within the range of 35-50 DEG C and the conversion rate is controlled within the range of 10-20%; collecting a photochemical reaction liquid, recovering 70-80% of solvent, centrifuging and recovering the 7-dehydrocholesterol, and crystallizing and filtering filtrate, and recovering the solvent from the filtrate to obtain vitamin P3 mixture; (2) dissolving the vitamin P3 mixture into an adsorption solvent, and carrying out column chromatography separation to obtain vitamin P3 component; and (3) carrying out thermal isomerization reaction on the vitamin P3 component, basically converting the vitamin P3 into the vitamin D3, then freezing and crystallizing to obtain the vitamin D3 crystal. The technology is simple in technical process, large in handling capacity, low in toxicity and environmental pollution and high in yield, thus the technology is used for preparing the vitamin D3 pure product which is in accordance with the requirements of pharmacopeia.

Description

technical field [0001] The invention belongs to the field of fine chemicals, and relates to a preparation process of pure vitamin D3, in particular to a preparation process of pure vitamin D3 meeting the requirements of the Pharmacopoeia. Background technique [0002] Vitamin D3 is one of the important vitamins essential for human health, normal growth and reproduction of livestock and poultry. With the in-depth research on vitamin D3, it is found that vitamin D3 has good effects in anti-cancer and improving immunity. Vitamin D3 pure The product market is growing at a rate of 30% every year. Therefore, a technology with simple process, low cost and industrialization is required to meet the ever-increasing market demand. [0003] CN1445215A discloses a method for photochemically synthesizing vitamin D3. First, 7-dehydrocholesterol is dissolved in a non-polar-polar solvent mixed system, and an antioxidant is added for photochemical reaction to generate vitamin P3. After recyc...

Claims

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Application Information

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IPC IPC(8): C07C401/00
Inventor 王子强刘建刚钱国平刘小平
Owner ZHEJIANG GARDEN BIOCHEM HIGH TECH
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