Continuous feeding intelligent chemical reaction device
By designing a continuous feed intelligent chemical reaction device in a chemical reaction device, using a high shear homogenization rotor and microchannel reaction combination, the continuous and instantaneous uniform mixing of each material is solved, and the problem of chemical enterprises being difficult to achieve uniform mixing of reaction materials and controllable reaction processes during chemical reactions is significantly reduced.
Patent Information
- Application Number
- CN202510231217.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-02-28
- Publication Date
- 2025-04-25
AI Technical Summary
While chemical enterprises can control the temperature, pressure and flow rate of the chemical reaction process, it is difficult for chemical enterprises to achieve continuous and equal batching ratios of each reaction material and instantly uniform mixing, resulting in the generation of by-products and the discharge of waste slag, wastewater and waste gas.
A continuous feed intelligent chemical reaction device is designed, and the entire chemical reaction process is connected by computer distribution control system (DCS). Through the combination of high shear homogenization rotor and microchannel reactions, the continuous equal distribution and instantaneous uniform mixing of each material is achieved, forcing the maximum coupling chemical reaction.
The continuous and instantaneous uniform mixing of various materials in chemical reactions is achieved, which maximizes the coupling degree of chemical reactions, reduces the generation of by-products, and effectively controls the temperature, pressure and flow during the reaction process, and reduces the emission of waste slag, wastewater and waste gas.
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Figure CN119869389A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to a chemical reaction device, in particular to a continuous feeding intelligent chemical reaction device. Background Art
[0002] The enhanced reaction mode used in petroleum, chemical industry and chemical synthesis drugs is mainly devoted to reducing the by-products caused by local heterogeneous reactions. For example, Chinese patents CN2006200785544, CN201410276754X, CN201520768934X, etc. partially solve the problem of instant mixing and immediate heat removal. However, how to achieve the initial reaction materials to be continuously fed at the same proportion; how to force the materials to be mixed uniformly in an instant, how to achieve the maximum degree of reaction coupling and how to control the temperature, pressure and flow rate of the chemical reaction process, is a fundamental problem for chemical companies to still discharge waste residues, wastewater and waste gas. Summary of the invention
[0003] The present invention provides a continuous feeding intelligent chemical reaction device, which is linked to a computer distributed control system (DCS) for the entire chemical reaction process, so that materials of specified proportions can simultaneously and continuously enter a customized mixing chamber for high shear homogenization, and then forced to achieve a maximum degree of coupled chemical reaction in a microchannel reaction combination.
[0004] The technical solution adopted by the present invention is: A continuous feeding intelligent chemical reaction device comprises a computer distributed control system DCS, a material mixing chamber, a speed regulating stirring motor, and a high shear homogenizing rotor, wherein the speed regulating stirring motor is connected to the high shear homogenizing rotor, and the high shear homogenizing rotor is arranged in the material mixing chamber; the material inlet is sequentially connected through a solenoid valve, an extrusion filter, an ultrafilter, a terminal sensor combination, and the rear of the solenoid valve and the material mixing chamber; the catalyst inlet is sequentially connected through a solenoid valve, an extrusion filter, an ultrafilter, a terminal sensor combination, a mixing chamber pipeline, and the rear of the solenoid valve and the material mixing chamber; the nitrogen replacement inlet is sequentially connected through a solenoid valve, an extrusion filter, an ultrafilter, a terminal sensor combination, a mixing chamber pipeline, and the rear of the solenoid valve and the material mixing chamber. The filter, the terminal sensor assembly, the mixing chamber pipeline, the electromagnetic valve and the material mixing chamber are connected; the material mixing chamber outlet is formed after passing through the microchannel reactor, the static mixer, the reaction material manifold, the terminal sensor assembly, the relay extrusion gear pump, the single-tube static mixer and the terminal sensor assembly in sequence; the outlet includes a circulation outlet, a qualified product outlet and a unqualified product outlet, and each outlet is controlled by its own electromagnetic valve; a heat carrier / cold carrier jacket is provided on the periphery of the static mixer; the electromagnetic valve, the terminal sensor assembly, the relay extrusion gear pump and the speed regulating stirring motor are all electrically connected to the computer distributed control system DCS.
[0005] It includes a flushing mechanism, wherein the outlet end of the reaction material manifold is connected to the flushing material inlet through a solenoid valve, and the liquid material mixing chamber is connected to the flushing material outlet through a two-stage solenoid valve; a solenoid valve is arranged between the solenoid valve in front of the flushing material outlet and the outlet end of the reaction material manifold; the solenoid valve is electrically connected to a computer distributed control system DCS.
[0006] A continuous feeding intelligent chemical reaction device comprises a computer distributed control system DCS, a material mixing chamber, a speed regulating stirring motor, and a high shear homogenizing rotor, wherein the speed regulating stirring motor is connected to the high shear homogenizing rotor, and the high shear homogenizing rotor is arranged in the liquid material mixing chamber; the material inlet is connected to the material mixing chamber through a terminal sensor combination and an electromagnetic valve; the liquid / gas catalyst material inlet is divided into two routes, one route is connected to the material mixing chamber after passing through the terminal sensor combination and the electromagnetic valve; the other route is a backwashing mechanism, the liquid / gas catalyst material inlet is connected to the upper buffer manifold through the electromagnetic valve, and the lower buffer manifold is connected to the electromagnetic valve and The backwash residue liquid outlet is connected; a microchannel reactor is arranged between the upper buffer manifold and the lower buffer manifold; the upper buffer manifold forms an outlet through a static mixer, a single-tube series static mixer group, and a terminal sensor, and the outlet includes a circulation outlet, a qualified product outlet, and a non-qualified product outlet, and each outlet is controlled by a respective solenoid valve; the lower buffer manifold is connected to the material mixing chamber; the static mixer and the single-tube series static mixer group are both provided with a heat carrier / cold carrier jacket on their peripheries; the solenoid valve, the terminal sensor assembly, and the speed regulating stirring motor are all electrically connected to a computer distributed control system DCS.
[0007] The static mixer is an SK type static mixer with adjustable length.
[0008] The positions of the static mixer and the microchannel reactor are adjustable.
[0009] A continuous feeding intelligent chemical reaction device comprises a computer distributed control system DCS, a material mixing chamber, a speed regulating stirring motor, and a high shear homogenizing rotor, wherein the speed regulating stirring motor is connected to the high shear homogenizing rotor, and the high shear homogenizing rotor is arranged in a cylinder of a continuous polymerization reaction device; a material inlet is connected to the cylinder of the continuous polymerization reaction device through a terminal sensor combination and an electromagnetic valve, and a catalyst inlet is connected to the cylinder of the continuous polymerization reaction device through a terminal sensor combination and an electromagnetic valve; the high shear homogenizing rotor is sealed by a dynamic seal; an outlet of the cylinder of the continuous polymerization reaction device is formed through the terminal sensor combination, and the outlet comprises an outlet for qualified products and an outlet for unqualified products, and each outlet is controlled by a respective electromagnetic valve; a heat carrier / cold carrier pipeline is arranged in the cylinder of the continuous polymerization reaction device.
[0010] In the present invention, each material is pre-filtered to remove tiny mechanical impurities, and a microchannel reaction combination is customized for the backwash cleaning process. The chemical reaction device is provided with a three-way pipe and a solenoid valve at a specified position to control the circulation of fluid materials, and the qualified intermediate products and unqualified intermediate products are output to different pipes and enter the subsequent processing unit after online automatic detection. The entire chemical reaction process is linked to a computer distributed control system (DCS), so that each material with a specified ratio can enter the customized mixing chamber simultaneously and continuously, perform high shear homogenization, and then force the maximum degree of coupled chemical reaction in the microchannel reaction combination. BRIEF DESCRIPTION OF THE DRAWINGS
[0011] Figure 1 This is a schematic diagram of the structure of Embodiment 1 of the present invention; Figure 2 This is a schematic diagram of the structure of Embodiment 2 of the present invention; Figure 3 This is a schematic diagram of the structure of Example 3 of the present invention. DETAILED DESCRIPTION
[0012] The present invention is further described below in conjunction with the accompanying drawings and specific production practices.
[0013] Example 1, reference Figure 1A continuous feeding intelligent chemical reaction device comprises a computer distributed control system DCS, a material mixing chamber 5, a speed regulating stirring motor 6 (rotation speed is 1.5-20,000 rpm), and a high shear homogenizing rotor 7. The speed regulating stirring motor 6 is connected to the high shear homogenizing rotor 7, and the high shear homogenizing rotor 7 is arranged in the material mixing chamber 5; the material inlet 1 passes through the electromagnetic valve 20-1, the extrusion filter 2-1 (diameter 200mm), the ultrafilter 3-1 (pore size <0.45µm), the terminal sensor combination 4-1, and the electromagnetic valve 20-3 in sequence and then passes through the material mixing chamber 5; the catalyst inlet 15 passes through the electromagnetic valve 20-2, the extrusion filter 2-1 (diameter 200mm), the ultrafilter 3-1 (pore size <0.45µm), the terminal sensor combination 4-1, and the electromagnetic valve 20-3 in sequence. 2, ultrafilter 3-2, terminal sensor assembly 4-2, mixing chamber pipeline 16, solenoid valve 20-4 and material mixing chamber 5 are connected; nitrogen replacement inlet 18-1 passes through solenoid valve 20-13, extrusion filter 2-2, ultrafilter 3-2, terminal sensor assembly 4-2, mixing chamber pipeline 16, solenoid valve 20-4 and material mixing chamber 5 in sequence; the outlet of the material mixing chamber 5 passes through microchannel reactor 8, static mixer 9 (single tube inner diameter <50mm, length can be increased or decreased), reaction material manifold 11, terminal sensor assembly 4-3, relay extrusion gear pump 12, single tube static mixer 13 (single tube inner diameter >25mm x length>300mm static mixer), terminal sensor combination 4-4 and then form an outlet; the outlet includes a circulation outlet 14-3, a qualified product outlet 14-1, and a non-qualified product outlet 14-2, each outlet is controlled by a respective solenoid valve; the outer periphery of the static mixer is provided with a heat carrier / cold carrier jacket, and the heat carrier / cold carrier jacket has an inlet 10-1 and an outlet 10-2; the solenoid valve, terminal sensor combination, relay extrusion gear pump, and speed regulating stirring motor are all electrically connected to the computer distributed control system DCS. The outlet end of the reaction material manifold 11 is provided with a slag removal pipe port 17 for maintenance.
[0014] The terminal sensor combination includes a pressure sensor-P, a temperature sensor-T, a flow sensor-L, and an online quality detection sensor Q.
[0015] Example 1 The specific process of the reaction of sulfonating industrial naphthalene with liquid sulfur trioxide to synthesize 1,5-naphthalene disulfonate is as follows: Start the DCS computer control program, add 82.0 tons of solid industrial naphthalene and inert solvent of the specified ingredients into the original jacketed reactor, slowly heat to 60℃±2, and stir at constant temperature for 2 hours. Open the solenoid valves 20-1, 20-3, 20-5, and 20-11. Start the pump to output the mixed material through the material inlet 1, the squeeze filter 2-1, and the ultrafilter 3-1 for precision filtration. The solid impurities in the mixed material are detected by the terminal sensor combination 4-1 with a diameter of less than 0.8µm and then input into the feed mixing chamber 5 and the high shear homogenizing rotor 7 with a speed regulating stirring motor 6 driving >150 rpm, pass through the microchannel reactor 8, and then pass through the tube bundle (single tube inner diameter <30mm) SX type static mixer 9, open the heat carrier / cold carrier jacket to keep the temperature of the mixed material at 48℃±2 and enter the reaction material manifold 11. The relay extrusion gear pump 12 is started to output the mixed material through the single-tube static mixer 13, and then returns to the original reactor through the circulation outlet 14-3 for circulation and constant temperature at 48°C ± 2 (4-3).
[0016] At the same time, the commercially available raw material liquid sulfur trioxide is in the original 5.0M3 storage tank. The DCS command opens the solenoid valves 20-2, 20-4, 20-5, and 20-10; at the same time, the solenoid valve 20-13 is closed. The magnetic pump is started to output liquid sulfur trioxide and the pressure in the catalyst inlet 15 pipeline is increased to ≯0.3MPa, which is detected by the terminal sensor combination 4-2. After the specified proportion of sulfur trioxide is finely filtered by the extrusion filter 2-2 and the ultrafilter 3-2, the solid impurities are detected by the terminal sensor combination 4-2. After the diameter is less than 0.8µm, the terminal sensor combination 4-2 automatically measures and enters the feed mixing chamber 5.
[0017] After the nitrogen is filtered through the electromagnetic valve 20-13, the squeeze filter 2-2, and the ultrafilter 3-2 from the nitrogen replacement inlet 18-1, the end sensor combination 4-2 detects that the diameter of solid impurities in the industrial nitrogen is less than 0.8µm, and then enters the material mixing chamber 5 after passing through the mixing chamber pipeline 16 and the electromagnetic valve 20-4 to force the air in the liquid mixture to be replaced for ≮2 hours to ensure the shear safety of the subsequent reaction process and the appearance of the reaction product. Then the DCS slowly increases the speed of the speed-adjusting stirring motor 6 to >1200 rpm to continue the cycle.
[0018] The liquid industrial naphthalene mixture and liquid sulfur trioxide with the specified proportion are continuously fed into the feed mixing chamber 5 at the flow rate and linear speed ≮3m / s specified by DCS. They are forced to mix by the high shear homogenizing rotor 7 in ≯0.3s to achieve the specified high degree of reaction coupling. The reaction materials are then forced into the microchannel reactor 8 with an inner diameter of <1.0mm for chemical reaction. The intense heat generated by the reaction is quickly removed by the water in the heat carrier / cold carrier jacket outside the tube bundle of the SX type static mixer 9. The temperature of the reactants is kept constant at 50℃±2. The product generated by the reaction enters the inlet of the relay extrusion gear pump 12 from the lower part of the reaction material collection pipe 11, is pressurized by the gear pump, and then enters the SK type series single tube (inner diameter>50mmXlength>2m) static mixer 13 for forced aging reaction. After the conversion rate of the sulfonated product detected by the terminal sensor combination 4-4 reaches ≮95, the solenoid valve 20-9 is automatically opened and then enters the designated conventional reactor through the qualified product outlet 14-1 to supplement the aging reaction; otherwise, the solenoid valve 20-10 is automatically opened, and at the same time, the solenoid valve 20-9 is closed and enters the designated unit through the unqualified outlet 14-2.
[0019] The blockage disposal structure of the microchannel reactor is a flushing mechanism, wherein the outlet end of the reaction material manifold 11 is connected to the flushing material inlet 18-2 through the solenoid valve 20-12, and the material mixing chamber 5 is connected to the flushing material outlet 19 (where the pipeline pressure resistance is greater than 1.6 MPa) through the two-stage solenoid valves 20-8 and 20-7; a solenoid valve 20-6 is provided between the solenoid valve 20-7 before the flushing material outlet and the outlet end of the reaction material manifold 11; the solenoid valve is electrically connected to the computer distributed control system DCS.
[0020] When the pressure in the microchannel reactor 8, the static reactor 9 and the reaction material manifold 11 suddenly rises to >0.3MPa, the DCS instructs the solenoid valves 20-1, 20-2, 20-3, 20-4, 20-5 and 20-6 to close automatically. At the same time, the solenoid valves 20-7, 20-8 and 20-12 at the specified position of the flushing pipe 18-2 are automatically opened. The terminal sensor assembly 4-3 begins to flush the microchannel reactor 8, the static reactor 9 and the reaction material manifold 11 with nitrogen of the specified standard and pressure, and the waste residue and waste gas after flushing enter the designated unit through the flushing material outlet 19. Until the pressure in the microchannel reactor 8, the static reactor 9 and the reaction material manifold 11 suddenly drops to <0.2MPa, the DCS instructs the recovery process, and the material inlet 1 and the catalyst inlet 15 are in the simultaneous continuous feeding and instantaneous mixing uniform operation state. According to the change of working conditions, the microchannel reactor 8 and the tube bundle static mixer 9 can be disassembled or exchanged; the inner diameter of the microchannel reactor 8 is less than 0.7 mm, and it is a commercially available device.
[0021] This method uses DCS program control to achieve reaction process intensification and achieve maximum chemical reaction coupling; it reduces oversulfonation byproducts by more than 95%; and reduces waste acid emissions by more than 90%. This method can also be used to sulfonate naphthalene using the gaseous sulfur trioxide / concentrated sulfuric acid method.
[0022] Example 2, reference Figure 2 A continuous feeding intelligent chemical reaction device comprises a computer distributed control system DCS, a material mixing chamber 25, a homogenizing pump 26 provided with a stator, a high shear homogenizing rotor 27, and a speed regulating stirring motor 28, wherein the speed regulating stirring motor 28 is connected to the high shear homogenizing rotor 27, and the high shear homogenizing rotor 27 is arranged in the liquid material mixing chamber 25; a material inlet 21 is connected to the material mixing chamber 25 through a terminal sensor combination 24-1 and a solenoid valve 23-1; a liquid / gas catalyst material inlet 22 is divided into two paths, one of which is connected to the material mixing chamber 25 after passing through a terminal sensor combination 24-2 and a solenoid valve 23-2; the other path is a backwashing mechanism, the liquid / gas catalyst material inlet 22 is connected to an upper buffer manifold 31-2 through a solenoid valve 23-3, and a lower buffer manifold 31-1 is connected to a backwashing residue liquid outlet 29 through a solenoid valve 23-4; a microchannel reactor 30 is arranged between the upper buffer manifold 31-2 and the lower buffer manifold 31-1, and its inner diameter is less than 1.0 mm. The upper buffer manifold 31-2 forms an outlet through a static mixer 32 (a tube bundle (single tube inner diameter <30mm) SX / SK type static mixer), a single tube series static mixer group 34, and a terminal sensor combination 24-3, the outlet includes a circulation outlet 36, a qualified product outlet 38, and a non-qualified product outlet 37, each outlet is controlled by a respective solenoid valve, the circulation outlet 36 is controlled by a solenoid valve 23-5; the qualified product outlet 38 is controlled by a solenoid valve 23-7; the non-qualified product outlet 37 is controlled by a solenoid valve 23-6; the lower buffer manifold 31-1 is connected to the material mixing chamber 25; the static mixer 32 is provided with a heat carrier / cold carrier jacket on the periphery, the jacket has an inlet 33-1 and an outlet 33-2; the single tube series static mixer group 34 is provided with a heat carrier / cold carrier jacket on the periphery, the jacket has an inlet 35-1 and an outlet 35-2; all the above-mentioned solenoid valves, all the terminal sensor combinations, and the speed regulating stirring motor are electrically connected to the computer distributed control system DCS.
[0023] Example 2 is applied to the addition reaction process of synthesizing metformin hydrochloride with dimethylamine: Start the DCS computer control program, open the solenoid valve 23-1, and clear the material inlet 21; at the same time, open the solenoid valve 23-5 and clear the material circulation pipeline. Add the specified ingredients of dimethylamine hydrochloride and 25.0 tons of isoamyl alcohol and 10.0 tons of distilled water into 60M 3The materials in the original mixing tank are mixed at 45℃×3.0 hours. The mixed liquid material is finely filtered, and the end sensor combination 24-1 controls the solid impurities in the liquid material to a diameter of <0.8µm and then inputs it into the feed port 21, passes through the material mixing chamber 25, turns on the homogenizing pump 26, and the high shear homogenizing rotor 27 is driven by the speed regulating motor 28 to gradually increase the speed to >500 rpm. The mixed material passes through the microchannel reactor 30, the upper and lower manifolds 31-2, 31-1, the static mixer 32 and the single-tube series static mixer group 34, and then returns to the spare 60M through the circulation outlet 36. 3 In the original mixing tank, keep the temperature at 45±1℃ while stirring.
[0024] 12.5 tons of dicyandiamide / isoamyl alcohol mixed liquid with dimethylamine hydrochloride and other proportions are finely filtered. The terminal sensor combination 24-2 controls the solid impurities in the liquid material to a diameter of <0.8µm and then inputs it into the mixed material chamber 25. The high shear homogenizing rotor 27 of the homogenizing pump 26 gradually increases the speed under the drive of the speed regulating stirring motor 28, reaching a speed of >1200 rpm until the terminal sensor combination 24-3 detects and shows that the coupling reaction state can be achieved. The mixed material returns to the spare 30M through the circulation outlet 36 respectively. 3 In the original reactor, the reaction materials were stirred and the temperature was kept at 50±1℃.
[0025] The DCS program control system changes the process, instructing each metering of the dimethylamine hydrochloride mixture and the dicyandiamide mixture of the specified ratio to enter the mixing chamber 25 continuously at the same time; the speed regulating stirring motor 28 drives the high shear homogenizing rotor 27 to increase the speed to >1500 rpm until each material is in the specified coupling reaction state. The reaction materials then enter the SX-type tube bundle static mixer 32, and the heat carrier / cold carrier jacket is passed through ≮1.6MPa main steam to force the temperature of each reaction material with the specified ratio to reach 145±1℃.
[0026] The reaction material then enters the microchannel reactor 30 with an inner diameter of less than 0.8 mm for initial reaction, and then enters the static mixer 32 through the upper manifold 31-2 to continue the temperature-controlled reaction; the heat carrier / cold carrier jacket of the static mixer 32 controls the reaction material to be maintained at 145±1°C for continued forced stirring reaction. Then enter the single-tube series static mixer group 34 (SK-type single tube (length ≮3m)). The temperature of the heat carrier / cold carrier jacket is controlled to keep the reaction material at 145±1°C for continued forced stirring reaction. When the terminal sensor combination 24-3 detects that the dicyandiamide residue in the material is ≯0.1%, it is displayed as qualified after the reaction. The DCS program command opens the solenoid valve 23-7 to export the qualified product outlet 38; otherwise, the program switches to open the solenoid valve 23-6 to export the unqualified product outlet 37.
[0027] After the reaction, qualified products can be injected into the original 10M through the qualified product outlet 38 at a flow rate of ≮10 tons / hour. 3 Conventional reactor with stirring; the reactor is kept in stirring state and vacuumed to <0.09MPa, and the cold carrier jacket is kept at 150℃ to continue distillation to remove most of the water, and then dried on a conveyor belt to obtain metformin hydrochloride in the form of white transparent needle-shaped crystals with a melting point of 223±0.5℃. The yield of the product using this production process can reach more than 95%; the purity can reach more than 99.9%.
[0028] Example 2 is applied to the steam heating concentration production process of crude cystine hydrochloride: Start the DCS computer control program, filter 4 tons of crude cystine hydrochloride aqueous solution (I mother) in the primary neutralization section and then input it into the conventional 5M 3 Enamel reactor. Start the copper-nickel alloy screw pump to output I and then return to the reactor for circulation for ≯20 minutes.
[0029] The program control system changes the process to allow water vapor with a pressure of more than 0.5MPa to enter from the liquid / gas catalyst material inlet 22 after precise filtration; at the same time, the I mother after precise filtration is input into the material inlet 21 by the screw pump at the specified linear speed and enters the mixing chamber 25. The two materials with the specified proportion are forced to be evenly mixed in an instant of ≯0.3s, and then enter the microchannel reactor 30 with an inner diameter of less than 1.0mm for deep coupling. Then it enters the copper-nickel alloy steel tube bundle static mixer 32 to heat up with main steam of less than 1.6MPa, and the temperature of the mixture is kept constant at 122℃±1. The I mother and water vapor mixture then enters the single-tube (length ≮2m) single-tube series static mixer group 34. The temperature of the heat carrier / cold carrier jacket keeps the mixed material at more than 130℃ to continue forced vapor / liquid mixing. After the end sensor combination 24-3 detects that the specified mixing state has been reached, it is sprayed into the conventional 5M standby next to it. 3 Enamel reactor. Maintain ≯120℃ under stirring, slight vacuum <0.08MPa, continue dehydration for ≯3 hours. Stop vacuum and introduce nitrogen protection for ≯3 hours.
[0030] Under abnormal conditions, L-arginine crystals in the mixed material may block the microchannel reactor 30, causing the system pressure to rise suddenly to >0.5MPa. At this time, the control program instructions change the process, close the solenoid valves 23-1, 23-2, 23-5, 23-6, and 23-7, and at the same time, open the solenoid valves 23-3 and 23-4 to backwash the microchannel reactor 30 with >0.5MPa water vapor 22.
[0031] The method can reduce the dehydration time of the aqueous solution (I mother) of crude cystine hydrochloride by more than 18%. When the product L-arginine is post-processed and recrystallized, the crystal transition point stability is improved by more than 30% compared with the original process.
[0032] Example 3, reference Figure 3 A continuous feeding intelligent chemical reaction device, comprising a computer distributed control system DCS, a continuous polymerization reaction device cylinder 39 (with fluorine coating or enamel inside), a speed regulating stirring motor 45, and a high shear homogenizing rotor 42. The speed regulating stirring motor 45 is connected to the high shear homogenizing rotor 42, and the high shear homogenizing rotor 42 is arranged in the continuous polymerization reaction device cylinder 39; the material inlet 40 is connected to the continuous polymerization reaction device cylinder through the terminal sensor combination 47-1 and the electromagnetic valve 48-1, and the catalyst inlet 41 is connected to the continuous polymerization reaction device cylinder through the terminal sensor combination 47-2 and the electromagnetic valve 48-2. The cylinder 39 is connected; the high shear homogenizing rotor 42 is connected through the transmission stirring shaft 44 and the speed regulating stirring motor 45 and is sealed by the dynamic seals 43-1 and 43-2 inside and outside the cylinder 39 of the continuous polymerization reaction device; the outlet of the cylinder 39 of the continuous polymerization reaction device is formed through the terminal sensor combination 47-3, and the outlet includes a qualified product outlet 50 and a non-qualified product outlet 51, each outlet is controlled by its own electromagnetic valve, the qualified product outlet 50 is controlled by the electromagnetic valve 48-3; the non-qualified product outlet 51 is controlled by the electromagnetic valve 48-4; the cylinder of the continuous polymerization reaction device is provided with a heat carrier / cold carrier pipeline 46. The cylinder 39 of the continuous polymerization reaction device is provided with a post-reaction material slurry guide plate 49 (with a poor arc angle of less than 300).
[0033] Example 3 is applied to acrylonitrile polymerization of acrylic fiber in a 3,000-ton / year acrylic fiber production facility in Lanzhou. Start the DCS program control system, use the recovered monomer to circulate through the liquid material inlet 40 times for ≮0.5 hours; acrylonitrile AN and vinyl acetate VAc and the recovered monomer with the specified ratio are forced to stir and mix in the original mixing kettle for ≮3 hours, and a precision filtration cycle is performed at the same time; industrial distilled water, initiator, activator and regulator with the specified ratio are forced to stir and mix in the original mixing kettle for ≮3 hours, and a precision filtration cycle is performed at the same time. After the two mixed components are qualified by the online quality inspection of the DCS link terminal sensor combination 47-1, 47-2, they are simultaneously input into the cylinder 39 of the continuous polymerization reaction device through the pipeline by a metering pump, and are instantly mixed and uniformly through the high-speed, high-polish (Ra<0.1) high-shear homogenizing rotor 42 at a speed of more than 150 rpm to reach a chemical coupling reaction state, and polymerization occurs immediately to form flocculent slurry. The reaction heat is removed by regulating the heat carrier / cold carrier pipeline 46, so that the temperature in the cylinder 39 of the continuous polymerization reaction device is kept at 55°C ± 2. The residual value of the raw material acrylonitrile AN is less than 0.1% in the liquid after the reaction detected by the terminal sensor combination 47-3, which is a compliance indicator. The DCS program control system instructs the solenoid valve 48-3 to open, and the flocculent reaction product is guided by the guide plate 49 to the outlet pipe 50 with the mixed liquid and enters the original stirred liquid slurry tank. Add a reaction terminator to the liquid slurry tank and control the pH value between 4-5. Otherwise, the program control system instructs the solenoid valves 48-1 and 48-2 to stop feeding at the same time. The non-conforming products produced in the early stage of the polymerization reaction are output through the non-conforming product outlet 51 by the program control system instructing the opening of the solenoid valve 48-4.
[0034] The molecular weight distribution of the polyacrylonitrile produced by the present invention is lower than 1.5; the AN / VAc ratio in the raw solution participating in the reaction is increased to more than 30%.
[0035] The static mixer in Example 1-2 can be a SK type static mixer with adjustable length according to different working conditions such as reaction temperature, pressure, etc. The positions of the static mixer and the microchannel reactor can be adjusted according to different positions of the reaction materials.
Claims
1. A continuous feeding intelligent chemical reaction device, comprising a computer distributed control system DCS, a material mixing chamber, a speed regulating stirring motor, and a high shear homogenizing rotor, wherein the speed regulating stirring motor is connected to the high shear homogenizing rotor, and the high shear homogenizing rotor is arranged in the material mixing chamber; characterized in that: The material inlet is connected with the material mixing chamber through the solenoid valve, the extrusion filter, the ultrafilter, the terminal sensor combination, the solenoid valve and the material mixing chamber in sequence; the catalyst inlet is connected with the solenoid valve, the extrusion filter, the ultrafilter, the terminal sensor combination, the mixing chamber pipeline, the solenoid valve and the material mixing chamber in sequence; the nitrogen replacement inlet is connected with the solenoid valve, the extrusion filter, the ultrafilter, the terminal sensor combination, the mixing chamber pipeline, the solenoid valve and the material mixing chamber in sequence; the material mixing chamber outlet is connected with the microchannel reactor, the static mixer, the reaction material manifold, the terminal sensor combination, the relay extrusion gear pump, the single tube static mixer and the terminal sensor combination in sequence to form an outlet; the outlet includes a circulation outlet, a qualified product outlet and a non-qualified product outlet, and each outlet is controlled by its own solenoid valve; a heat carrier / cold carrier jacket is arranged on the periphery of the static mixer; the solenoid valve, the terminal sensor combination, the relay extrusion gear pump and the speed regulating stirring motor are all electrically connected to the computer distributed control system DCS.
2. A continuous feeding intelligent chemical reaction device according to claim 1, characterized in that: It includes a flushing mechanism, wherein the outlet end of the reaction material manifold is connected to the flushing material inlet through a solenoid valve, and the liquid material mixing chamber is connected to the flushing material outlet through a two-stage solenoid valve; a solenoid valve is arranged between the solenoid valve in front of the flushing material outlet and the outlet end of the reaction material manifold; the solenoid valve is electrically connected to a computer distributed control system DCS.
3. A continuous feeding intelligent chemical reaction device, comprising a computer distributed control system DCS, a material mixing chamber, a speed regulating stirring motor, and a high shear homogenizing rotor, wherein the speed regulating stirring motor is connected to the high shear homogenizing rotor, and the high shear homogenizing rotor is arranged in the liquid material mixing chamber; characterized in that: The material inlet is connected through the terminal sensor combination, the electromagnetic valve and the material mixing chamber; the liquid / gas catalyst material inlet is divided into two routes, one route is connected to the material mixing chamber after passing through the terminal sensor combination and the electromagnetic valve; the other route is a backwashing mechanism, the liquid / gas catalyst material inlet is connected to the upper buffer manifold through the electromagnetic valve, and the lower buffer manifold is connected to the backwashing residual liquid outlet through the electromagnetic valve; a microchannel reactor is arranged between the upper buffer manifold and the lower buffer manifold; the upper buffer manifold forms an outlet through a static mixer, a single-tube series static mixer group and a terminal sensor, and the outlet includes a circulation outlet, a qualified product outlet and a non-qualified product outlet, and each outlet is controlled by its own electromagnetic valve; the lower buffer manifold is connected to the material mixing chamber; the static mixer and the single-tube series static mixer group are both provided with a heat carrier / cold carrier jacket on their peripheries; the electromagnetic valve, the terminal sensor combination and the speed regulating stirring motor are all electrically connected to a computer distributed control system DCS.
4. A continuous feeding intelligent chemical reaction device according to claim 1 or 2, characterized in that: The static mixer is an SK type static mixer with adjustable length.
5. A continuous feeding intelligent chemical reaction device according to claim 1 or 2, characterized in that: The positions of the static mixer and the microchannel reactor are adjustable.
6. A continuous feeding intelligent chemical reaction device, comprising a computer distributed control system DCS, a material mixing chamber, a speed regulating stirring motor, and a high shear homogenizing rotor, wherein the speed regulating stirring motor is connected to the high shear homogenizing rotor, and the high shear homogenizing rotor is arranged in the cylinder of the continuous polymerization reaction device; characterized in that: The material inlet is connected to the cylinder of the continuous polymerization reaction device through the terminal sensor combination and the solenoid valve, and the catalyst inlet is connected to the cylinder of the continuous polymerization reaction device through the terminal sensor combination and the solenoid valve; the high shear homogenization rotor is sealed by a dynamic seal; the outlet of the cylinder of the continuous polymerization reaction device is formed by the terminal sensor combination, and the outlet includes an outlet for qualified products and an outlet for unqualified products, and each outlet is controlled by its own solenoid valve; a heat carrier / cold carrier pipeline is provided in the cylinder of the continuous polymerization reaction device.