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Actinic chemistry reaction device and method for synthesizing provitamin D3

A technology of photochemical reaction and synthesis method, applied in the field of photochemical reactors, can solve problems such as instability and unsuitability for industrial production, and achieve the effect of high utilization rate of light source

Active Publication Date: 2007-12-12
XIAMEN KINGDOMWAY VI TAMIN INC +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But because D 3 Instability, two times of light will further occur secondary reactions, generate photochemical reaction by-products, and generate some harmful over-irradiation products, such as toxic sterol, supersterol, vitamin D 3 , Isovitamin D 3 , this process is not suitable for industrial production

Method used

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  • Actinic chemistry reaction device and method for synthesizing provitamin D3

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Dissolve 5 g of the 7-DHC sample in 1000 ml of ethanol, the 7-DHC content is 97.5%, and the container is evacuated and protected by nitrogen. Use 0.7M NaWO 4 As filter a, 1.1MCoSO 4 -5% H 2 SO 4 As a filter b. The filter solution a is passed through the inner jacket of the actinator, and the filter solution b is passed through the outer jacket of the actinator. The filter solution is circulated closely through the condenser to maintain a constant temperature of the filter solution at 24°C. Turn on the mercury lamp power supply, when the current reaches the rated current, start feeding, the 7-DHC solution is fed from the bottom of the actinator, adjust the flow meter to 6L / h, and at the same time pass nitrogen through the feeding tube to control the material layer of the actinator mixing. The reaction temperature under illumination is 36.3℃, and the finished solution is sampled and tested after illumination. Vitamin D is pre-examined. 3 The content is 68.7%.

[0026] Pre-vit...

Embodiment 2

[0028] Dissolve 5 g of the 7-DHC sample in 1000 ml of ethanol, and the 7-DHC content is 97.1%. The container is evacuated and protected by nitrogen. Use 0.7M NaWO 4 , 0.7MPbAc as filter a, 1.05MCoSO 4 -6%H 2 SO 4As a filter b. The filter solution a is passed through the inner jacket of the actinator, and the filter solution b is passed through the outer jacket of the photochemical device. The filter solution is circulated through the condenser to keep the filter solution at a constant temperature of 25°C. Turn on the power of the mercury lamp and start feeding when the current reaches the rated current. The 7-DHC solution is fed from the bottom of the actinator, and the flowmeter is adjusted to 6L / h. At the same time, nitrogen is introduced from the feed pipe to mix the material layer of the actinator. The reaction temperature was 35.5°C under illumination. Sampling and testing of the finished liquid after illumination, pre-vitamin D 3 The content is 68.2%.

Embodiment 3

[0030] Dissolve 5 g of the 7-DHC sample in 1000 ml of ethanol, and evacuate the container with nitrogen protection. Use 0.75M NaWO with 7-DHC content 97.7% 4 As filter a, 1.0MCoSO 4 , 0.8MNiSO 4 -5% H 2 SO 4 As a filter b. The filter solution a is passed through the inner jacket of the photochemical device, and the filter solution b is passed through the outer jacket of the photochemical device. The filter solution is circulated through the condenser to maintain a constant temperature of the filter solution at 23°C. Turn on the power of the mercury lamp and start feeding when the current reaches the rated current. The 7-DHC solution is fed from the bottom of the actinator, and the flowmeter is adjusted to 6L / h. At the same time, nitrogen is introduced from the feed pipe to mix the material layer of the actinator. Illumination reaction temperature is 36℃, sampling and testing of finished liquid after illumination, pre-vitamin D 3 The content is 68.5%.

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Abstract

The invention discloses a photochemical reaction device and a method for synthesizing vitamin D3 by using narrowed high-voltage mercury lamp wavelength and one- step optical isomerism, relating to a vitamin D3. It comprises container, internal pipe, mercury vapour lamp, mediolateral jacket and collecting bottle, the mercury vapour lamp is installed in internal pipe, external jacket is set inside of internal pipe, internal jacket is installed outside of internal pipe, internal jacket is installed between internal tubular lamp and external jacket, the irradiation liquid export of container is connected with collecting bottle. Said method comprises following steps: preparing 7- desmesterol solution and dissloving it in ethanol; evacuating and ventilating nitrogen gas, preparing solution with sodium tungstate or acetate of lead, feeding it into external jacket as filtering liquid, preparing solution with cobalt sulfate, nickel sulfate, sulphuric acid and water, feeding it into internal jacket as filtering liquid, feeding 7- desmesterol solution from feed inlet through condenser circulation for photochemical reaction, ventilating nitrogen gas from feed inlet to mix with 7- desmesterol solution, discharging solution after photochemical process into collecting bottle.

Description

Technical field [0001] The present invention relates to a pre-vitamin D 3 In particular, it relates to a photochemical reactor and the use of one-step photoisomerization method to improve the synthesis of pre-vitamin D from 7-dehydrocholesterol 3 The method of yield. Background technique [0002] Pre-vitamin D 3 In the photochemical synthesis of X-ray, the ultraviolet wavelength plays a decisive role in the distribution of 7-dehydrocholesterol (7-DHC) illumination products. 7-DHC isomerization to generate pre-vitamin D 3 The optimal wavelength of 295nm is 295nm. After irradiated by 295nm ultraviolet wavelength, vitamin D 3 The content is 70%. Single-wavelength ultraviolet light can improve pre-vitamin D 3 The yield. At present, the control of a single ultraviolet wavelength can only be achieved by a tunable wavelength ultraviolet laser. William G et al. (William G, Daubenand Richard B, Phillips. J. AM. Chen. Soc. 1982, 104: 5780-5781) have done a lot of research on laser irradiat...

Claims

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Application Information

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IPC IPC(8): C07C401/00B01J19/08
Inventor 何剑洋吴轶郑文
Owner XIAMEN KINGDOMWAY VI TAMIN INC
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