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Method for photochemically synthesizing vitamin D2 and D3 in tubular reactor

A tubular reactor, photochemical synthesis technology, applied in the direction of organic chemistry, etc., can solve the problems of changing the residence time of reactants, gas expansion, fusion and acceleration of total flow rate, etc.

Active Publication Date: 2018-12-25
SHANDONG TSINGCHUANG CHEMICALSCO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the application of gas separation is limited, especially for high-pressure systems, the requirements for gas transmission power are high; and affected by the large pressure drop in microchannels and tubular reactors, the pressure of the gas column continues to drop during the flow process , the phenomenon of gas expansion occurs, causing the fusion of adjacent liquid columns and the acceleration of the total flow rate, thereby changing the residence time of the reactants; in addition, many photochemical reactions use highly volatile solvents, and the way of gas separation is at the outlet of the reactor. It is easy to bring out volatile organic gases, which will further cause the problem of exhaust emissions

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  • Method for photochemically synthesizing vitamin D2 and D3 in tubular reactor
  • Method for photochemically synthesizing vitamin D2 and D3 in tubular reactor
  • Method for photochemically synthesizing vitamin D2 and D3 in tubular reactor

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Embodiment 1

[0044] Photochemical reaction synthesis of vitamin D in the tubular reactor of Example 1 of the present invention 3 The method of the method, wherein the tubular photochemical reaction device comprises a tubular reactor, a light source and a cold trap.

[0045] The liquid-liquid micro-mixing unit is a coaxial ring tube structure, the inner diameter of the inner channel is 0.2mm, and the inner diameter of the outer channel is 2mm; the light source is a 1000-watt high-pressure mercury lamp; the cold trap is made of quartz glass, which filters out ultraviolet light below 200nm. Cover the high-pressure mercury lamp; the tubular reactor is a quartz glass tube with an inner diameter of 2mm and an outer diameter of 4mm, and the tubular reactor is spirally wound outside the quartz glass tube.

[0046] Synthesis of vitamin D by photochemical reaction using the above-mentioned device 2 The steps are:

[0047] 1) Using ethanol as a solvent, prepare 150 mL of an ergosterol solution with...

Embodiment 2

[0051] Photochemical reaction synthesis of vitamin D in the tubular reactor of Example 2 of the present invention 2 The method, the device is composed of a liquid-liquid micro-mixing unit and a tubular photochemical reaction device, that is, a liquid-liquid micro-mixing unit and a tubular photochemical reaction device (including a tubular reactor, a light source and a cold trap).

[0052] The liquid-liquid micro-mixing unit has a Y-shaped structure, and the inner diameter of the two branch channels is 1mm; the light source is a 100-watt high-pressure mercury lamp; the cold trap is made of silicate glass, which filters out ultraviolet light below 280nm and covers the high-pressure mercury lamp The tubular reactor is a quartz glass tube with an inner diameter of 2 mm and an outer diameter of 4 mm, and the tubular reactor is spirally wound outside the quartz glass tube.

[0053] Synthesis of vitamin D by photochemical reaction using the above-mentioned device 2 The steps are:

...

Embodiment 3

[0058] Photochemical reaction synthesis of vitamin D in the tubular reactor of Example 3 of the present invention 3 The method, the device is composed of a liquid-liquid micro-mixing unit and a tube-type photochemical reaction device, that is, a liquid-liquid micro-mixing unit and a tube-type photochemical reaction device (including a tube reactor and a light source).

[0059] The liquid-liquid micro-mixing unit is a T-shaped structure, the inner diameter of the main channel is 1mm, and the inner diameter of the side channel is 0.05mm; the light source is an 8-watt low-pressure mercury lamp, and the main wavelength is 308nm; Fluoroethylene propylene copolymer tube, the tubular reactor is spirally wound outside the low-pressure mercury lamp, and the distance between the control tube wall and the mercury lamp is 3cm.

[0060] Use the above-mentioned device to carry out photochemical reaction to synthesize vitamin D 3 The steps are:

[0061] 1) Using methyl tert-butyl ether as ...

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Abstract

The invention relates to a method for photochemically synthesizing vitamin D2 and D3 in a tubular reactor. The method is characterized in that the vitamin D2 and D3 are synthesized by ultraviolet light of different bands, the residence time of reaction liquid fed at different times in the tubular reactor is controlled to be the same by not dissolving with reaction liquid, not participating in reaction liquid separation and carrying ergosterol and 7-dehydrocholesterol reaction liquid and enhancing internal disturbance of the reaction liquid; the method has the advantages of continuous, stable and high efficiency of solar energy utilization, the operation is simple, and the process is controllable; the method has great prospect in the industrial production of the photochemically synthesizedvitamin D2 and D3.

Description

technical field [0001] The invention belongs to the field of organic photochemical synthesis, in particular to photochemical synthesis of vitamin D in a tubular reactor 2 、D 3 Methods. Background technique [0002] Among vitamin D compounds, vitamin D 2 、D 3 It has the most prominent effect on the human body. It can promote the absorption of calcium and phosphorus by the human body to form and maintain the mechanical strength of bones. Vitamin D 2 Mainly synthesized by photochemical reaction of ergosterol, vitamin D 3 It is mainly synthesized by photochemical reaction of 7-dehydrocholesterol, and the photochemical reaction process of the two is very similar [Fuse, S.; Tanabe, N.; Yoshida, M.; Yoshida, H.; Doi, T., Takahashi, T. , Chem.Commun.2010,46,8722], each compound has only the difference of R group, and the main reaction and side reaction involved are shown in the following formula. From the reactions involved, it can be seen that the light ring-opening step is ...

Claims

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Application Information

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IPC IPC(8): C07C401/00
CPCC07C401/00C07C2601/14C07C2602/24
Inventor 陈桂光杜乐申春
Owner SHANDONG TSINGCHUANG CHEMICALSCO LTD
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