Continuous photochlorination reaction device and process with built-in light source
By using multi-layer quartz landfills and built-in ultraviolet light source lamps in the photochlorization reaction device, combined with reflux pump and gas-liquid phase balance control, the problems of low production efficiency and low chlorine utilization of existing photochlorization reaction devices are solved, and efficient continuous photochlorization reaction is achieved.
Patent Information
- Application Number
- CN202311872693.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2023-12-29
- Publication Date
- 2025-07-22
AI Technical Summary
The existing photochlorination reaction devices have problems with low production efficiency and low chlorine utilization. The built-in light source reactor cannot achieve continuous operation, while the material residence time of the external light source reactor is short, resulting in low reaction efficiency.
A built-in light source continuous photochlorination reaction device is designed, using multi-layer quartz landfill and ultraviolet light source tubes in high-temperature resistant glass sleeves, continuous feeding and discharge through a reflow pump, and the chlorine flow rate and liquid spraying amount are controlled to maintain full contact between the gas and liquid phase.
It improves the use rate of chlorine gas and the photochlorination conversion efficiency, realizes continuous operation and flexible control of the reaction, adapts to different reaction processes, is easy to maintain light sources, and improves production efficiency.
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Figure CN120346762A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the field of fine chemicals, and particularly to a continuous photochlorination reaction device and process with an internal light source. Background Art
[0002] Photochlorination reaction is a common chemical engineering unit operation and has wide applications in the pharmaceutical and fine chemical fields. In recent years, with the continuous development of photochlorination technology, various types of photochlorination reactor application technologies have emerged. Starting from the earliest structure of a reaction kettle, a light source, and a stirrer, various device types have been derived, including tower-type photochlorination devices, tube-type photochlorination devices, and so on. Although the manufacturing technology of photochlorination equipment is constantly innovating, these devices often have many drawbacks in the chlorination production process.
[0003] Currently, photochlorination reaction devices are mainly divided into two categories: internal light source type and external light source type. The internal light source type is generally a fixed kettle-type reactor, that is, a light source is installed inside the reaction kettle, and the material is in full contact with the light source. This type of reaction has a higher efficiency and avoids personnel injury caused by ultraviolet light. However, such a reactor can only perform single-kettle operation and cannot perform continuous operation, resulting in low production efficiency. The external light source type is generally a tower-type reactor with light-transmitting holes designed on the tower wall, and the light source irradiates the inside. Although this type of reactor can achieve continuous operation, there are problems such as short residence time of the material in the chlorination device, resulting in low photochlorination reaction efficiency and low chlorine utilization rate. Summary of the Invention
[0004] The purpose of the present invention is to provide a continuous photochlorination reaction device and process with an internal light source that can improve the reaction efficiency.
[0005] The present invention is implemented as follows:
[0006] The present invention provides a continuous photochlorination reaction device with an internal light source, including a tower body and a tower bottom liquid reflux pump. A photochlorination reaction zone is provided inside the tower body. It is characterized in that the photochlorination reaction zone is composed of multiple layers of quartz packed materials, and a plurality of radially extending high-temperature resistant glass sleeves are hermetically arranged outside the tower body corresponding to each layer of the packing. The high-temperature resistant glass sleeves are hermetically arranged between the tower body and the packing, and an ultraviolet light source lamp tube is hermetically configured inside each high-temperature resistant glass sleeve.
[0007] According to the above technical solution, a feed inlet and a reflux pump return port are provided on the tower body above the photochlorination reaction zone. A liquid distributor is provided below the feed inlet and the return port. A gas distributor is provided on the tower body below the reaction zone. Chlorine gas is introduced into the tower through the gas distributor. A reflux pump input port is provided at the bottom of the tower body. The input port of the reflux pump is connected to the bottom of the tower body, and the return port of the reflux pump is connected to the upper part of the tower body. An outlet for transporting the reaction product is also configured on the reflux pump.
[0008] According to the above technical solution, temperature monitoring ports are respectively arranged above and below the photochlorination reaction zone, and the severity of the reaction in the reaction zone is understood through the change of the temperature difference between the two points.
[0009] According to the above technical solution, the ultraviolet light source lamp tube is connected to the high-temperature resistant glass sleeve seat through an angle adjustment mechanism to realize the adjustment of a certain angle of the ultraviolet light source lamp tube in the sleeve.
[0010] According to the above technical solution, the angle adjustment mechanism includes a high-temperature resistant flexible seal sleeved on the outermost end of the ultraviolet light source lamp tube and a fixing member for fixing the ultraviolet light source lamp tube at a certain angle, and the high-temperature resistant flexible seal is hermetically configured with the high-temperature resistant glass sleeve.
[0011] According to the above technical solution, the height of the filler is 400 - 600 mm, and the wavelength of the ultraviolet light source is 200 - 400 nm.
[0012] According to the above technical solution, the high-temperature resistant glass sleeve and the filler are arranged at 90°, and multiple high-temperature resistant glass sleeves in each layer are circumferentially and uniformly arranged.
[0013] According to the above technical solution, a pressure monitoring port and a tail gas discharge port are arranged at the top of the tower for monitoring and adjusting the tower pressure and discharging the tail gas.
[0014] According to the above technical solution, the quartz packed bed has at least three layers, and the height between adjacent packings is 250 - 400 mm.
[0015] A process for photochlorination reaction using the above-mentioned built-in light source continuous photochlorination reaction device, characterized in that it includes the following steps:
[0016] Step 1: Feed through the feed port, establish the liquid level in the tower kettle, start the reflux pump, control the reflux feed ratio at 2 - 2.5, and continue feeding until the material circulation in the tower is stable;
[0017] Step 2: Pause feeding, start the light source in the photochlorination reaction zone, introduce 10 - 15 KG / H of chlorine at the chlorine inlet, the chlorine is introduced in excess, the material fully contacts with the chlorine in the quartz packing, and the photochlorination reaction is carried out through the excitation of the light source. The unreacted chlorine increases the tower pressure, and the tail gas discharge valve is opened to relieve the pressure.
[0018] Step 3: Monitor the pressure at the top of the tower, and control the pressure at 30 - 50 Kpa; monitor the change of the temperature monitoring above and below the photochlorination reaction zone, and control the temperature difference between the upper and lower at 2 - 2.5 °C. If it exceeds 3 °C, control the reaction rate by reducing the reflux amount or reducing the number of ultraviolet light sources.
[0019] Step 4: The materials in the tower are fully refluxed for 1.5-2 hours, at which time the liquid level drops to 450-500mm; the feed flow rate is restored, the liquid level rises to the set height, the reflux pump outlet is opened to extract the reaction product, and the tower bottom is maintained at 700-750mm. After normal operation, the tower bottom material is sampled for analysis.
[0020] According to the above technical scheme, in step one and two, the process of the present invention needs to control the point to balance the gas velocity and liquid spraying amount. During the reaction, the spray material (feed amount and reflux amount) contacts the chlorine gas in reverse on the packing layer, and the flow rate when the chlorine gas rise speed causes the liquid blocking phenomenon to begin in the packed tower is called the gas velocity of the load point. The gas velocity of the load point refers to that in the packed tower or the plate tower, the gas is from bottom to top, and the fluid is from top to bottom. When the gas velocity upward is too low, the liquid from top to bottom cannot be carried, and liquid leakage will occur, that is, the liquid does not flow downward according to the normal passage, but flows downward from the plug hole of the packing or the plate tower, and the flow rate when the chlorine gas rise speed causes the liquid blocking phenomenon to begin in the packed tower is called the gas velocity of the load point, and when the gas just carries the liquid, the critical gas velocity is the gas velocity of the load point, and liquid leakage will occur below this speed, affecting mass transfer and heat transfer. And the flooding point speed refers to that the gas velocity is too large, causing the liquid to not flow down normally, which will cause a large amount of liquid to accumulate in the packed tower or the plate tower, which will affect mass transfer and heat transfer, so that the tower cannot operate normally. When the gas velocity increases to the loading point velocity, the friction between the rising airflow and the descending liquid hinders the liquid from flowing down smoothly, so the liquid holding capacity of the packing layer increases with the increase of gas velocity. Therefore, its pressure drop increases faster, and the reaction rate is higher than before the loading point.
[0021] Therefore, the key points of this process control are
[0022] 1) Chlorine gas flow rate, that is, controlled between the two (the gas velocity at the loading point and the gas velocity at the flooding point). When the operating gas velocity of the packed tower is operated with the flooding point velocity as the limit, in most cases, it is 60% to 80% of the flooding point velocity, preferably about 70% of the flooding point velocity, that is, roughly around the gas velocity at the loading point. The gas velocity at the loading point is the basis for selecting the gas velocity. If the gas velocity is too high, the resistance is too large; if it is too low, the reaction rate is too low.
[0023] 2) Liquid spray volume (the sum of feed volume and reflux volume) The corresponding formula between liquid spray volume and gas velocity in the tower is:
[0024] Spray flow rate Q = tower cross-sectional area Scut * spray density uL.
[0025] The corresponding formula of the loading point gas velocity uVS and liquid spray density uL is:
[0026]
[0027] Where: L-liquid phase flow rate in the tower, Kg / h; V-gas phase flow rate in the tower, Kg / h;
[0028] ρv - Gas density in the tower, Kg / m 3 ; ρ L - Liquid density in the tower, Kg / m 3 .
[0029] In the present invention, by controlling the chlorine gas flow rate and liquid spraying amount (the sum of the feed amount and the reflux amount) in the photochlorination reaction zone, the gas-liquid phase is maintained in full contact on the packing to reach an equilibrium state, greatly improving the photochlorination reaction efficiency.
[0030] The beneficial effects of the present invention are as follows:
[0031] 1. In the present invention, multiple layers of packing are provided in the photochlorination reaction zone to increase the contact time and area between the materials and chlorine gas, improving the utilization rate of chlorine gas; then, an externally inserted built-in light source is adopted, combined with the light conduction of transparent quartz packing, greatly improving the photochlorination conversion efficiency.
[0032] 2. By respectively arranging temperature monitoring ports above and below the photochlorination reaction zone, that is, understanding the severity of the reaction through the change of the temperature difference between two points, the operability is strong.
[0033] 3. The irradiation angle of the ultraviolet light source lamp tube in the present invention can be adjusted according to the actual situation to be arranged at the best refraction angle, realizing full contact between the materials and the light source, and the photochlorination reaction process can be flexibly regulated according to the reaction situation, with strong applicability.
[0034] 4. The present invention adopts a sleeve-type lamp tube installation, which is easy for light source maintenance and replacement.
[0035] 5. The present invention adopts a reflux pump to realize continuous feeding and discharging operations, improving production efficiency.
[0036] 6. In the present invention, by controlling the chlorine gas flow rate and liquid spraying amount in the photochlorination reaction zone, the gas-liquid phase is maintained in full contact on the packing to reach an equilibrium state, greatly improving the photochlorination reaction efficiency. BRIEF DESCRIPTION OF THE DRAWINGS
[0037] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the following will briefly introduce the drawings required to be used in the embodiments. It should be understood that the following drawings only show some embodiments of the present invention, and therefore should not be regarded as limiting the scope. For those of ordinary skill in the art, other related drawings can be obtained based on these drawings without creative efforts.
[0038] Figure 1 It is the front view of a built-in light source continuous photochlorination reaction device provided by an embodiment of the present invention.
[0039] Figure 2 It is the cross-sectional schematic view of the packing layer provided by an embodiment of the present invention. DETAILED DESCRIPTION OF THE INVENTION
[0040] To make the objectives, technical solutions and advantages of the embodiments of the present invention clearer, the following will clearly and completely describe the technical solutions in the embodiments of the present invention with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are some, but not all, of the embodiments of the present invention. Components of the embodiments of the present invention generally described and illustrated in the accompanying drawings here can be arranged and designed in a variety of different configurations.
[0041] Therefore, the following detailed description of the embodiments of the present invention provided in the drawings is not intended to limit the scope of the claimed invention, but merely represents selected embodiments of the present invention. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts fall within the scope of protection of the present invention.
[0042] It should be noted that like reference numerals and letters denote like items in the following drawings. Therefore, once an item is defined in one drawing, it does not need to be further defined and explained in subsequent drawings.
[0043] In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc. indicate the orientation or positional relationship based on the orientation or positional relationship shown in the drawings, or the orientation or positional relationship in which the product of this application is customarily placed during use. This is 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 construed as a limitation of the present invention. In addition, the terms "first", "second", "third", etc. are only used for descriptive distinction and should not be construed as indicating or implying relative importance.
[0044] In addition, terms such as "horizontal", "vertical", "overhanging", etc. do not mean that the components are required to be absolutely horizontal or overhanging, but may be slightly inclined. For example, "horizontal" only means that its direction is more horizontal relative to "vertical", and does not mean that the structure must be completely horizontal, but may be slightly inclined.
[0045] In the description of the present invention, it should also be noted that unless otherwise clearly specified and defined, the terms "set", "installed", "connected", "connected to" should be understood in a broad sense. For example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be directly connected or indirectly connected through an intermediate medium, and it can be the communication inside two elements. For those of ordinary skill in the art, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.
[0046] In the present invention, unless otherwise clearly specified and defined, the first feature being "on" or "under" the second feature may include direct contact between the first and second features, or may include the first and second features not being in direct contact but in contact through additional features therebetween. Moreover, the first feature being "above", "over" and "on top of" the second feature includes the first feature being directly above and obliquely above the second feature, or merely indicating that the horizontal height of the first feature is higher than that of the second feature. The first feature being "under", "beneath" and "underneath" the second feature includes the first feature being directly below and obliquely below the second feature, or merely indicating that the horizontal height of the first feature is less than that of the second feature.
[0047] The features and performance of the present invention will be further described in detail below in conjunction with embodiments.
[0048] As Figure 1 , 2 shown, the present invention provides a continuous photochlorination reaction device with an internal light source, which includes a three-stage photochlorination tower. The tower body is made of carbon steel with a Teflon coating on the inner wall. From top to bottom, the first stage is the material feeding area, which has a material feeding port 6 and a reflux port 8. A liquid distributor 12 is installed to evenly distribute the material downward. There is a tail gas discharge port 10 and a pressure monitoring port 4 at the top of the tower. The second stage is the photochlorination reaction area 1, where the material and chlorine contact and react in a countercurrent manner. The third stage is the gas feeding and bottom liquid collection area, which is provided with a chlorine gas inlet 7. A gas distributor 16 is installed to evenly distribute the chlorine gas upward to the reaction area. A pressure monitoring port is provided at the lower part of the tower, and a liquid level monitor 11 is provided in the bottom liquid collection area. A bottom liquid reflux pump 2 is provided at the bottom of the tower. When the bottom liquid level is higher than the set level, the bottom liquid returns to the upper feeding area of the tower through the reflux pump, realizing the cyclic reaction of the material in the tower. A stream of reacted material is taken out at the pump outlet for discharging. Continuous photochlorination reaction is achieved with simultaneous feeding and discharging.
[0049] In this embodiment, the photochlorination reaction area is composed of 6 layers of quartz packed fillers 13. Corresponding to each layer of filler 13 outside the tower body, a plurality of high-temperature resistant glass sleeves 14 extending radially are hermetically arranged. The high-temperature resistant glass sleeves 14 are hermetically arranged between the tower body and the filler 13. An ultraviolet light source lamp tube 15 is hermetically configured in each high-temperature resistant glass sleeve 14. Chlorine gas enters the tower through the chlorine gas inlet 7 and is introduced into the tower through the gas distributor 16. The chlorine gas and the material contact in a countercurrent manner in the filler layer. At the same time, the built-in ultraviolet light source irradiates and conducts through the quartz filler, exciting the photochlorination reaction. By arranging an internal ultraviolet reaction light source in the filler in the present invention, the light source conduction effect is greatly increased in the quartz filler, improving the photochlorination excitation effect. Since the photochlorination reaction is an exothermic reaction, temperature monitoring ports (18, 3) are provided at the upper and lower parts of the reaction area to understand the severity of the reaction through the change of the temperature difference between the two points.
[0050] The reflux pump 2 is used to pump the bottom material of the tower to the top of the tower and back into the tower, so that the material can circulate in the tower. The reflux pump is provided with an outlet for discharging the product after the reaction. Specifically, a reflux pump inlet 17 is provided at the bottom of the tower body. The inlet of the reflux pump is connected to the bottom of the tower body, and the return material port 8 of the reflux pump is connected to the upper part of the tower body. An outlet 9 for transporting the reaction product is also configured on the reflux pump.
[0051] In this embodiment, a sight glass 5 is arranged between every two layers of packing for observing the light source illumination.
[0052] Specifically, 4 borosilicate high-temperature resistant glass sleeves 14 are inserted into the middle of each layer of packing 13. The 4 high-temperature resistant glass sleeves of each layer are circumferentially and evenly arranged. Among them, the tower diameter D is 600 mm, the height between adjacent packings is 300 mm, the packing height is 500 mm, and the quartz packing is Dg50 Raschig rings or Pall rings. The sleeve 14 and the tower body are sealed with fluororubber. The included angle between each high-temperature resistant glass sleeve and the packing is 90 degrees. Then, the ultraviolet light source lamp tube 15 is inserted into the sleeve 14 to install the built-in light source. The wavelength of the light source is 200 - 400 nm, preferably 280 - 330 nm.
[0053] In this embodiment, when it is necessary to adjust the angle of the ultraviolet light source lamp tube, an angle adjustment mechanism can be set so that the ultraviolet light source lamp tube can be adjusted up and down by 15 - 30 degrees in the sleeve. It can flexibly control the photochlorination reaction process according to the reaction conditions to achieve the best light reflection effect and improve the photochlorination conversion efficiency. Specifically, the angle adjustment mechanism includes a high-temperature resistant flexible seal sleeved on the outermost end of the ultraviolet light source lamp tube and a fixing member for fixing the ultraviolet light source lamp tube at a certain angle. The high-temperature resistant flexible seal is hermetically configured with the high-temperature resistant glass sleeve.
[0054] This embodiment also provides a process for photochlorination reaction, which includes the following steps:
[0055] Step 1: Feed the material from the feed port 6, with the content being 98.3% silicon tetrachloride, 1.6% methylchlorosilane, and 0.1% other impurities; the feeding rate is 830 KG / H. Establish the height of the bottom tower liquid level 11 to be 900 mm. Start the reflux pump 2, and control the reflux feeding ratio to be 2 - 2.5. Continue feeding until the material in the tower circulates and the bottom tower liquid level reaches equilibrium at 750 mm liquid level, and then pause feeding.
[0056] Step 2: Start the light source in the photochlorination reaction zone 1, and introduce 10 - 15 KG / H of chlorine gas at the chlorine gas inlet 7. The chlorine gas is introduced in excess. The material fully contacts with the chlorine gas in the quartz packing 13 and undergoes a photochlorination reaction by being excited by the light source 15. The unreacted chlorine gas causes the tower pressure to rise, and the tail gas discharge 10 is opened for pressure relief.
[0057] Step 3, monitor the pressure at the top of the tower, and control the pressure at 30-50Kpa; monitor the temperature changes of the upper and lower parts of the photochlorination reaction zone 1, and monitor 3 and 18, and control the upper and lower temperature difference by 2-2.5°C. If it exceeds 3°C, control the reaction rate by reducing the reflux flow or reducing the number of ultraviolet light sources;
[0058] Step 4: The materials in the tower are fully refluxed for 1.5-2 hours, at which time the liquid level drops to 450-500 mm; the feed flow rate of 830 kg / h is restored, the liquid level rises to 750 mm, the reflux pump outlet is opened to extract the reaction product, and the tower bottom is maintained at 700-750 mm. After normal operation, the tower bottom material is sampled for analysis. Methylchlorosilane reacts with chlorine to generate chloromethylchlorosilane, and the methylchlorosilane content is less than 0.05%.
[0059] In the present embodiment, in step one and two, the process of the present invention needs to control the point to be the balance of the gas velocity and liquid spraying amount. During the reaction, the spray material (feed amount and reflux amount) contacts the chlorine gas in reverse on the packing layer, and the flow rate when the chlorine gas rise speed causes the liquid blocking phenomenon to begin in the packed tower is called the gas velocity of the load point. The gas velocity of the load point refers to that in a packed tower or a plate tower, the gas is from bottom to top, and the fluid is from top to bottom. When the gas velocity upward is too low, the liquid from top to bottom cannot be carried, and liquid leakage will occur, that is, the liquid does not flow downward according to the normal passage, but flows downward from the plug hole of the packing or the plate tower, and the flow rate when the chlorine gas rise speed causes the liquid blocking phenomenon to begin in the packed tower is called the gas velocity of the load point, and when the gas just carries the liquid, the critical gas velocity is the gas velocity of the load point, and liquid leakage will occur below this speed, affecting mass transfer and heat transfer. And the flooding point speed refers to that the gas velocity is too large, causing the liquid to not flow down normally, which will cause a large amount of liquid to accumulate in the packed tower or the plate tower, which will affect mass transfer and heat transfer, so that the tower cannot operate normally. When the gas velocity increases to the loading point velocity, the friction between the rising airflow and the descending liquid hinders the liquid from flowing down smoothly, so the liquid holding capacity of the packing layer increases with the increase of gas velocity. Therefore, its pressure drop increases faster, and the reaction rate is higher than before the loading point.
[0060] Therefore, the key points of this process control are
[0061] 3) Chlorine gas flow rate, that is, controlled between the two (the gas velocity at the loading point and the gas velocity at the flooding point). When the operating gas velocity of the packed tower is operated with the flooding point velocity as the limit, in most cases, it is 60% to 80% of the flooding point velocity, preferably about 70% of the flooding point velocity, that is, roughly around the gas velocity at the loading point. The gas velocity at the loading point is the basis for selecting the gas velocity. If the gas velocity is too high, the resistance is too large; if it is too low, the reaction rate is too low.
[0062] 4) Liquid spray volume (the sum of feed volume and reflux volume) The corresponding formula between liquid spray volume and gas velocity in the tower is:
[0063] Spray flow rate Q = tower cross-sectional area Scut * spray density uL.
[0064] The corresponding formulas for the loading point gas velocity uVS and the liquid spraying density uL are as follows:
[0065]
[0066] In the formula: L is the liquid phase flow rate in the tower, Kg / h; V is the gas phase flow rate in the tower, Kg / h;
[0067] ρv is the gas phase density in the tower, Kg / m 3 ; ρ L - is the liquid density in the tower, Kg / m 3 .
[0068] In the present invention, by controlling the chlorine gas flow rate and the liquid spraying amount (the sum of the feed amount and the reflux amount) in the photochlorination reaction zone, the gas-liquid phase is maintained in full contact on the packing to reach an equilibrium state, greatly improving the photochlorination reaction efficiency.
[0069] The embodiments described above are some, but not all, of the embodiments of the present invention. The detailed description of the embodiments of the present invention is not intended to limit the scope of the present invention claimed, but merely represents selected embodiments of the present invention. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without making creative efforts fall within the scope of protection of the present invention.
Claims
1. A continuous photochlorination reaction device with an internal light source, comprising a tower body and a tower bottom liquid reflux pump. A photochlorination reaction zone is provided inside the tower body, and it is characterized in that, The photochlorination reaction zone is composed of multiple layers of quartz stack fillers. A plurality of radially extending high-temperature resistant glass sleeves are sealed outside the tower body corresponding to each layer of fillers. The high-temperature resistant glass sleeves are sealed with the tower body and the fillers. An ultraviolet light source lamp is sealed in each high-temperature resistant glass sleeve.
2. The continuous photochlorination reaction device with an internal light source according to claim 1, characterized in that, A feed inlet and a reflux pump return port are provided on the tower body above the photochlorination reaction zone, a liquid distributor is provided below the feed inlet and the return port, a gas distributor is provided on the tower body below the reaction zone, chlorine gas is introduced into the tower through the gas distributor, a reflux pump input port is provided at the bottom of the tower body, the input port of the reflux pump is connected to the bottom of the tower body, the return port of the reflux pump is connected to the upper part of the tower body, and an outlet for conveying reaction products is also arranged on the reflux pump.
3. The continuous light chlorination reaction device with built-in light source according to claim 1 or 2, characterized in that Temperature monitoring ports are set up above and below the photochlorination reaction zone, and the intensity of the reaction in the reaction zone can be understood by the temperature difference between the two points.
4. The continuous photochlorination reaction device with built-in light source according to claim 1 or 2, characterized in that, The ultraviolet light source lamp tube is connected to the high temperature resistant glass sleeve seat through an angle adjustment mechanism to achieve the adjustment of the ultraviolet light source lamp tube to a certain angle in the sleeve tube.
5. The continuous photochlorination reaction device with an internal light source according to claim 4, characterized in that, The angle adjustment mechanism comprises a high temperature resistant flexible seal sleeved on the outermost end of the ultraviolet light source tube and a fixing member for fixing the ultraviolet light source tube at a certain angle. The high temperature resistant flexible seal is sealed with the high temperature resistant glass sleeve.
6. The continuous light chlorination reaction device with built-in light source according to claim 1 or 2, characterized in that The quartz pile filler is provided with at least three layers, and the height between adjacent fillers is 250-400 mm; the height of the filler is 400-600 mm, and the wavelength of the ultraviolet light source is 200-400 nm.
7. The continuous light chlorination reaction device with an internal light source according to claim 1 or 2, characterized in that The high temperature resistant glass sleeves are arranged at 90 degrees to the filler, and the multiple high temperature resistant glass sleeves in each layer are evenly arranged in the circumferential direction.
8. The continuous photochlorination reaction device with built-in light source according to claim 1 or 2, characterized in that A pressure monitoring port and an exhaust gas discharge port are provided on the top of the tower to monitor and adjust the tower pressure and exhaust gas discharge.
9. A process for carrying out a photochlorination reaction using the built-in light source continuous photochlorination reaction device according to any one of claims 1-9, characterized in that: The steps include: Step 1: Feed material from the feed inlet, establish the tower bottom liquid level, start the reflux pump, control the reflux feed ratio to 2-2.5, and continue feeding until the material circulation in the tower is stable; Step 2: Pause feeding, start the light source in the photochlorination reaction zone, introduce 10-15KG / H chlorine at the chlorine inlet, the chlorine is introduced in excess, the material is fully in contact with the chlorine on the quartz filler, the light source is used to excite the photochlorination reaction, the unreacted chlorine increases the tower pressure, and the tail gas is discharged to release the pressure. Step 3, monitor the pressure at the top of the tower, and control the pressure at 30-50Kpa; monitor the changes in the temperature monitoring above and below the photochlorination reaction zone, and control the upper and lower temperature difference at 2-2.5°C. If it exceeds 3°C, control the reaction rate by reducing the reflux flow or the number of ultraviolet light sources; Step 4: The materials in the tower are fully refluxed for 1.5-2 hours, at which time the liquid level drops to 450-500mm; the feed flow rate is restored, the liquid level rises to the set height, the reflux pump outlet is opened to extract the reaction product, and the tower bottom is maintained at 700-750mm. After normal operation, the tower bottom material is sampled for analysis.
10. The process of photochlorination according to claim 9, wherein: In steps 1 and 2, the chlorine gas flow rate and liquid spraying amount in the photochlorination reaction zone are controlled to maintain sufficient contact between the gas and liquid phases on the filler to reach an equilibrium state; Among them, the calculation relationship between the chlorine gas flow rate and the liquid spraying amount is shown in the following formula: The spray flow rate Q = the cross-sectional area of the tower S_sect * the spray density uL; (1) The corresponding formulas for the flooding gas velocity uVS and the liquid spray density uL are as follows: Where: L - the liquid phase flow rate in the tower, Kg / h; V - the gas phase flow rate in the tower, Kg / h; ρv - Gas density in the tower, Kg / m 3 ; ρ L - Liquid density in the tower, Kg / m 3 .