A photochemical reaction device and synthesis method for synthesizing vitamin D3

Abstract

The present invention belongs to the technical field of vitamin D3 synthesis, specifically, a photochemical reaction device and synthesis method for vitamin D3 synthesis, including a reactor, a jacket, a light cylinder and a spiral tube; the reactor is provided with a water inlet at the top and a drain at the bottom; the jacket is divided into an inner filter chamber and an outer filter chamber; the inner filter chamber and the outer filter chamber are connected with a liquid injection pipe at the top; a high-pressure mercury lamp is provided inside the light cylinder; the spiral tube is connected with a feed pipe at the top and a discharge pipe at the bottom. The spiral tube is used to transport the reaction raw materials, so that the raw materials can be exposed to light to the greatest extent and undergo a synthesis reaction, which not only realizes continuous and uninterrupted production, but also can take into account the output of vitamin D3 to the greatest extent, meet large-scale industrialization needs, and the spiral tube is completely immersed in cooling water, so that the cooling water directly exchanges heat with the high-temperature material through the spiral tube wall from all directions, thereby improving the cooling efficiency of the raw materials.

Description

Technical Field

[0001] The invention belongs to the technical field of vitamin D3 synthesis, and specifically relates to a photochemical reaction device and a synthesis method for vitamin D3 synthesis. Background Art

[0002] Vitamin D3, also known as cholecalciferol, is a member of the vitamin D family and a very important nutrient for the human body. It can promote the absorption and utilization of calcium and phosphorus, immune regulation, nerve and muscle function, cell differentiation and proliferation, etc. Industrial production of vitamin D3 is usually carried out through two main methods: chemical synthesis or microbial fermentation. Among them, the photochemical reaction synthesis method uses appropriate light to irradiate 7-DHC to convert it into pre-vitamin D3 in a chemical reaction. This method synthesizes vitamin D3 by simulating human skin exposed to sunlight, so it is more natural, efficient, and environmentally friendly, and the product is relatively pure without producing a large number of by-products or harmful substances.

[0003] A Chinese patent application CN101085755B discloses a photochemical reaction device and a method for synthesizing previtamin D3. The technical solution includes a container, an inner tube, a mercury lamp, inner and outer jackets, and a collection bottle. The mercury lamp is arranged inside the inner tube, the outer jacket is arranged outside the inner tube, the inner jacket is arranged between the inner tube lamp and the outer jacket, and the illumination liquid outlet of the container receives the collection bottle. Prepare 7-dehydrocholesterol solution and dissolve it in ethanol; evacuate and pass nitrogen; pass an aqueous solution prepared with sodium tungstate or lead acetate as a filter liquid into the outer jacket, and pass an aqueous solution prepared with cobalt sulfate, nickel sulfate, sulfuric acid and water as a filter liquid into the inner jacket, circulate through the condenser, feed 7-dehydrocholesterol solution from the feed port, and perform photochemical reaction; pass nitrogen from the feed port to mix the 7-dehydrocholesterol solution entering the photochemical reaction device, and the solution after the photochemical reaction flows into the collection bottle.

[0004] A Chinese patent application CN103553993B discloses a method for synthesizing resinous vitamin D3 using microfluidic photoreaction technology and a microfluidic photochemical reactor. The key points of its technical solution are: light irradiation reaction is carried out in a microfluidic photochemical reactor and under the protection of nitrogen (preferably high-purity nitrogen). During the reaction, the temperature of the photochemical reaction liquid is controlled below 28°C, and a peristaltic pump is used to regulate the flow rate of the photochemical reaction liquid in the microfluidic tube; after the light irradiation reaction, the conversion rate of 7-dehydrocholesterol reaches 90.5% to 95%, and the HPLC yield of pre-vitamin D3 is increased to 70 to 73.1%. Resinous vitamin D3 is prepared by thermal isomerization reaction, wherein the HPLC yield of resinous vitamin D3 is 68% to 71.1%. The entire preparation process is simple and easy to operate, which is conducive to large-scale production.

[0005] However, the above-mentioned technologies often have the following defects: the existing vitamin D3 photochemical reaction devices all have many drawbacks. For example, the technology disclosed in CN101085755 adds raw materials into a container, and then discharges the products after photochemical reaction. It can only produce a certain amount of products at a time and cannot achieve continuous production. In addition, the uniformity of light irradiation on the raw materials is low, and the synthesis efficiency is low. For example, the technology disclosed in CN103553993B introduces materials into a spiral microfluidic tube. Although it can achieve continuous production and improve uniformity, its structure, volume, and flow rate are limited, making it difficult to continuously produce large quantities of pre-vitamin D3, which is particularly insufficient when facing large-scale production needs.

[0006] To this end, the present invention provides a photochemical reaction device and a synthesis method for synthesizing vitamin D3. Summary of the invention

[0007] In order to make up for the deficiencies of the prior art, at least one technical problem raised in the background technology is solved.

[0008] The technical solution adopted by the present invention to solve the technical problem is: a photochemical reaction device for synthesizing vitamin D3 described in the present invention comprises a reaction kettle, a jacket, a light cylinder and a spiral tube; the jacket, the light cylinder and the spiral tube are all made of transparent materials;

[0009] The top of the reactor is provided with a water inlet, and the bottom of the reactor is provided with a drain outlet;

[0010] The jacket is fixedly connected to the interior of the reactor; the interior of the jacket is divided into an inner filter chamber and an outer filter chamber from the inside to the outside; the tops of the inner filter chamber and the outer filter chamber are respectively connected with injection pipes;

[0011] The light tube is fixedly connected to the inside of the jacket; a high-pressure mercury lamp is arranged inside the light tube;

[0012] The spiral tube is coiled on the outside of the jacket; the top of the spiral tube is connected with a feed pipe, and the bottom of the spiral tube is connected with a discharge pipe.

[0013] Preferably, the bottom of the spiral tube is connected to an air inlet pipe, and the top of the spiral tube is connected to an air outlet pipe.

[0014] Preferably, the air inlet pipe is tangent to the bottom of the spiral tube; an air duct is connected between the feed pipe and the top of the spiral tube, and the air duct is bent upward; and the air outlet pipe is connected to the middle of the air duct.

[0015] Preferably, the inner wall surface of the reactor is coated with reflective material.

[0016] Preferably, a servo motor is fixedly connected to the lower side of the reactor; the output end of the servo motor is connected to a rotating shaft; the rotating shaft extends to the bottom of the reactor and is provided with a turntable; a group of stirring blades are evenly distributed on the circumference of the turntable surface.

[0017] Preferably, the turntable is sleeved on the outside of the rotating shaft and is slidably connected thereto; a group of limit strips are evenly distributed on the surface of the rotating shaft; a limit groove that slidably cooperates with the limit strip is provided on the inner side of the turntable; a pressure plate is fixedly connected to the surface of the rotating shaft at a position above the turntable; a spring is fixedly connected between the pressure plate and the turntable; a support ring is fixedly connected to the bottom of the reactor at a position below the turntable, and the rotating shaft passes through the support ring; a group of rollers are evenly distributed on the lower side of the turntable; the upper side of the support ring is designed to be corrugated.

[0018] Preferably, the upper end of the rotating shaft extends to the inside of the jacket and is rotatably sealed therewith; two groups of levers are evenly distributed on the surface of the rotating shaft, and the two groups of levers are respectively located inside the inner filter chamber and the outer filter chamber.

[0019] Preferably, a group of connecting ropes are evenly distributed inside the spiral tube; the upper end of the connecting rope is fixedly connected to the inner wall of the spiral tube, and the lower end of the connecting rope is fixedly connected to a magnetic block; a group of guide plates are fixedly connected to the surface of the magnetic block; the magnetic block and the lever attract each other when they are close to each other.

[0020] A method for photochemical synthesis of vitamin D3, which uses the above-mentioned photochemical reaction device for synthesizing vitamin D3, comprises the following steps:

[0021] S1: Prepare chemical filter liquid and reaction raw materials, inject cooling water into the reactor through the water inlet, and inject chemical filter liquid into the inner filter chamber and the outer filter chamber through the injection pipe;

[0022] S2: Turn on the high-pressure mercury lamp inside the light tube. When the high-pressure mercury lamp reaches the rated power, use a peristaltic pump to inject the reaction raw materials into the spiral tube through the feed pipe at a constant speed. The raw materials flow in a spiral from top to bottom inside the spiral tube;

[0023] S3: using two layers of chemical filter liquid to absorb and filter wavelengths that are not conducive to the generation of pre-vitamin D3, and using cooling water inside the reactor to cool the spiral tube and the jacket;

[0024] S4: nitrogen is introduced into the bottom of the spiral tube through the air inlet pipe to protect the raw materials with nitrogen, and the bubbles formed spiral up along the spiral tube, in the opposite direction of the flow direction of the raw materials, stirring and disturbing the raw materials;

[0025] S5: Part of the light emitted by the high-pressure mercury lamp shines on the surface of the spiral tube, and the other part is scattered to the surroundings through the gaps between the spiral tubes, and after being reflected by the inner wall of the reactor, it shines on the surface of the spiral tube again.

[0026] The beneficial effects of the present invention are as follows:

[0027] 1. The photochemical reaction device and synthesis method for synthesizing vitamin D3 described in the present invention utilize a spiral helical tube to transport the reaction raw materials, so that the raw materials can be exposed to light to the greatest extent and undergo a synthesis reaction, thereby achieving continuous and uninterrupted production and improving the uniformity of mercury lamp irradiation on the raw materials, while also taking into account the output of vitamin D3 to the greatest extent and meeting large-scale industrial needs. The spiral tube is completely immersed in cooling water, allowing the cooling water to directly exchange heat with the high-temperature material through the spiral tube wall from all directions, thereby improving the cooling efficiency of the raw materials.

[0028] 2. The photochemical reaction device and synthesis method for synthesizing vitamin D3 described in the present invention introduce nitrogen into the bottom of the spiral tube through an air inlet pipe, and nitrogen protects the raw materials in the spiral tube, thereby reducing the generation rate of by-products. The formed nitrogen bubbles spiral up along the spiral tube under the action of buoyancy, which is exactly opposite to the flow direction of the raw materials in the spiral tube. The raw materials can be stirred and disturbed to improve the turbulent effect of the raw materials. On the one hand, the raw materials in the spiral tube are continuously exchanged and dispersed with each other to improve the uniformity of light irradiation on the raw materials, thereby improving the synthesis efficiency of pre-vitamin D3. On the other hand, the raw materials can fully dissipate heat and improve the heat exchange efficiency between the raw materials and cooling water. BRIEF DESCRIPTION OF THE DRAWINGS

[0029] The present invention will be further described below in conjunction with the accompanying drawings.

[0030] Figure 1 is a stereogram of the present invention;

[0031] Figure 2 It is a structural schematic diagram of the spiral tube in the present invention;

[0032] Figure 3 It is a structural schematic diagram of the lever in the present invention;

[0033] Figure 4 yes Figure 3 A partial enlarged view of the middle part;

[0034] Figure 5 It is a schematic diagram of the structure of the support ring in the present invention;

[0035] Figure 6 is a cross-sectional view of the present invention;

[0036] Figure 7 yes Figure 6 A partial enlarged view of point B in the middle;

[0037] Figure 8 It is a schematic flow chart of the method of the present invention.

[0038] In the figure: reactor 1, jacket 2, light cylinder 3, spiral tube 4, water inlet 5, drain outlet 6, inner filter chamber 7, outer filter chamber 8, injection tube 9, high-pressure mercury lamp 10, feed pipe 11, discharge pipe 12, air inlet pipe 13, air outlet pipe 14, air duct 15, servo motor 16, rotating shaft 17, turntable 18, stirring blade 19, limit bar 20, pressure plate 21, spring 22, support ring 23, roller 24, lever 25, connecting rope 26, magnetic block 27, guide plate 28. DETAILED DESCRIPTION

[0039] In order to make the technical means, creative features, objectives and effects achieved by the present invention easy to understand, the present invention is further explained below in conjunction with specific implementation methods.

[0040] like Figures 1 to 7 As shown, a photochemical reaction device for synthesizing vitamin D3 according to the present invention comprises a reaction vessel 1, a jacket 2, a light cylinder 3 and a spiral tube 4; the jacket 2, the light cylinder 3 and the spiral tube 4 are all made of transparent materials, such as quartz or glass;

[0041] The top of the reactor 1 is provided with a water inlet 5, and the bottom of the reactor 1 is provided with a drain outlet 6;

[0042] The jacket 2 is fixedly connected to the inside of the reactor 1; the inside of the jacket 2 is divided into an inner filter chamber 7 and an outer filter chamber 8 from the inside to the outside; the tops of the inner filter chamber 7 and the outer filter chamber 8 are respectively connected to injection pipes 9;

[0043] The light tube 3 is fixedly connected to the inside of the jacket 2; a high-pressure mercury lamp 10 is arranged inside the light tube 3;

[0044] The spiral tube 4 is coiled on the outside of the jacket 2 ; the top of the spiral tube 4 is connected to a feed pipe 11 , and the bottom of the spiral tube 4 is connected to a discharge pipe 12 .

[0045] The vitamin D3 photochemical reaction devices in the prior art all have many disadvantages. For example, in the technology disclosed in CN101085755, raw materials are added into a container, and the products are discharged after the photochemical reaction. It can only produce a certain amount of products at a time and cannot achieve continuous production. In addition, the uniformity of light irradiation on the raw materials is low, and the synthesis efficiency is low. For example, in the technology disclosed in CN103553993B, the materials are introduced into a spiral microfluidic tube. Although it can achieve continuous production and improve uniformity, its structure, volume, and flow rate are limited, making it difficult to continuously produce large quantities of pre-vitamin D3, which is particularly insufficient when facing large-scale production needs.

[0046] When the present invention is in use, first, cooling water is injected into the reactor 1 through the water inlet 5, and chemical filter liquid is injected into the inner filter chamber 7 and the outer filter chamber 8 respectively through the injection tube 9, and the high-pressure mercury lamp 10 inside the light tube 3 is turned on. Then, the reaction raw materials are injected into the spiral tube 4 through the feed tube 11 by a peristaltic pump. The raw materials flow in a spiral from top to bottom inside the spiral tube 4 and can be fully irradiated by the high-pressure mercury lamp 10, thereby improving the reaction degree of photochemical synthesis. Two layers of chemical filter liquid are used to absorb and filter wavelengths that are not conducive to the generation of pre-vitamin D3, thereby improving the yield of pre-vitamin D3. The final product is discharged and collected through the discharge pipe 12, and subsequent detection and purification work is carried out.

[0047] Among them, the chemical filter liquid in the inner filter chamber 7 can be prepared from sodium tungstate and lead acetate, etc., and the chemical filter liquid in the inner filter chamber 7 can be prepared from cobalt sulfate and nickel sulfate, etc.; the reaction raw material can be 7-dehydrocholesterol (7-DHC) dissolved in 95% ethanol, heated to 36°C and dissolved to transparency.

[0048] The present invention utilizes the spiral spiral tube 4 to transport the reaction raw materials, so that the raw materials can be exposed to light to the greatest extent and undergo a synthesis reaction, thereby achieving continuous and uninterrupted production and improving the uniformity of the mercury lamp irradiating the raw materials, while also taking into account the output of pre-vitamin D3 to the greatest extent and meeting large-scale industrial needs. The spiral tube 4 is completely immersed in cooling water, allowing the cooling water to directly exchange heat with the high-temperature material through the wall of the spiral tube 4 from all directions, thereby improving the cooling efficiency of the raw materials.

[0049] In order to further improve the cooling effect, the cooling water inside the reactor 1 can also be circulated, that is, a pump is used to allow the cooling water to continuously flow in from one port and then out from another port, continuously taking away the heat in the form of running water, thereby achieving efficient heat dissipation.

[0050] As a preferred embodiment of the present invention, the bottom of the spiral tube 4 is connected to an air inlet pipe 13, and the top of the spiral tube 4 is connected to an air outlet pipe 14; nitrogen is introduced into the bottom of the spiral tube 4 through the air inlet pipe 13, and the raw materials in the spiral tube 4 are protected by nitrogen, thereby reducing the generation rate of by-products, and the formed nitrogen bubbles spiral up along the spiral tube 4 under the action of buoyancy, which is exactly opposite to the flow direction of the raw materials in the spiral tube 4, and can stir and interfere with the raw materials to improve the turbulent effect of the raw materials. On the one hand, the raw materials in the spiral tube 4 are continuously exchanged and dispersed with each other to improve the uniformity of light irradiation on the raw materials, thereby improving the synthesis efficiency of pre-vitamin D3, and on the other hand, the raw materials can fully dissipate heat and improve the heat exchange efficiency between the raw materials and cooling water.

[0051] The air inlet pipe 13 is tangent to the bottom of the spiral tube 4; an air duct 15 is connected between the feed pipe 11 and the top of the spiral tube 4, and the air duct 15 is bent upward; the air outlet pipe 14 is connected to the middle of the air duct 15; since the air inlet pipe 13 is tangent to the spiral tube 4, the nitrogen can directly collide with the flowing raw material when it is introduced into the spiral tube 4 through the air inlet pipe 13, further improving the disturbance effect on the raw material. After passing through the inside of the spiral tube 4, the nitrogen reaches the air duct 15. Under the action of the bent air duct 15, the bubbles float upward and are discharged outward through the air outlet pipe 14.

[0052] As a preferred embodiment of the present invention, the inner wall surface of the reactor 1 is coated with a reflective material; part of the light emitted by the high-pressure mercury lamp 10 is irradiated on the surface of the spiral tube 4, and the other part is scattered to the surroundings through the gaps between the spiral tubes 4, resulting in a waste of light. By coating the reflective material, the light emitted through the gaps between the spiral tubes 4 can be reflected by the inner wall of the reactor 1 and re-irradiated on the surface of the spiral tube 4, thereby improving the utilization rate of the light and allowing both the inner and outer sides of the spiral tube 4 to be illuminated, further improving the degree of reaction.

[0053] As a preferred embodiment of the present invention, a servo motor 16 is fixedly connected to the lower side of the reactor 1; the output end of the servo motor 16 is connected to a rotating shaft 17; the rotating shaft 17 extends to the bottom of the reactor 1 and is provided with a turntable 18; a group of stirring blades 19 are evenly distributed on the circumference of the surface of the turntable 18; during the reaction process, the servo motor 16 is used to drive the rotating shaft 17 to rotate, and then the rotating shaft 17 drives the turntable 18 and multiple stirring blades 19 to rotate, and the stirring blades 19 are used to stir the cooling water inside the reactor 1, thereby improving the heat absorption efficiency of the cooling water to the spiral tube 4 and the jacket 2.

[0054] The turntable 18 is sleeved on the outside of the rotating shaft 17 and slidably connected thereto; a group of limit strips 20 are evenly distributed on the surface of the rotating shaft 17; a limit groove that slidably cooperates with the limit strip 20 is arranged on the inner side of the turntable 18; a pressure plate 21 is fixedly connected to the surface of the rotating shaft 17 at a position above the turntable 18; a spring 22 is fixedly connected between the pressure plate 21 and the turntable 18; a support ring 23 is fixedly connected to the bottom of the reactor 1 at a position below the turntable 18, and the rotating shaft 17 passes through the support ring 23; a group of rollers 24 are evenly distributed on the lower side of the turntable 18; the upper side of the support ring 23 is designed to be corrugated; as the rotating shaft 17 drives the turntable 18 to rotate, the rollers 24 on the lower side of the turntable 18 can roll on the wavy surface on the upper side of the support ring 23 and cooperate with the spring 22 to promote the turntable 18 to continuously reciprocate up and down, and use the stirring blade 19 to continuously push up the cooling water at the bottom of the reactor 1, so that the cooling water at the top and bottom of the reactor 1 can be exchanged, thereby enhancing the convection effect of heat, making the heat distribution of the cooling water at each position uniform, and improving its cooling efficiency for the spiral tube 4 and the jacket 2. In addition, in the process of the raw material flowing downward inside the spiral tube 4, as the reaction degree and the reaction process gradually accumulate, the temperature at the bottom of the spiral tube 4 will be higher than that at the top. Therefore, the cooling water surging upward at this time can flow on both sides of the spiral tube 4 and the outer surface of the jacket 2, and fully take away its heat upward, so that the heat at the bottom of the spiral tube 4 is balanced upward, further preventing overheating.

[0055] The upper end of the rotating shaft 17 extends to the inside of the jacket 2 and is rotatably sealed therewith; two groups of levers 25 are evenly distributed on the surface of the rotating shaft 17, and the two groups of levers 25 are respectively located inside the inner filter chamber 7 and the outer filter chamber 8; when the rotating shaft 17 rotates, it can drive the two groups of levers 25 to rotate synchronously, and then the two groups of levers 25 respectively stir the chemical filter liquid inside the inner filter chamber 7 and the outer filter chamber 8, so as to promote the uniform dispersion of the filter liquid at each position, prevent the deposition of components, improve the filtering uniformity of light, and promote the filter liquid to fully exchange heat with cooling water.

[0056] As a preferred embodiment of the present invention, a group of connecting ropes 26 are evenly distributed inside the spiral tube 4; the upper end of the connecting rope 26 is fixedly connected to the inner wall of the spiral tube 4, and the lower end of the connecting rope 26 is fixedly connected to a magnetic block 27; a group of guide pieces 28 are fixedly connected to the surface of the magnetic block 27; the magnetic block 27 and the lever 25 attract each other when they are close to each other; during the rotation of the lever 25, when the lever 25 rotates to a position close to the magnetic block 27, it can attract it and cause the magnetic block 27 to swing to one side, and when the lever 25 is away from the magnetic block 27, the magnetic block 27 swings back to the other side, so that the magnetic block 27 keeps swinging left and right inside the spiral tube 4, and the guide pieces 28 are used to disturb the raw materials inside the spiral tube 4, on the one hand, to promote the exchange and mixing of the raw material fluid in the radial direction, so as to improve the uniformity of illumination and the heat exchange efficiency, on the other hand, during the swinging process of the guide pieces 28, the nitrogen bubbles can be dispersed and broken, so as to reduce the size of the bubbles and increase the action area and effect of the bubbles on the raw materials.

[0057] In order to prevent the guide plate 28 from blocking the light, the guide plate 28 is preferably made of a transparent material, such as quartz, glass or high-temperature resistant plastic, so as to reduce the influence of the guide plate 28 on the raw material.

[0058] like Figure 8 As shown, a method for photochemical synthesis of vitamin D3, which uses the above-mentioned photochemical reaction device for synthesizing vitamin D3, comprises the following steps:

[0059] S1: Prepare chemical filter liquid and reaction raw materials, inject cooling water into the reactor 1 through the water inlet 5, and inject the chemical filter liquid into the inner filter chamber 7 and the outer filter chamber 8 through the injection pipe 9;

[0060] S2: Turn on the high-pressure mercury lamp 10 inside the light tube 3. When the high-pressure mercury lamp 10 reaches the rated power, use a peristaltic pump to inject the reaction raw materials into the spiral tube 4 through the feed pipe 11 at a constant speed, and the raw materials spirally flow from top to bottom inside the spiral tube 4;

[0061] S3: using two layers of chemical filter liquid to absorb and filter wavelengths that are not conducive to the generation of pre-vitamin D3, and using cooling water inside the reactor 1 to cool the spiral tube 4 and the jacket 2;

[0062] S4: nitrogen is introduced into the bottom of the spiral tube 4 through the air inlet pipe 13 to protect the raw material with nitrogen, and the bubbles formed spiral up along the spiral tube 4, in the opposite direction of the flow direction of the raw material, stirring and disturbing the raw material;

[0063] S5: A part of the light emitted by the high pressure mercury lamp 10 irradiates the surface of the spiral tube 4, and the other part is scattered to the surroundings through the gaps between the spiral tubes 4, and after being reflected by the inner wall of the reactor 1, it irradiates the surface of the spiral tube 4 again.

[0064] The above-mentioned front, back, left, right, top and bottom are all based on the figures in the specification. Figure 1 As a benchmark, according to the person's observation perspective, the side of the device facing the observer is defined as the front, the left side of the observer is defined as the left, and so on.

[0065] In the description of the present invention, it should be understood that the terms "center", "longitudinal", "lateral", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside" and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be understood as limiting the scope of protection of the present invention.

[0066] The above shows and describes the basic principles, main features and advantages of the present invention. It should be understood by those skilled in the art that the present invention is not limited to the above embodiments. The above embodiments and descriptions are only for explaining the principles of the present invention. Without departing from the spirit and scope of the present invention, the present invention may have various changes and improvements, which fall within the scope of the present invention. The scope of protection of the present invention is defined by the attached claims and their equivalents.

Claims

1. A photochemical reaction device for synthesizing vitamin D3, characterized in that: It comprises a reaction kettle (1), a jacket (2), a light cylinder (3) and a spiral tube (4); the jacket (2), the light cylinder (3) and the spiral tube (4) are all made of transparent materials; The top of the reactor (1) is provided with a water inlet (5), and the bottom of the reactor (1) is provided with a drain outlet (6); The jacket (2) is fixedly connected to the interior of the reaction kettle (1); the interior of the jacket (2) is divided into an inner filter chamber (7) and an outer filter chamber (8) from the inside to the outside; the tops of the inner filter chamber (7) and the outer filter chamber (8) are respectively connected to injection pipes (9); The light cylinder (3) is fixedly connected to the interior of the jacket (2); a high-pressure mercury lamp (10) is arranged inside the light cylinder (3); The spiral tube (4) is coiled on the outside of the jacket (2); the top of the spiral tube (4) is connected to a feed tube (11), and the bottom of the spiral tube (4) is connected to a discharge tube (12); A servo motor (16) is fixedly connected to the lower side of the reactor (1); an output end of the servo motor (16) is connected to a rotating shaft (17); the rotating shaft (17) extends to the bottom of the reactor (1) and is provided with a rotating disk (18); a group of stirring blades (19) are evenly distributed on the circumference of the surface of the rotating disk (18); The upper end of the rotating shaft (17) extends into the interior of the jacket (2) and is rotatably sealed therewith; two groups of levers (25) are evenly distributed on the surface of the rotating shaft (17), and the two groups of levers (25) are respectively located inside the inner filter chamber (7) and the outer filter chamber (8); A group of connecting ropes (26) are evenly distributed inside the spiral tube (4); the upper ends of the connecting ropes (26) are fixedly connected to the inner wall of the spiral tube (4), and the lower ends of the connecting ropes (26) are fixedly connected to a magnetic block (27); a group of guide plates (28) are fixedly connected to the surface of the magnetic block (27); and the magnetic block (27) and the lever (25) attract each other when they are close to each other.

2. A photochemical reaction device for synthesizing vitamin D3 according to claim 1, characterized in that: The bottom of the spiral tube (4) is connected to an air inlet pipe (13), and the top of the spiral tube (4) is connected to an air outlet pipe (14).

3. A photochemical reaction device for synthesizing vitamin D3 according to claim 2, characterized in that: The air inlet pipe (13) is tangent to the bottom of the spiral tube (4); an air duct (15) is connected between the feed pipe (11) and the top of the spiral tube (4), and the air duct (15) is bent upward; and the air outlet pipe (14) is connected to the middle of the air duct (15).

4. A photochemical reaction device for synthesizing vitamin D3 according to claim 3, characterized in that: The inner wall surface of the reaction kettle (1) is coated with a reflective material.

5. A photochemical reaction device for synthesizing vitamin D3 according to claim 4, characterized in that: The turntable (18) is sleeved on the outside of the rotating shaft (17) and is slidably connected thereto; a group of limit strips (20) are evenly distributed on the surface of the rotating shaft (17); a limit groove slidably matched with the limit strip (20) is provided on the inside of the turntable (18); a pressure plate (21) is fixedly connected to the surface of the rotating shaft (17) at a position above the turntable (18); a spring (22) is fixedly connected between the pressure plate (21) and the turntable (18); a support ring (23) is fixedly connected to the bottom of the reactor (1) at a position below the turntable (18), and the rotating shaft (17) passes through the support ring (23); a group of rollers (24) are evenly distributed on the lower side of the turntable (18); and the upper side of the support ring (23) is designed to be corrugated.

6. A method for photochemical synthesis of vitamin D3, the method using the photochemical reaction device for synthesizing vitamin D3 according to claim 5, characterized in that: The following steps are involved: S1: preparing a chemical filter liquid and reaction raw materials, injecting cooling water into the reaction kettle (1) through a water inlet (5), and injecting the chemical filter liquid into the inner filter chamber (7) and the outer filter chamber (8) through a liquid injection pipe (9); S2: Turn on the high-pressure mercury lamp (10) inside the light tube (3). When the high-pressure mercury lamp (10) reaches the rated power, use a peristaltic pump to inject the reaction raw materials into the spiral tube (4) through the feed pipe (11) at a constant speed. The raw materials flow in a spiral from top to bottom inside the spiral tube (4); S3: using two layers of chemical filter liquid to absorb and filter wavelengths that are not conducive to the generation of pre-vitamin D3, and using cooling water inside the reaction kettle (1) to cool the spiral tube (4) and the jacket (2).

7. A method for photochemical synthesis of vitamin D3 according to claim 6, characterized in that: The method further comprises the following steps: S4: nitrogen is introduced into the bottom of the spiral tube (4) through the air inlet pipe (13) to protect the raw material with nitrogen, and the bubbles formed spiral up along the spiral tube (4) in the opposite direction of the flow direction of the raw material, thereby stirring and disturbing the raw material; S5: A portion of the light emitted by the high-pressure mercury lamp (10) is irradiated onto the surface of the spiral tube (4), and another portion is scattered in all directions through the gaps between the spiral tubes (4), and after being reflected by the inner wall of the reaction vessel (1), is irradiated onto the surface of the spiral tube (4) again.

Images