CN112495324B - Photochemical reaction device - Google Patents
Photochemical reaction device Download PDFInfo
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- CN112495324B CN112495324B CN202011224984.3A CN202011224984A CN112495324B CN 112495324 B CN112495324 B CN 112495324B CN 202011224984 A CN202011224984 A CN 202011224984A CN 112495324 B CN112495324 B CN 112495324B
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
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Abstract
The invention relates to photochemical reaction equipment and discloses a photochemical reaction device. The photochemical reaction device comprises a reaction kettle, a transparent tube positioned inside the reaction kettle and a transparent tube positioned inside the reaction kettleA light source and a liquid conveying mechanism inside the exposed pipe, wherein an inner overflow groove and an outer overflow groove are arranged in the inner cavity of the reaction kettle, and a feed inlet is formed on the inner overflow groove; the inner overflow groove is also provided with an inner overflow port facing the outer wall of the transparent pipe, so that the reaction liquid in the inner overflow groove can overflow from the inner overflow port and flow down along the outer wall of the transparent pipe, the outer overflow groove is provided with an outer overflow port facing the inner wall of the reaction kettle, so that the reaction liquid in the outer overflow groove can overflow from the outer overflow port and flow down along the inner wall of the reaction kettle, and the reaction liquid conveying mechanism can collect the reaction liquid flowing down from the outer wall of the transparent pipe and convey the reaction liquid into the outer overflow groove. The reaction device can utilize the reaction liquid to filter light and improve the generation of vitamin D by photochemical reaction3Yield and purity.
Description
Technical Field
The invention relates to photochemical reaction equipment, in particular to a photochemical reaction device.
Background
Vitamin D3The vitamin is used as an additive for mainly regulating the metabolism of calcium and phosphorus of human bodies and animals, promoting the absorption of calcium and phosphorus by intestinal tracts, controlling the excretion of calcium and phosphorus and the storage and transformation of calcium and phosphorus in bones, and is an essential vitamin for the normal growth of the human bodies and the animals. Industrial production of vitamin D3The intermediate 7-dehydrocholesterol is generally adopted by a photochemical method and is firstly converted into vitamin D after being irradiated by ultraviolet light (the wavelength is 280-310nm)3precursor-Previtamin D3And then converted into vitamin D by thermal isomerization3。
At present, vitamin D3In the production of the ultraviolet light source, an ultraviolet high-pressure mercury lamp is usually adopted as the ultraviolet light source, and the spectrum emitted by the ultraviolet high-pressure mercury lamp covers the whole ultraviolet region, and contains both required ultraviolet light and redundant stray light. Therefore, the photochemical reaction process is exceptIn addition to the products, a large amount of tachysterol, a toxic by-product, is also produced. In order to reduce the generation of the reaction by-products of the illumination, various researches including the use of light filtering liquid, light filtering glass, and the use of LED light source have been carried out at home and abroad, but such researches or applications have not been realized industrially because of poor effects or limited by equipment cost. Thus, vitamin D3Production of (A) it is highly desirable to provide a composition capable of increasing vitamin D3And an industrial process or apparatus for reducing by-products.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a photochemical reaction device, which can utilize reaction liquid to filter light, improve the photocatalytic efficiency and improve the generation of vitamin D by photochemical reaction3Yield and purity.
The inventor of the present application found in the research that 7-dehydrocholesterol produces vitamin D by a photochemical method3The wavelength of the required ultraviolet light is 280-310nm, meanwhile, the byproduct tachysterol is generated under the action of the ultraviolet light with the wavelength of 250nm, most of short-wave light below 310nm is filtered after the light emitted by the high-pressure mercury lamp passes through the reaction liquid of the reaction, and most of the transmitted light is the ultraviolet light with the wavelength of above 310 nm. Because tachysterol can be converted into pre-vitamin D under the irradiation of ultraviolet light with the wavelength of about 350nm3Thus, the present application utilizes a light source to produce vitamin D via 7-dehydrocholesterol3The light penetrating from the reaction liquid promotes the reversion of the sterol in the reaction system, thereby improving the vitamin D3Yield and purity.
In order to solve the technical problems, based on the findings, the invention provides a photochemical reaction device, which comprises a reaction kettle, a transparent tube positioned inside the reaction kettle, a light source positioned inside the transparent tube and a liquid conveying mechanism, wherein an inner overflow groove and an outer overflow groove are arranged in an inner cavity of the reaction kettle, and a feed inlet is arranged on the inner overflow groove; the inner overflow groove is also provided with an inner overflow port facing the outer wall of the transparent pipe, so that the reaction liquid in the inner overflow groove can overflow from the inner overflow port and flow down along the outer wall of the transparent pipe, the outer overflow groove is provided with an outer overflow port facing the inner wall of the reaction kettle, so that the reaction liquid in the outer overflow groove can overflow from the outer overflow port and flow down along the inner wall of the reaction kettle, and the reaction liquid conveying mechanism can collect the reaction liquid flowing down from the outer wall of the transparent pipe and convey the reaction liquid into the outer overflow groove.
Preferably, an inner guide plate facing the transparent pipe is arranged at the inner overflow port on the inner overflow groove, the inner guide plate can guide the reaction liquid overflowing from the inner overflow port to the outer wall of the transparent pipe, an outer guide plate facing the reaction is arranged at the outer overflow port on the outer overflow groove, and the outer guide plate can guide the reaction liquid overflowing from the outer overflow port to the inner wall of the reaction kettle.
More preferably, the inner deflector is hinged to the inner overflow chute, and the outer deflector is hinged to the outer overflow chute.
Further preferably, the length of the inner guide plate extending towards the transparent pipe is matched with the distance from the inner overflow port to the outer wall of the transparent pipe, and the length of the outer guide plate extending towards the reaction kettle is matched with the distance from the outer overflow port to the inner wall of the reaction kettle.
Specifically, the distance from the inner overflow port to the outer wall of the transparent pipe is 1-5cm, and the distance from the outer overflow port to the inner wall of the reaction kettle is 1-5 cm.
Typically, the distance between the inner overflow port and the bottom of the inner overflow groove is 3-20cm, and the distance between the outer overflow port and the bottom of the outer overflow groove is 3-20 cm.
As a preferable mode, the inner overflow groove and the outer overflow groove are connected through a partition plate, a balance hole is arranged on the partition plate, and the height of the balance hole is higher than the height of the inner overflow port and the height of the outer overflow port.
Preferably, the transparent pipe and the reaction kettle are respectively of a double-layer jacket structure, a refrigerant inlet and a refrigerant outlet are respectively arranged on the double-layer jacket structure, and each refrigerant inlet and each refrigerant outlet are respectively connected with a reflux condenser.
More preferably, the inner cavity of the reaction kettle is further provided with a gas distributor for introducing protective gas into the reaction kettle.
Specifically, the liquid conveying mechanism comprises a collecting tank and a transfer tank which are positioned in the reaction kettle, the collecting tank is positioned below the transparent pipe, the bottom of the collecting tank is connected with the transfer tank and the bottom of the transfer tank is connected with the overflow tank through liquid conveying pipelines respectively, and a liquid pump is arranged on the liquid conveying pipeline between the transfer tank and the overflow tank.
Through the technical scheme, the photochemical reaction device provided by the invention utilizes the inner overflow groove and the inner overflow port facing the outer wall of the transparent pipe, so that the reaction liquid entering the inner overflow groove from the feeding hole can overflow from the inner overflow port and flow down along the outer wall of the transparent pipe to form a liquid film, the reaction liquid flowing down from the outer wall of the transparent pipe is collected and conveyed into the outer overflow groove through the reaction liquid conveying mechanism, then overflows from the outer overflow port and flows down along the inner wall of the reaction kettle to form the liquid film again, at the moment, the light of the light source can sequentially penetrate through the liquid film on the outer wall of the transparent pipe and the liquid film on the inner wall of the reaction kettle, so that the reaction liquid is subjected to primary illumination reaction on the outer wall of the transparent pipe, and then secondary illumination reaction is performed on the inner wall of the reaction kettle, and the generation of vitamin D by the photochemical reaction is effectively improved3The yield and purity of the photocatalyst are improved, and the photocatalytic efficiency is improved.
Other technical features and advantages of the present invention will be further described in the following detailed description.
Drawings
The following drawings are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the scope of the invention. In the drawings:
FIG. 1 is a schematic structural diagram of an embodiment of a photochemical reaction apparatus according to the present invention;
FIG. 2 is a schematic structural view of an embodiment of the overflow launder and reactor of the present invention;
FIG. 3 is a schematic diagram of the construction of one embodiment of the internal isopipe and transparent tube of the present invention.
Description of the reference numerals
1 reaction kettle 2 overflow groove
21 outer overflow port 22 outer flow guide plate
3 inner overflow outlet of inner overflow groove 31
32 feed inlet 33 inner guide plate
4 light source 5 transparent tube
6 collecting tank 7 transfer jar
8 liquid pump 9 reflux condenser
10 partition 11 balance hole
12 gas distributor
Detailed Description
The following detailed description of embodiments of the invention refers to the accompanying drawings. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
It should be noted that in the following description of the present invention, the terms "inside", "outside", "bottom", "below", and the like are used to indicate the orientation or positional relationship based on the orientation or positional relationship shown in the drawings, which are only used for convenience of description and simplification of description, but do not indicate or imply that the device or element referred to must have a specific orientation, be constructed in a specific orientation, and be operated, and thus should not be construed as limiting the present invention.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "connected," "mounted," and "fixed" are to be construed broadly, e.g., the connection may be a fixed connection, a detachable connection, or an integral connection; the connection may be direct or indirect through an intermediate medium, and may be a connection within two components or an interaction relationship between two components. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
The photochemical reaction device provided by the invention, referring to fig. 1 to fig. 3, comprises a reaction kettle 1, a transparent tube 5 positioned in the reaction kettle 1, a light source 4 positioned in the transparent tube 5 and a liquid conveying mechanism, wherein an inner overflow groove 3 and an outer overflow groove 2 are arranged in an inner cavity of the reaction kettle 1, and a feed inlet 32 is arranged on the inner overflow groove 3; the inner overflow groove 3 is also provided with an inner overflow port 31 facing the outer wall of the transparent pipe 5, so that the reaction liquid in the inner overflow groove 3 can overflow from the inner overflow port 31 and flow down along the outer wall of the transparent pipe 5, the outer overflow groove 2 is provided with an outer overflow port 21 facing the inner wall of the reaction kettle 1, so that the reaction liquid in the outer overflow groove 2 can overflow from the outer overflow port 21 and flow down along the inner wall of the reaction kettle 1, and the reaction liquid conveying mechanism can collect the reaction liquid flowing down from the outer wall of the transparent pipe 5 and convey the reaction liquid into the outer overflow groove 2.
The photochemical reaction device is not limited to be used for producing the vitamin D by 7-dehydrocholesterol through a photochemical method3And can also be used for other reaction processes with similar reaction principles with the photochemical reaction process. The combined 7-dehydrocholesterol is used for producing vitamin D by a photochemical method3The photochemical reaction apparatus of the present invention will be described with reference to specific operation procedures and reaction principles, and accordingly, the light source 4 is provided as an ultraviolet high-pressure mercury lamp. In the present invention, the transparent tube 5 functions to utilize the gap between the inner overflow port 31 and the outer wall of the transparent tube 5 to make the reaction liquid overflowing from the inner overflow port 31 flow down along the outer wall of the transparent tube 5 to form a liquid film, and at the same time, the light irradiated by the light source 4 can completely irradiate the liquid film on the outer wall of the transparent tube 5, so the bottom of the transparent tube 5 can be open or closed, the transparent tube 5 can be made of glass material or other transparent materials, and specifically, the transparent tube 5 is a quartz glass tube. It should be noted that a valve may be disposed on a connection line between the reaction kettle 1 and other external devices to control an open or close state of the liquid or gas to be delivered or output into the reaction kettle 1.
The photochemical reaction device of the basic technical scheme of the invention is usedThe process and the reaction principle are as follows: turning on a light source 4, inputting a reaction liquid containing 7-dehydrocholesterol into the inner overflow groove 3 from a feed inlet 32, overflowing the reaction liquid in the inner overflow groove 3 from the inner overflow opening 31 along with the rise of the liquid level of the inner overflow groove 3 to the inner overflow opening 31, flowing down along the outer wall of the transparent pipe 5 to form a liquid film, collecting and conveying the reaction liquid flowing down along the outer wall of the transparent pipe 5 to the outer overflow groove 2 through a reaction liquid conveying mechanism, and overflowing the reaction liquid in the outer overflow groove 2 from the outer overflow opening 21 along with the rise of the liquid level of the outer overflow groove 2 to the outer overflow opening 21 to form a liquid film again along the inner wall of the reaction kettle 1; at this time, the light of the light source 4 can sequentially pass through the liquid film on the outer wall of the transparent tube 5 and the liquid film on the inner wall of the reaction kettle 1, so that the reaction liquid performs a first-stage illumination reaction on the outer wall of the transparent tube 5, absorbs the ultraviolet light with the wavelength of 280-310nm and part of the ultraviolet light with the wavelength of 250nm, and generates the pre-vitamin D3And byproduct tachysterol, wherein most of light rays transmitted from the liquid film on the outer wall of the transparent tube 5 irradiate the liquid film on the inner wall of the reaction kettle 1, and the wavelength of the ultraviolet light is about 350nm, so that the reaction liquid obtained by the primary illumination reaction is subjected to secondary illumination reaction on the inner wall of the reaction kettle 1, and the tachysterol in the reaction liquid is converted into the vitamin D3Then the reaction liquid flowing down from the inner wall of the reaction kettle 1 flows out from the bottom of the reaction kettle 1 and enters the next working procedure. The photochemical reaction device can effectively improve the generation of vitamin D by the photochemical reaction3The yield and purity of the photocatalyst are improved, and the photocatalytic efficiency is improved.
In the present invention, the gap between the inner overflow port 31 and the transparent tube 5 needs to be designed to enable the reaction liquid overflowing from the inner overflow port 31 to flow down along the outer wall of the transparent tube 5 and form a liquid film, and the gap between the outer overflow port 21 and the reaction kettle 1 needs to be designed to enable the reaction liquid overflowing from the outer overflow port 21 to flow down along the inner wall of the reaction kettle 1 and form a liquid film. As a preferred embodiment of the present invention, the inner overflow launder 3 is provided with an inner guide plate 33 facing the transparent pipe 5 at the inner overflow port 31, the inner guide plate 33 can guide the reaction liquid overflowing from the inner overflow port 31 to the outer wall of the transparent pipe 5, the outer overflow launder 2 is provided with an outer guide plate 22 facing the reaction kettle 1 at the outer overflow port 21, and the outer guide plate 22 can guide the reaction liquid overflowing from the outer overflow port 21 to the inner wall of the reaction kettle 1. The reaction liquid in the inner overflow groove 3 can be completely conveyed to the outer wall of the transparent tube 5 by the diversion action of the inner diversion plate 33 and the outer diversion plate 22, and the reaction liquid in the outer overflow groove 2 can be completely conveyed to the inner wall of the reaction kettle 1 to form uniformly distributed liquid films respectively, so that the photocatalysis efficiency of the light source 4 is further improved.
Preferably, referring to fig. 2 and 3, the inner baffle 33 is hinged to the inner overflow launder 3, and the outer baffle 22 is hinged to the outer overflow launder 2, respectively. The angle between the inner guide plate 33 and the side wall of the inner overflow groove 3 and the angle between the outer guide plate 22 and the outer wall of the outer overflow groove 2 are respectively adjustable, so that the thickness of liquid films on the outer wall of the transparent pipe 5 and the inner wall of the reaction kettle 1 can be adjusted, and the reaction rate of the device can be adjusted conveniently. It should be noted that the hinges between the inner baffle 33 and the inner overflow chute 3 and between the outer baffle 22 and the outer overflow chute 2 are respectively a hinge connection piece capable of fixing an angle in the prior art, and the inner baffle 33 and the outer baffle 22 can be respectively fixed after being adjusted to a proper angle.
More preferably, the length of the inner baffle 33 extending towards the transparent pipe 5 is matched with the distance from the inner overflow port 31 to the outer wall of the transparent pipe 5, and the length of the outer baffle 22 extending towards the reaction kettle 1 is matched with the distance from the outer overflow port 21 to the inner wall of the reaction kettle 1. The length of interior guide plate 33 needs to set up to be not more than the vertical distance of interior overflow mouth 31 and hyaline tube 5, and the length of outer guide plate 22 needs to set up to be not more than the vertical distance of outer overflow mouth 21 and reation kettle 1 to it is more convenient to make the angle modulation of interior guide plate 33 and outer guide plate 22. Specifically, the distance from the inner overflow port 31 to the outer wall of the transparent tube 5 is 1-5cm, and the distance from the outer overflow port 21 to the inner wall of the reaction kettle 1 is 1-5 cm.
In the present invention, the distance between the inner overflow port 31 and the bottom of the inner overflow launder 3 and the distance between the outer overflow port 21 and the bottom of the outer overflow launder 2 are not particularly limited, but as a preferred embodiment of the present invention, the distance between the inner overflow port 31 and the bottom of the inner overflow launder 3 is 3-20cm, and the distance between the outer overflow port 21 and the bottom of the outer overflow launder 2 is 3-20cm, so as to prevent excessive reaction solution from remaining in the inner overflow launder 3 and the outer overflow launder 2.
In the present invention, the inner overflow chute 3 and the outer overflow chute 2 may be independently arranged or connected to each other, as a preferred embodiment of the present invention, referring to fig. 2, the inner overflow chute 3 and the outer overflow chute 2 are connected through a partition plate 10, the partition plate 10 is provided with a balance hole 11, the height of the balance hole 11 is higher than the height of the inner overflow port 31 and the height of the outer overflow port 21, the balance hole 11 can balance the pressure between the inner overflow chute 3 and the outer overflow chute 2, and it is ensured that the reaction solution can smoothly overflow from the inner overflow port 31 and the outer overflow port 21.
In the invention, the temperature in the reaction kettle 1 can be adjusted by introducing steam into the reaction kettle 1, so that the reaction temperature of the reaction liquid flowing down from the outer wall of the transparent pipe 5 and the reaction liquid flowing down from the inner wall of the reaction kettle 1 can be controlled, the transparent pipe 5 and/or the reaction kettle 1 can be set into a jacket structure, and the reaction temperature can be adjusted by the flow and the temperature of a refrigerant in the jacket structure. As a preferred embodiment of the present invention, the transparent tube 5 and the reaction kettle 1 are respectively of a double-layer jacket structure, the double-layer jacket structure is respectively provided with a refrigerant inlet and a refrigerant outlet, and each refrigerant inlet and each refrigerant outlet are respectively connected with the reflux condenser 9. At this moment, every refrigerant import and reflux condenser 9's exit linkage, every refrigerant export and reflux condenser 9's access connection, reflux condenser 9 is used for adjusting the temperature of refrigerant, and then the coolant that flows through in the jacket structure of hyaline tube 5 can adjust the reaction liquid temperature that the 5 outer walls of hyaline tube flowed down, the reaction liquid temperature that 1 inner wall of reation kettle flowed down can be adjusted to the coolant that flows through in reation kettle 1's the jacket structure, thereby make reaction temperature adjust more accurately, be favorable to improving reaction efficiency. More preferably, referring to fig. 1, the diameter of the double-layer jacket structure of the reaction kettle 1 is gradually reduced from top to bottom, and the included angle between the extending direction from top to bottom and the vertical direction is 0-30 °, so that the reaction liquid overflowing from the overflow tank 2 to the inner wall of the reaction kettle 1 can be promoted to flow down to form a film, and the film is collected or flowed from the bottom of the reaction kettle 1 and then enters the next process.
Preferably, the inner cavity of the reaction kettle 1 is further provided with a gas distributor 12 for introducing protective gas into the reaction kettle 1, and correspondingly, the side wall of the reaction kettle 1 is provided with a gas outlet. More preferably, the gas distributor 12 is disposed near the bottom of the reaction vessel 1, so that the introduced gas is exhausted from the reaction vessel 1 during the rising process, thereby avoiding the influence of the air on the reaction process in the reaction apparatus and improving the conversion rate. Specifically, the gas distributor 12 may be purged with nitrogen, argon, or other inert gas.
As a preferred embodiment of the invention, the liquid conveying mechanism comprises a collecting tank 6 and a transfer tank 7 which are positioned in the reaction kettle 1, the collecting tank 6 is positioned below the transparent pipe 5, the bottom of the collecting tank 6 is connected with the transfer tank 7, the bottom of the transfer tank 7 is connected with the overflow tank 2 through a liquid conveying pipeline, and a liquid pump 8 is arranged on the liquid conveying pipeline between the transfer tank 7 and the overflow tank 2. The reaction liquid flowing down from the outer wall of the transparent pipe 5 falls into the collecting tank 6 to be collected, and is conveyed to the transfer tank 7 from the bottom of the collecting tank 6 through the infusion pipeline, and is conveyed to the overflow tank 2 through the bottom of the transfer tank 7 through the infusion pipeline. Specifically, the diameter of collecting vat 6 is greater than hyaline tube 5 to can collect all reaction liquid that hyaline tube 5 outer wall flows down, also can set up the bottom of hyaline tube 5 into the structure that the diameter reduces gradually, more do benefit to the reaction liquid and fall into in the collecting vat 6.
In a relatively optimized embodiment of the invention, the photochemical reaction device comprises a reaction kettle 1, a transparent tube 5 positioned inside the reaction kettle 1, a light source 4 positioned inside the transparent tube 5 and a liquid conveying mechanism, wherein an inner overflow groove 3 and an outer overflow groove 2 are arranged in an inner cavity of the reaction kettle 1, a feed inlet 32 and an inner overflow port 31 facing the outer wall of the transparent tube 5 are arranged on the inner overflow groove 3, and an inner guide plate 33 hinged with the inner overflow groove 3 is arranged at the inner overflow port 31, so that a reaction liquid in the inner overflow groove 3 can overflow from the inner overflow port 31 and is guided to the transparent tube 5 by the inner guide plate 33 and then flows down along the outer wall of the transparent tube 5; an outer overflow port 21 facing the inner wall of the reaction kettle 1 is arranged on the outer overflow groove 2, an outer guide plate 22 hinged with the outer overflow groove 2 is arranged at the position of the outer overflow port 21, so that reaction liquid in the outer overflow groove 2 can overflow from the outer overflow port 21 and is guided to the reaction kettle 1 by the outer guide plate 22 to flow down along the inner wall of the reaction kettle 1, the distance from the inner overflow port 31 to the outer wall of the transparent pipe 5 is 2cm, the distance from the outer overflow port 21 to the inner wall of the reaction kettle 1 is 2cm, the length of the inner guide plate 33 extending towards the transparent pipe 5 is 2cm, the length of the outer guide plate 22 extending towards the reaction kettle 1 is 2cm, the distance from the inner overflow port 31 to the bottom of the inner overflow groove 3 is 15cm, and the distance from the outer overflow port 21 to the bottom of the outer overflow groove 2 is 15 cm; the inner overflow groove 3 is connected with the outer overflow groove 2 through a partition plate 10, a balance hole 11 is arranged on the partition plate 10, and the height of the balance hole 11 is higher than that of the inner overflow port 31 and the outer overflow port 21; the transparent tube 5 is a double-layer quartz glass tube, the reaction kettle 1 is of a double-layer jacket structure, the double-layer quartz glass tube and the double-layer jacket structure are respectively provided with a refrigerant inlet and a refrigerant outlet, and each refrigerant inlet and each refrigerant outlet are respectively connected with the reflux condenser 9; 1 inner chamber of reation kettle still is provided with gas distributor 12 and gas outlet, reation kettle 1's double-deck jacket structure top is 15 with the contained angle of vertical orientation to the extending direction of bottom, liquid conveying mechanism is including being located reation kettle 1 collecting vat 6 and transfer jar 7, collecting vat 6 is located the below of hyaline tube 5, the bottom and the transfer jar 7 of collecting vat 6, the bottom and the outer overflow launder 2 of transfer jar 7 are respectively through the transfusion tube coupling, be provided with liquid pump 8 on the transfer line between transfer jar 7 and the outer overflow launder 2.
The photochemical reaction device provided by the embodiment has the following use process and reaction principle: opening a gas distributor 12 to introduce nitrogen into the reaction kettle 1, and opening a reflux condenser 9 to introduce refrigerants into the double-layer quartz glass tube and the double-layer jacket structure of the reaction kettle 1; turning on a light source 4 and a liquid pump 8, inputting a reaction liquid containing 7-dehydrocholesterol into an inner overflow groove 3 from a feed inlet 32, leading the reaction liquid in the inner overflow groove 3 to overflow from an inner overflow port 31 along with the rise of the liquid level of the inner overflow groove 3 to the position of the inner overflow port 31, leading the reaction liquid to flow down along the outer wall of a transparent pipe 5 from an inner guide plate 33 to the transparent pipe 5 to form a liquid film, collecting the reaction liquid flowing down along the outer wall of the transparent pipe 5 by a collecting tank 6, conveying the reaction liquid to a transfer tank 7 by a conveying pipeline, conveying the reaction liquid into an outer overflow groove 2 by the conveying pipeline, leading the reaction liquid in the outer overflow groove 2 to flow down along the inner wall of a reaction kettle 1 to form a liquid film again along with the rise of the liquid level of the outer overflow groove 2 to the position of the outer overflow port 21; at this time, the light of the light source 4 can sequentially pass through the liquid film on the outer wall of the transparent tube 5 and the liquid film on the inner wall of the reaction kettle 1, so that the reaction liquid performs a first-stage illumination reaction on the outer wall of the transparent tube 5, and absorbs the ultraviolet light with the wavelength of 280-310nm and part of the wavelengthUltraviolet light of 250nm to produce pre-vitamin D3And byproduct tachysterol, wherein most of light transmitted from the liquid film on the outer wall of the transparent tube 5 irradiates the liquid film on the inner wall of the reaction kettle 1, and is ultraviolet light with the wavelength of about 350nm, so that reaction liquid obtained by the primary illumination reaction is subjected to secondary illumination reaction on the inner wall of the reaction kettle 1, and tachysterol in the reaction liquid is converted into pre-vitamin D3Then the reaction liquid flowing down from the inner wall of the reaction kettle 1 flows out from the bottom of the reaction kettle 1 and enters the next working procedure.
Through the technical scheme, the photochemical reaction device provided by the invention utilizes the inner overflow groove 3 and the inner overflow port 31 facing the outer wall of the transparent pipe 5, so that the reaction liquid entering the inner overflow groove 3 from the feed inlet 32 can overflow from the inner overflow port 31 and flow down along the outer wall of the transparent pipe 5 to form a liquid film, the reaction liquid flowing down from the outer wall of the transparent pipe 5 is collected and conveyed into the outer overflow groove 2 through the reaction liquid conveying mechanism, then overflows from the outer overflow port 21 and flows down along the inner wall of the reaction kettle 1 to form the liquid film again, at the moment, the light of the light source 4 can sequentially penetrate through the liquid film on the outer wall of the transparent pipe 5 and the liquid film on the inner wall of the reaction kettle 1, so that the reaction liquid can carry out primary reaction on the outer wall of the transparent pipe 5, and then carry out secondary illumination reaction on the inner wall of the reaction kettle 1, and the generation of vitamin D generated by the photochemical reaction is effectively improved3The yield and purity of the photocatalyst are improved, and the photocatalytic efficiency is improved.
The preferred embodiments of the present invention have been described in detail above with reference to the accompanying drawings, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, numerous simple modifications can be made to the technical solution of the invention, including combinations of the specific features in any suitable way, and the invention will not be further described in relation to the various possible combinations in order to avoid unnecessary repetition. Such simple modifications and combinations should be considered within the scope of the present disclosure as well.
Claims (10)
1. A photochemical reaction device is characterized by comprising a reaction kettle (1), a transparent tube (5) positioned in the reaction kettle (1), a light source (4) positioned in the transparent tube (5) and a liquid conveying mechanism, wherein an inner overflow groove (3) and an outer overflow groove (2) are arranged in an inner cavity of the reaction kettle (1), and a feed inlet (32) is formed in the inner overflow groove (3);
the inner overflow groove (3) is also provided with an inner overflow port (31) facing the outer wall of the transparent pipe (5), so that the reaction liquid in the inner overflow groove (3) can overflow from the inner overflow port (31) and flow down along the outer wall of the transparent pipe (5), the outer overflow groove (2) is provided with an outer overflow port (21) facing the inner wall of the reaction kettle (1), so that the reaction liquid in the outer overflow groove (2) can overflow from the outer overflow port (21) and flow down along the inner wall of the reaction kettle (1), and the reaction liquid conveying mechanism can collect the reaction liquid flowing down from the outer wall of the transparent pipe (5) and convey the reaction liquid into the outer overflow groove (2);
so that the reaction liquid can enter the inner overflow groove (3) from the feed port (32), a liquid film is formed on the outer wall of the transparent pipe (5) and is irradiated by the light of the light source (4) to carry out primary illumination reaction, then the reaction liquid is conveyed into the outer overflow groove (2) by the reaction liquid conveying mechanism, and finally a liquid film is formed on the inner wall of the reaction kettle (1) and is irradiated by the light penetrating from the liquid film on the outer wall of the transparent pipe (5) to carry out secondary illumination reaction.
2. The photochemical reaction device according to claim 1, characterized in that the inner overflow groove (3) is provided with an inner guide plate (33) facing the transparent pipe (5) at the inner overflow port (31), the inner guide plate (33) can guide the reaction liquid overflowing from the inner overflow port (31) to the outer wall of the transparent pipe (5), the outer overflow groove (2) is provided with an outer guide plate (22) facing the reaction kettle (1) at the outer overflow port (21), and the outer guide plate (22) can guide the reaction liquid overflowing from the outer overflow port (21) to the inner wall of the reaction kettle (1).
3. Photochemical reaction device according to claim 2, characterized in that the inner flow deflector (33) is hinged to the inner overflow launder (3) and the outer flow deflector (22) is hinged to the outer overflow launder (2).
4. Photochemical reaction device according to claim 2, characterized in that the inner flow guide plate (33) extends towards the transparent tube (5) for a length matching the distance from the inner overflow opening (31) to the outer wall of the transparent tube (5), and the outer flow guide plate (22) extends towards the reaction vessel (1) for a length matching the distance from the outer overflow opening (21) to the inner wall of the reaction vessel (1).
5. Photochemical reaction device according to claim 4, characterized in that the distance from the inner overflow opening (31) to the outer wall of the transparent tube (5) is 1-5cm and the distance from the outer overflow opening (21) to the inner wall of the reaction vessel (1) is 1-5 cm.
6. The photochemical reaction device according to any one of claims 1 to 5, characterized in that the distance between the inner overflow port (31) and the bottom of the inner overflow launder (3) is 3-20cm, and the distance between the outer overflow port (21) and the bottom of the outer overflow launder (2) is 3-20 cm.
7. The photochemical reaction device according to any one of claims 1 to 5, characterized in that the inner overflow launder (3) and the outer overflow launder (2) are connected by a partition (10), and a balance hole (11) is provided on the partition (10), and the height of the balance hole (11) is higher than the height of the inner overflow port (31) and the outer overflow port (21).
8. The photochemical reaction device according to any one of claims 1 to 5, characterized in that the transparent tube (5) and the reaction kettle (1) are respectively a double-layer jacket structure, the double-layer jacket structure is respectively provided with a coolant inlet and a coolant outlet, and each coolant inlet and each coolant outlet are respectively connected with a reflux condenser (9).
9. Photochemical reaction device according to any one of claims 1-5, characterized in that the reactor (1) is further provided with a gas distributor (12) for feeding protective gas into the reactor (1).
10. The photochemical reaction device according to any one of claims 1 to 5, wherein the liquid conveying mechanism comprises a collecting tank (6) and a transfer tank (7) located in the reaction kettle (1), the collecting tank (6) is located below the transparent pipe (5), the bottom of the collecting tank (6) and the transfer tank (7), the bottom of the transfer tank (7) and the overflow tank (2) are respectively connected by a liquid conveying pipeline, and a liquid pump (8) is arranged on the liquid conveying pipeline between the transfer tank (7) and the overflow tank (2).
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