A photoreactor for vitamin synthesis

Abstract

The utility model relates to vitamin synthetic equipment technical field, a kind of light reaction device for vitamin synthesis includes shell body, rotating cooperation is equipped with rotary drum in shell body, the outer wall of shell body is sandwich structure, cooling water pipeline is arranged in sandwich structure, the bottom of shell body is equipped with feed pipe, air inlet pipe;The lower part of rotary drum is equipped with inlet, and the upper part is equipped with overflow hole;Air inlet pipe passes through the inlet, for into gas into rotary drum;Rotary drum is equipped with ultraviolet lamp, ultraviolet lamp uses cylindrical lamp, and it is coaxially arranged in rotary drum;The bottom of shell body is equipped with lamp holder, for installing the ultraviolet lamp. Material is spirally ascending flow from bottom to top in rotary drum by centrifugal force, mass transfer speed between material is greatly promoted compared with kettle type or spiral pipe type, the uniformity of light source to raw material irradiation is enhanced, material mutual exchange is strengthened, and material and rotary drum are promoted fast heat exchange;Adopt excimer lamp or ultraviolet led lamp, structure is simplified.

Description

Technical Field

[0001] This utility model relates to the field of vitamin synthesis equipment technology, specifically to a photoreactor for vitamin synthesis. Background Technology

[0002] The industrial synthesis of vitamin D3 (cholecalciferol) mainly relies on photochemical isomerization reactions. The core of this process is to irradiate 7-dehydrocholesterol (7-DHC) with ultraviolet light of a specific wavelength to generate pre-vitamin D3, which is then thermally isomerized to obtain the target product. However, this process has stringent requirements regarding the wavelength of the light source, the uniformity of the reaction, and temperature control.

[0003] Patent CN101085755 uses a double-layer filter jacket (inner layer sodium tungstate / lead acetate, outer layer cobalt sulfate / nickel sulfate) to absorb stray wavelengths (<260 nm and >325 nm) from high-pressure mercury lamps, narrowing the effective spectrum to 260-325 nm, and enhancing mixing through nitrogen bubbling. This is a traditional batch reactor, which suffers from problems such as discontinuous reaction and poor uniformity of light intensity. Patent CN103553993B uses a microfluidic photochemical reactor, effectively solving problems such as discontinuous reaction, uneven light intensity, and mass and heat transfer; however, the equipment structure results in slow feeding, making it difficult to meet the needs of large-scale production. Regarding the light source, the above patents generally adopt a design of high-pressure mercury lamp with a filter jacket, resulting in a large light source size. Utility Model Content

[0004] The purpose of this invention is to provide a photoreaction device for vitamin synthesis that combines the characteristics of continuous reaction, uniform light intensity, and small light source size.

[0005] To achieve the above objectives, the present invention adopts the following technical solution: A photoreactor for vitamin synthesis includes an outer shell containing a rotating drum. The outer wall of the outer shell has a sandwich structure with cooling water pipes arranged in the sandwich structure. The bottom of the outer shell has a feed pipe and an air inlet pipe. The lower part of the rotating drum has a feed port and the upper part has an overflow hole. The air inlet pipe passes through the feed port and is used to introduce gas into the rotating drum. The drum is equipped with an ultraviolet lamp, which is a cylindrical lamp tube and is coaxial with the drum; the bottom of the outer casing is equipped with a lamp holder for mounting the ultraviolet lamp.

[0006] Furthermore, the inner wall of the drum is provided with spiral grooves for guiding the reaction liquid upward.

[0007] Furthermore, the cooling water pipe is spirally coiled, with an inlet pipe at one end and a return pipe at the other end, and the inlet and return pipe are located on the outside of the outer casing.

[0008] Furthermore, the upper part of the outer shell is provided with an overflow ring groove, and there are multiple overflow holes distributed along the circumference of the drum. The overflow ring groove is located around the overflow holes. The outer shell is connected to a discharge pipe, which is connected to the overflow ring groove. The discharge pipe is used to discharge the overflowed reaction liquid to the receiving tank.

[0009] Furthermore, the upper part of the drum is provided with a conical end, and each of the overflow holes is provided at the conical end.

[0010] Furthermore, a thermometer is provided on the upper part of the outer casing for detecting the temperature of the reaction liquid in the overflow ring tank.

[0011] Furthermore, the ultraviolet lamp is an excimer lamp or an ultraviolet LED lamp.

[0012] Furthermore, the bottom of the outer casing is provided with a mounting hole, and a mounting base is sealed and connected at the mounting hole. The lamp holder is located on the upper side of the mounting base. The lamp holder is provided with a wire hole and a first connecting flange hole for fixing the ultraviolet lamp. The mounting base is provided with a second connecting flange hole for connecting with the outer casing. The mounting base is also provided with a vent hole and a feed hole, and the feed hole is used to install the feed tube.

[0013] Furthermore, the outer periphery of the mounting base is provided with a sealing ring groove, and a sealing ring is installed thereon for sealing and engaging with the mounting hole.

[0014] Furthermore, the intake pipe is used to introduce nitrogen gas, and the intake pipe is provided with multiple exhaust holes for exhausting gas into the drum.

[0015] The beneficial effects of this utility model are: (1) The material flows upward from bottom to top in the drum by centrifugal force, and the mass transfer rate between materials is greatly improved compared with that of the kettle or spiral tube. The rapid mass transfer not only enhances the uniformity of the light source irradiation of the raw materials, but also strengthens the mutual exchange between materials, and promotes rapid heat exchange between the material and the drum, thereby ensuring the uniform temperature of the reaction system.

[0016] (2) By adjusting the feed rate, the residence time of the material in the drum can be controlled, thereby achieving continuous material feeding and discharging while taking into account the reaction efficiency, thus meeting the needs of large-scale industrialization.

[0017] (3) Low-temperature nitrogen is used to protect the reaction system with nitrogen. At the same time, the low-temperature nitrogen carries away the heat emitted by the light source inside the drum, thereby cooling the light source and indirectly cooling the material.

[0018] (4) The cylindrical lamp source used is an excimer lamp or ultraviolet LED lamp, which has a more accurate wavelength range and significantly reduced heat generation than traditional high-pressure mercury lamps. It eliminates the need for filter interlayer and forced heat dissipation interlayer, simplifying the structure. Attached Figure Description

[0019] Figure 1 This is a schematic diagram of the photoreactor device for vitamin synthesis according to this utility model; Figure 2 It is a 3D diagram of the rotating drum; Figure 3 This is a 3D view of the mounting base at the bottom of the outer casing.

[0020] 1. Outer casing; 11. Overflow ring groove; 2. Cooling water pipe; 21. Water inlet; 22. Water return pipe; 3. Drum; 31. Overflow hole; 32. Drive shaft; 33. First sealing ring groove; 34. Feed inlet; 4. Thermometer; 5. Ultraviolet lamp; 61. Air inlet pipe; 62. Air supply pipe; 7. Peristaltic pump; 81. Mounting base; 811. Second sealing ring groove; 812. Second connecting flange hole; 813. Feed hole; 814. Vent hole; 82. Lamp holder; 821. Slot; 822. First connecting flange hole; 823. Wiring hole. Detailed Implementation

[0021] The technical solutions of the present utility model will be clearly and completely described below with reference to the accompanying drawings of the embodiments. Obviously, the described embodiments are only some embodiments of the present utility model, and not all embodiments. All other embodiments obtained by those skilled in the art based on the embodiments of the present utility model are within the protection scope of the present utility model.

[0022] Embodiments of this utility model: like Figures 1-3 As shown, a photoreactor for vitamin synthesis includes a housing 1, within which a rotating drum 3 is rotatably fitted. The housing 1 is cylindrical, open at the top, and has a bottom for feeding or air intake. The rotating drum 3 is cylindrical, made of stainless steel for heat conduction and dissipation. A first sealing ring groove 33 is provided on the outer circumference of the drum 3, with two grooves, one at the top and one at the bottom. The first sealing ring groove 33 is used to install a sealing ring, achieving a seal with the inner wall of the housing 1. Preferably, the sealing ring has good wear resistance. In other embodiments, the drum may also adopt a cylindrical structure that is wider at the top and narrower at the bottom, i.e., the bottom is conical. The vitamin primarily refers to vitamin D3.

[0023] The outer wall of the outer casing 1 has a sandwich structure, within which cooling water pipes 2 are arranged. The cooling water pipes 2 are spirally coiled, with one end connected to an inlet 21 and the other end connected to an outlet 22. The inlet 21 and outlet 22 are located on the outside of the outer casing 1. The cooling water pipes 2 are connected to an external chiller, and through water circulation, are used to cool the outer casing 1, indirectly cooling the rotating drum.

[0024] The drum 3 has a feed inlet 34 at the bottom and an overflow hole 31 at the top. An air inlet pipe 61 passes through the feed inlet 34 and is used to introduce gas into the drum 3. The air inlet pipe 61 is used to introduce nitrogen gas. The effective section of the air inlet pipe 61 inside the drum 3 is vertically arranged and has multiple exhaust holes for venting gas into the drum 3. The nitrogen gas is cooled before being introduced and is used for nitrogen protection and auxiliary cooling inside the drum 3.

[0025] The upper part of the drum 3 is provided with a conical end, and each of the overflow holes 31 is provided at the conical end to facilitate the overflow of the reaction liquid.

[0026] The upper part of the outer casing 1 is provided with an overflow ring groove 11. Multiple overflow grooves are provided and distributed around the circumference of the drum 3. The overflow ring groove 11 is located outside the overflow hole 31. The outer casing 1 is connected to a discharge pipe, which communicates with the overflow ring groove 11. The discharge pipe is used to discharge the overflowed reaction liquid to the receiving tank. If the inlet 34 of the receiving tank is relatively low, the discharge pipe can discharge directly. If there is no height difference, the discharge pipe needs to be connected to a pump. Non-powered collection is preferred.

[0027] The inner wall of the drum 3 is provided with spiral grooves for guiding the reaction liquid upward. The upper part of the drum 3 is closed (except for the overflow hole 31), and a drive shaft 32 is connected to the upper part. The drive mechanism drives the drum 3 to rotate from the top. The specific drive mechanism is relatively mature and will not be described in detail. For example, common tubular centrifuges use a similar mechanism.

[0028] A thermometer 4 is provided on the upper part of the outer casing 1 to detect the temperature of the reaction liquid in the overflow ring tank 11.

[0029] The rotating drum 3 houses an ultraviolet lamp 5, which is a cylindrical tube and coaxially mounted with the drum 3. A lamp holder 82 is located at the bottom of the outer casing 1 for mounting the ultraviolet lamp 5. The ultraviolet lamp 5 is either an excimer lamp or an ultraviolet LED lamp. A 308nm excimer lamp is preferred. Compared to traditional high-pressure mercury lamps, this type of light source offers a more precise wavelength range and significantly reduces heat generation, eliminating the need for filter layers and forced heat dissipation layers, thus simplifying the illumination system structure.

[0030] Figure 3As shown, the bottom of the outer casing 1 is equipped with a feed pipe and an air inlet pipe 61 for feeding material and nitrogen gas from the bottom. Considering installation and sealing issues, the design is as follows: The bottom of the outer casing 1 is equipped with a mounting hole, which is a stepped hole, or countersunk hole, consisting of a large hole and a small hole. A mounting base 81 is sealed and connected at the mounting hole, and a lamp holder 82 is located on the upper side of the mounting base 81. The lamp holder 82 and the mounting base 81 can be integrally set. The lamp holder 82 is equipped with a wire hole 823 and a first connecting flange hole 822 for fixing the ultraviolet lamp 5. The lamp holder 82 is equipped with a slot 821, which communicates with the wire hole 823. The cable passes through the wire hole 823 downwards, and the slot 821 is for the lower end of the lamp to be inserted. Then, the lamp is fixed by connecting and fixing with a flange. During installation, a sealing gasket is provided between the flange plates to achieve a sealing effect. Furthermore, after the cable passes through, sealant can be filled into the wire hole 823.

[0031] Figure 3 As shown, the mounting base 81 is provided with a second connecting flange hole 812 for connecting to the outer casing 1. When the flange plate where the second connecting flange hole 812 is located mates with the mounting hole at the bottom of the outer casing 1 (mates with the large hole), a sealing gasket is added. The outer periphery of the mounting base 81 is provided with a second sealing ring groove 811, which is fitted with a sealing ring for sealing mating with the mounting hole (mates with the small hole).

[0032] Figure 3 As shown, the mounting base 81 is also provided with a vent 814 and a feed hole 813. The feed hole 813 is used to install the feed pipe. There is a certain gap between the bottom of the drum 3 and the bottom wall of the outer casing 1 to facilitate feeding and prevent excessive friction during rotation. The feed pipe is connected to the storage tank and can be powered by the peristaltic pump 7 to supply material. Other pumps can also be used in other embodiments. The vent 814 is connected to the air inlet pipe 61 mentioned above. The air inlet pipe 61 is made of stainless steel and can be threaded, achieving a sealed connection at the same time. The external air supply pipe 62 can be a flexible hose, and its connector can also be threaded, connected to the bottom outside of the outer casing 1.

[0033] When using the photoreactor for vitamin synthesis, this utility model is as follows: (1) Open the nitrogen inlet valve to introduce nitrogen, replace the air in the device, and maintain a slight positive pressure in the reaction system.

[0034] (2) Prepare the reaction materials, store the materials in a storage tank, and control the temperature of the materials to the predetermined reaction temperature through a temperature control device; wherein the temperature control method is existing technology.

[0035] (3) Turn on the circulating water in the cooling water pipe and control the temperature to the predetermined reaction temperature. Turn on the light source and start the drum after the light source stabilizes. Wait for the drum speed to reach the predetermined speed and run stably.

[0036] (4) Start the peristaltic pump and begin feeding. The material flows from bottom to top inside the drum and the reacted liquid is collected at the top of the drum through the overflow ring groove.

[0037] During the reaction, the heat generated by the light source and the reaction is carried away by low-temperature nitrogen gas and indirectly cooled by cooling water pipes on the rotating drum. A thermometer can also be installed at the feed inlet area, and its readings can be compared with those at the discharge outlet. Based on the temperature difference between the two readings, the temperature of the circulating water in the cooling water pipes can be adjusted in a timely manner to achieve temperature control of the reaction liquid inside the rotating drum. Thermometers, also known as temperature detectors, are temperature measuring devices in existing technology, such as thermocouples.

Claims

1. A photoreaction apparatus for vitamin synthesis, characterized in that: The device includes an outer shell, within which a rotating drum is rotatably fitted. The outer wall of the outer shell has a sandwich structure, within which cooling water pipes are arranged. The bottom of the outer shell is provided with a feed pipe and an air inlet pipe. The lower part of the rotating drum is provided with a feed port, and the upper part is provided with an overflow hole. The air inlet pipe passes through the feed port and is used to introduce gas into the rotating drum. The drum is equipped with an ultraviolet lamp, which is a cylindrical lamp tube and is coaxially arranged with the drum; the bottom of the outer casing is equipped with a lamp holder for mounting the ultraviolet lamp.

2. The photoreactor for vitamin synthesis according to claim 1, characterized in that: The inner wall of the drum is provided with spiral grooves for guiding the reaction liquid upward.

3. The photoreactor for vitamin synthesis according to claim 1, characterized in that: The cooling water pipe is spirally coiled, with an inlet pipe at one end and a return pipe at the other end. The inlet and return pipes are located on the outside of the outer casing.

4. The photoreactor for vitamin synthesis according to claim 1, characterized in that: The upper part of the outer shell is provided with an overflow ring groove, and there are multiple overflow holes distributed along the circumference of the drum. The overflow ring groove is located around the overflow holes. The outer shell is connected to a discharge pipe, which is connected to the overflow ring groove. The discharge pipe is used to discharge the overflowed reaction liquid to the receiving tank.

5. The photoreactor for vitamin synthesis according to claim 4, characterized in that: The upper part of the drum is provided with a conical end, and each of the overflow holes is provided at the conical end.

6. The photoreactor for vitamin synthesis according to claim 4, characterized in that: A thermometer is provided on the upper part of the outer shell to detect the temperature of the reaction liquid in the overflow ring tank.

7. The photoreactor for vitamin synthesis according to claim 1, characterized in that: The ultraviolet lamp is an excimer lamp or an ultraviolet LED lamp.

8. The photoreactor for vitamin synthesis according to claim 1, characterized in that: The bottom of the outer casing is provided with a mounting hole, and a mounting base is sealed and connected to the mounting hole. The lamp holder is located on the upper side of the mounting base. The lamp holder is provided with a wire hole and a first connecting flange hole for fixing the ultraviolet lamp. The mounting base is provided with a second connecting flange hole for connecting to the outer casing. The mounting base is also provided with a vent hole and a feed hole. The feed hole is used to install the feed tube.

9. The photoreactor for vitamin synthesis according to claim 8, characterized in that: The outer periphery of the mounting base is provided with a sealing ring groove, which is fitted with a sealing ring for sealing and mating with the mounting hole.

10. The photoreactor for vitamin synthesis according to claim 8, characterized in that: The air intake pipe is used to introduce nitrogen gas, and the air intake pipe is provided with multiple exhaust holes for exhausting gas into the drum.

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