Sulfentrazone nitration apparatus

Abstract

The utility model relates to the technical field of mesosulfuron-methyl synthesis, and particularly discloses a mesosulfuron-methyl nitration reaction device, which comprises a reaction kettle, a feed inlet and a waste gas outlet are arranged on the top of the reaction kettle, a discharge port is arranged at the bottom of the reaction kettle, and a detachable sealing cover is installed on the discharge port through a threaded connection mode; a spiral propelling type stirrer is vertically arranged in the reaction kettle, the spiral propelling type stirrer comprises a stirring shaft and spiral blades that are continuously distributed along the stirring shaft from top to bottom, the distance between the outer edge of the spiral blade and the inner wall of the reaction kettle is 5-8 mm, a polytetrafluoroethylene coating with a thickness of 0.2-0.5 mm is coated on the surface of the spiral blade, and a motor is coaxially and fixedly connected to the driving stirring shaft on the top of the reaction kettle; through the cooperation of the spiral propelling type stirrer and the polytetrafluoroethylene coating, the gradient temperature control of the multi-stage variable-diameter cooling coil, the precise distribution of the 40-degree inclined atomizing nozzle, and the synergistic design of the pH closed-loop discharge control, the nitration reaction efficiency and the product purity are significantly improved.

Description

Technical Field

[0001] This utility model relates to the field of metsulfuron-methyl synthesis technology, and specifically discloses a metsulfuron-methyl nitration reaction apparatus. Background Technology

[0002] In the production process of mesotrione, nitration is one of the key steps.

[0003] Traditional nitration reactors have many problems, such as uneven stirring leading to low reaction efficiency, inaccurate temperature control affecting reaction results, unreasonable distribution of nitrifying agent resulting in incomplete reaction, and inadequate waste gas treatment causing resource waste and environmental pollution.

[0004] To address these issues and improve the efficiency, quality, and safety of the metolachlor nitrification reaction, this metolachlor nitrification reaction apparatus was designed. Utility Model Content

[0005] This utility model proposes a metolachlor nitrification reaction device. Through optimized structural design of stirring, temperature control, nitrifying agent distribution, waste gas treatment and discharge control, the metolachlor nitrification reaction device achieves multiple beneficial effects such as improving reaction efficiency, precise temperature control, reducing material waste and environmental pollution, ensuring product quality and enhancing equipment durability.

[0006] This utility model is implemented as follows: a metolachlor nitrification reaction device includes: a reaction vessel, the top of which is provided with a feed inlet and a waste gas outlet, and the bottom of which is provided with a discharge outlet, the discharge outlet being fitted with a removable sealing cap by a threaded connection;

[0007] A helical propulsion stirrer is vertically installed inside the reactor. The helical propulsion stirrer includes a stirring shaft and helical blades continuously distributed from top to bottom along the stirring shaft. The distance between the outer edge of the helical blades and the inner wall of the reactor is 5-8 mm. The surface of the helical blades is covered with a 0.2-0.5 mm thick polytetrafluoroethylene coating. A motor is installed at the top of the reactor and is coaxially fixed to the driving stirring shaft.

[0008] A temperature control system, comprising a heating jacket covering the outer wall of the reactor, a heating resistance wire spirally embedded in the heating jacket, and a thermocouple disposed in the middle of the inner wall of the reactor;

[0009] Multi-stage cooling coils are arranged around the inner wall of the reactor, and each stage of the cooling coil is independently connected to an external refrigerant control system;

[0010] A nitrifying agent distributor is fixed to the upper part of the reactor, and the lower end of the nitrifying agent distributor is provided with uniformly distributed atomizing nozzles;

[0011] A condensation reflux device is connected to the exhaust gas outlet pipe;

[0012] The inner wall of the discharge port is equipped with an online pH meter, and the end of the discharge port is equipped with an electric shut-off valve that is linked to the online pH meter.

[0013] As a preferred embodiment of the metolachlor nitrification reaction device of this utility model, the multi-stage cooling coils are arranged in a total of 4 stages, and the vertical spacing between adjacent cooling coils from top to bottom is 15cm, 12cm, 8cm and 5cm respectively, and the pipe diameter increases stepwise to Φ10mm, Φ12mm, Φ15mm and Φ18mm. The refrigerant inlet / outlet of each stage of the cooling coil is connected to the external pipeline through a rotary sealing joint.

[0014] As a preferred embodiment of the metolachlor nitrification reaction apparatus of this utility model, the nitrifying agent distributor includes an annular main pipe horizontally fixed to the inner wall of the top of the reactor, branch pipes evenly distributed along the circumference of the annular main pipe, and atomizing nozzles inclinedly connected to the ends of each branch pipe. The axis of the atomizing nozzles forms a 40° angle with the horizontal plane, and the spray trajectories of all the atomizing nozzles converge at the central axis of the reactor. An anti-clogging filter screen is provided at the inlet of the annular main pipe, and the mesh size of the anti-clogging filter screen is 0.5-1mm.

[0015] As a preferred embodiment of the metolachlor nitrification reaction apparatus of this invention, the inner wall of the reactor is lined with an enamel layer of 2-3 mm thickness.

[0016] In a preferred embodiment of the metolachlor nitrification reaction apparatus of this utility model, the condensation reflux device includes a condenser and a gas-liquid separator. The condenser is connected to the exhaust gas outlet pipe via a flange. The inlet of the gas-liquid separator is connected to the outlet of the condenser via a quick-connect clamp. The gas outlet of the gas-liquid separator is connected to the tail gas treatment system, and the liquid outlet is returned to the reaction vessel via a reflux pipe.

[0017] In a preferred embodiment of the metolachlor nitrification reaction apparatus of this invention, the probe of the online pH meter is embedded in the inner wall of the discharge port through a threaded sealing joint, and the electric shut-off valve is connected to the probe signal to form a closed-loop control.

[0018] In a preferred embodiment of the metolachlor nitrification reaction apparatus of this invention, the heating resistance wire is evenly distributed in a spiral shape inside the heating jacket and forms a PID temperature control circuit with the thermocouple.

[0019] The beneficial effects of this utility model are:

[0020] 1. The spiral propeller agitator can fully mix the materials, and the nitrifying agent distributor can evenly disperse the nitrifying agent, promoting full contact between the materials and the nitrifying agent, effectively improving the efficiency of the nitration reaction. In addition, the inner wall of the reactor is lined with an enamel layer, and the surface of the spiral blades is coated with polytetrafluoroethylene, which can effectively prevent the equipment from being corroded and extend the service life of the equipment. The anti-clogging filter at the inlet of the nitrifying agent distributor can prevent impurities from entering and ensure the normal operation of the equipment.

[0021] 2. The temperature control system, through a PID temperature control loop and multi-stage cooling coils, can achieve precise adjustment and control of the reaction temperature, avoiding the impact of excessively high or low temperatures on the reaction effect and ensuring the quality and stability of the reaction.

[0022] 3. The condensation and reflux device condenses and refluxes the recyclable substances in the waste gas generated by the reaction back into the reactor, reducing material waste; at the same time, the gas after gas-liquid separation enters the tail gas treatment system, reducing environmental pollution.

[0023] 4. The pH online detector is linked with the electric shut-off valve to monitor the pH value of the discharged material in real time, ensuring that only materials that meet the set standards can be discharged, effectively guaranteeing product quality. Attached Figure Description

[0024] To more clearly illustrate the specific embodiments of this utility model or the technical solutions in the prior art, the drawings used in the description of the specific embodiments or the prior art will be briefly introduced below. In all the drawings, similar elements or parts are generally identified by similar reference numerals. In the drawings, the elements or parts are not necessarily drawn to scale.

[0025] Figure 1 This is a schematic diagram of the overall structure of this utility model.

[0026] Figure 2 This is a cross-sectional structural diagram of the spiral blade and polytetrafluoroethylene coating of this utility model.

[0027] Figure 3 This is a top view of the nitrifying agent distributor of this utility model.

[0028] Figure 4 This is a cross-sectional structural diagram of the reaction vessel and enamel layer of this utility model.

[0029] The markings in the diagram are as follows: 1. Reactor; 2. Feed inlet; 3. Exhaust gas outlet; 4. Discharge outlet; 5. Sealing cap; 6. Stirring shaft; 7. Spiral blades; 8. PTFE coating; 9. Motor; 10. Heating jacket; 11. Heating resistance wire; 12. Thermocouple; 13. Cooling coil; 14. Nitrating agent distributor; 15. Atomizing nozzle; 16. Online pH meter; 17. Electric shut-off valve; 18. Circular main pipe; 19. Diversion branch pipe; 20. Anti-clogging filter; 21. Enamel layer; 22. Condenser; 23. Gas-liquid separator; 24. Tail gas treatment system. Detailed Implementation

[0030] The present invention will be further described below with reference to the accompanying drawings and specific embodiments to aid in understanding its content. Unless otherwise specified, the methods used in this invention are conventional methods; the raw materials and apparatus used, unless otherwise specified, are conventional commercially available products.

[0031] Please see Figure 1-4 The metolachlor nitrification reaction unit includes:

[0032] The reactor 1 has a feed inlet 2 and an exhaust outlet 3 at the top and a discharge outlet 4 at the bottom. The discharge outlet 4 is fitted with a removable sealing cover 5 via a threaded connection.

[0033] A spiral propulsion agitator is vertically installed inside the reactor 1. The spiral propulsion agitator includes a stirring shaft 6 and spiral blades 7 continuously distributed from top to bottom along the stirring shaft 6. The distance between the outer edge of the spiral blades 7 and the inner wall of the reactor 1 is 5-8 mm. The surface of the spiral blades 7 is covered with a 0.2-0.5 mm thick polytetrafluoroethylene coating 8. A motor 9 is installed at the top of the reactor 1 and is coaxially fixed to the driving stirring shaft 6.

[0034] The temperature control system includes a heating jacket 10 covering the outer wall of the reactor 1, a heating resistance wire 11 spirally embedded in the heating jacket 10, and a thermocouple 12 located in the middle of the inner wall of the reactor 1.

[0035] Multi-stage cooling coils 13 are arranged around the inner wall of the reactor 1, and each stage of cooling coil 13 is independently connected to an external refrigerant control system.

[0036] The nitrifying agent distributor 14 is fixed to the upper part of the reactor 1, and the lower end of the nitrifying agent distributor 14 is provided with uniformly distributed atomizing nozzles 15.

[0037] A condenser reflux device is connected to the exhaust gas outlet pipe 3.

[0038] A pH online detector 16 is installed on the inner wall of the discharge port 4, and an electric shut-off valve 17 that is linked to the pH online detector 16 is installed at the end of the discharge port 4.

[0039] In this embodiment: the material enters the reactor 1 through the feed inlet 2 at the top of the reactor 1. Driven by the motor 9, the spiral propeller agitator rotates the spiral blades 7 using the stirring shaft 6 to agitate the material. The distance between the outer edge of the blades and the inner wall of the reactor 1 is small, and the surface is coated with polytetrafluoroethylene 8, which can effectively prevent material adhesion and achieve thorough agitation, promoting uniform mixing of the material. The thermocouple 12 in the temperature control system monitors the temperature in the middle of the reactor 1 in real time and feeds the temperature signal back to the control system. The heating resistance wire 11 is spirally embedded in the heating jacket 10. Based on the feedback signal from the thermocouple 12, it forms a PID temperature control loop with the thermocouple 12 to automatically adjust the heating power and heat the reactor 1 through the heating jacket 10. The multi-stage cooling coil 13 is arranged around the inner wall of the reactor 1. Each stage is independently connected to the external refrigerant control system, which can adjust the refrigerant flow according to the reaction requirements to achieve precise temperature control and ensure that the reaction is carried out at a suitable temperature.

[0040] The nitrifying agent distributor 14 is fixed to the upper part of the reactor 1. The nitrifying agent is sprayed out through the annular main pipe 18 and the branch pipe 19, and then through the atomizing nozzle 15 with its end set at an angle. The axis of the nozzle forms a 40° angle with the horizontal plane, and the spray trajectories of all nozzles converge at the central axis of the reactor 1, so that the nitrifying agent is evenly distributed in the reactor 1 and fully contacts the material, thereby improving the reaction efficiency. The waste gas generated by the reaction is discharged from the waste gas outlet 3. It is first condensed by the condenser 22 to convert the condensable substances into liquid, and then enters the gas-liquid separator 23 to achieve gas-liquid separation. The separated gas enters the tail gas treatment system 24, and the liquid is returned to the reactor 1 through the return pipe, reducing material waste and environmental pollution. After the reaction is completed, the pH online detector 16 on the inner wall of the discharge port 4 monitors the pH value of the material in real time. When the pH value reaches the set standard, the electric shut-off valve 17 is opened, and the material is discharged from the discharge port 4. If the pH value does not meet the standard, the electric shut-off valve 17 is closed, and the reaction continues to ensure the quality of the discharged product.

[0041] As a technical optimization of this utility model, the multi-stage cooling coil 13 is provided in four stages. The vertical spacing between adjacent cooling coils 13 from top to bottom is 15cm, 12cm, 8cm and 5cm respectively, and the pipe diameter increases step by step to Φ10mm, Φ12mm, Φ15mm and Φ18mm. The refrigerant inlet / outlet of each stage of cooling coil 13 is connected to the external pipeline through a rotary sealing joint.

[0042] In this embodiment, the specific settings of the multi-stage cooling coil 13 (number of stages, vertical spacing, and pipe diameter variation) can more rationally allocate cooling capacity according to the heat changes at different locations and stages during the reaction process, thereby further improving the accuracy and effectiveness of temperature control.

[0043] As a technical optimization of this utility model, the nitrifying agent distributor 14 includes an annular main pipe 18 horizontally fixed to the inner wall of the top of the reactor 1, branch pipes 19 evenly distributed around the annular main pipe 18, and atomizing nozzles 15 inclinedly connected to the ends of each branch pipe 19. The axis of the atomizing nozzle 15 forms a 40° angle with the horizontal plane, and the spray trajectories of all atomizing nozzles 15 converge at the central axis of the reactor 1. An anti-clogging filter screen 20 is provided at the inlet of the annular main pipe 18, and the mesh size of the anti-clogging filter screen 20 is 0.5-1mm.

[0044] In this embodiment, the structural design of the nitrifying agent distributor 14 (annular main pipe 18, branch pipe 19, atomizing nozzle 15 angle and spray trajectory) enables the nitrifying agent to be evenly and centrally distributed in the reactor 1, ensuring full contact between the nitrifying agent and the material, and improving reaction efficiency and effect; the anti-clogging filter 20 can prevent impurities from entering and ensure normal operation of the equipment (the nitrifying agent is a mixed solution of concentrated nitric acid and sulfuric acid).

[0045] As a technical optimization of this utility model, the inner wall of the reactor 1 is lined with an enamel layer 21 with a thickness of 2-3 mm.

[0046] In this embodiment, the enamel layer 21 on the inner wall of the reactor 1 can effectively prevent the reactor 1 from being corroded, extend the service life of the equipment, and at the same time ensure the safety and stability of the reaction process.

[0047] As a technical optimization of this utility model, the condensation reflux device includes a condenser 22 and a gas-liquid separator 23. The condenser 22 is connected to the pipe of the exhaust gas outlet 3 through a flange. The inlet of the gas-liquid separator 23 is connected to the outlet of the condenser 22 through a quick-connect clamp. The gas outlet of the gas-liquid separator 23 is connected to the tail gas treatment system 24, and the liquid outlet is returned to the reactor 1 through a reflux pipe.

[0048] In this embodiment: the condenser 22 and the gas-liquid separator 23 of the condensation reflux device work together to achieve effective treatment of waste gas. The condenser 22 liquefies condensable substances, the gas-liquid separator 23 achieves gas-liquid separation, liquid reflux reduces material waste, and the gas passes through the tail gas treatment system 24 to reduce environmental pollution. A one-way valve is provided on the reflux pipe to prevent material backflow.

[0049] As a technical optimization of this utility model, the probe of the pH online detector 16 is embedded in the inner wall of the outlet 4 through a threaded sealing joint, and the electric shut-off valve 17 is connected to the probe signal to form a closed-loop control.

[0050] In this embodiment: the pH online detector 16 probe is embedded in the inner wall of the discharge port 4, which can accurately monitor the pH value of the material; it is connected to the electric shut-off valve 17 to form a closed-loop control, which can automatically control the discharge according to the pH value to ensure product quality.

[0051] As a technical optimization of this utility model, the heating resistance wire 11 is evenly distributed in a spiral shape inside the heating jacket 10, and forms a PID temperature control circuit with the thermocouple 12.

[0052] In this embodiment, the heating resistance wire 11 is spirally and uniformly distributed in the heating jacket 10 and forms a PID temperature control circuit with the thermocouple 12, which can realize precise control of the reaction temperature, automatically adjust the heating power according to the reaction requirements, maintain the reaction temperature stability, and improve the reaction quality and stability.

[0053] Working principle and usage process of this utility model:

[0054] First, mesotrione and related materials are fed into reactor 1 through the feed inlet 2 at the top of reactor 1; the motor 9 is started to drive the spiral propeller agitator to mix the materials; the temperature control system starts working, the thermocouple 12 monitors the temperature inside reactor 1 in real time, and the heating resistance wire 11 and multi-stage cooling coil 13 automatically adjust according to the temperature to maintain a stable reaction temperature; the nitrifying agent is evenly sprayed into reactor 1 through the annular main pipe 18 and the branch pipe 19 of the nitrifying agent distributor 14 and the atomizing nozzle 15, mixing with the materials. The material comes into contact with the reactor and undergoes a nitration reaction. The waste gas generated during the reaction is discharged from the waste gas outlet 3 and passes through the condenser 22 and the gas-liquid separator 23 in sequence for condensation and gas-liquid separation. The liquid flows back to the reactor 1 and the gas enters the tail gas treatment system 24. When the reaction is nearing completion, the pH value of the material on the inner wall of the discharge port 4 is monitored in real time by the pH online detector. When the pH value reaches the set standard, the electric shut-off valve 17 is opened and the material is discharged from the discharge port 4. If the pH value does not reach the standard, the electric shut-off valve 17 is closed and the reaction continues until the pH value is qualified.

[0055] In the description of this utility model, it should be understood that the terms "left", "right", "up", "down", "top", "bottom", "front", "back", "inner", "outer", "back", "middle", etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are only for the convenience of describing this utility model and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on this utility model.

[0056] However, the above are merely specific embodiments of this utility model and should not be construed as limiting the scope of implementation of this utility model. Therefore, any substitution of equivalent components or equivalent changes and modifications made in accordance with the scope of protection of this utility model should still fall within the scope of the claims of this utility model.

Claims

1. A metsulfuron-methyl nitrification reaction apparatus, characterized in that, include: The reactor (1) has a feed inlet (2) and an exhaust outlet (3) at the top and a discharge outlet (4) at the bottom. The discharge outlet (4) is fitted with a removable sealing cap (5) by a threaded connection. A spiral propulsion stirrer is vertically installed inside the reactor (1). The spiral propulsion stirrer includes a stirring shaft (6) and spiral blades (7) continuously distributed from top to bottom along the stirring shaft (6). The distance between the outer edge of the spiral blades (7) and the inner wall of the reactor (1) is 5-8 mm. The surface of the spiral blades (7) is covered with a 0.2-0.5 mm thick polytetrafluoroethylene coating (8). The top of the reactor (1) is equipped with a motor (9) that is coaxially fixed to the driving stirring shaft (6). The temperature control system includes a heating jacket (10) covering the outer wall of the reactor (1), a heating resistance wire (11) spirally embedded in the heating jacket (10), and a thermocouple (12) disposed in the middle of the inner wall of the reactor (1). Multi-stage cooling coils (13) are arranged around the inner wall of the reactor (1), and each stage of the cooling coils (13) is independently connected to an external refrigerant control system; Nitrifying agent distributor (14) is fixed on the upper part of the reactor (1), and the lower end of the nitrifying agent distributor (14) is provided with uniformly distributed atomizing nozzles (15); A condensation reflux device is connected to the exhaust gas outlet (3) pipe; The inner wall of the outlet (4) is provided with an online pH detector (16), and the end of the outlet (4) is provided with an electric shut-off valve (17) that is linked to the online pH detector (16).

2. The metolachlor nitrification reactor according to claim 1, characterized in that: The multi-stage cooling coil (13) is provided in 4 stages. The vertical spacing between adjacent cooling coils (13) from top to bottom is 15cm, 12cm, 8cm and 5cm respectively, and the pipe diameter increases step by step to Φ10mm, Φ12mm, Φ15mm and Φ18mm. The refrigerant inlet / outlet of each stage of the cooling coil (13) is connected to the external pipeline through a rotary sealing joint.

3. The metsulfuron-methyl nitrification reaction apparatus according to claim 1, characterized in that: The nitrifying agent distributor (14) includes an annular main pipe (18) horizontally fixed to the inner wall of the top of the reactor (1), branch pipes (19) evenly distributed around the annular main pipe (18), and atomizing nozzles (15) inclinedly connected to the ends of each branch pipe (19). The axis of the atomizing nozzle (15) forms a 40° angle with the horizontal plane, and the spray trajectories of all the atomizing nozzles (15) converge at the central axis of the reactor (1). An anti-clogging filter (20) is provided at the inlet of the annular main pipe (18), and the mesh size of the anti-clogging filter (20) is 0.5-1mm.

4. The metsulfuron-methyl nitrification reaction apparatus according to claim 1, characterized in that: The inner wall of the reactor (1) is lined with a 2-3 mm thick enamel layer (21).

5. The metsulfuron-methyl nitrification reaction apparatus according to claim 1, characterized in that: The condensation reflux device includes a condenser (22) and a gas-liquid separator (23). The condenser (22) is connected to the pipe of the exhaust gas outlet (3) through a flange. The inlet of the gas-liquid separator (23) is connected to the outlet of the condenser (22) through a quick-connect clamp. The gas outlet of the gas-liquid separator (23) is connected to the tail gas treatment system (24), and the liquid outlet is returned to the reactor (1) through a reflux pipe.

6. The metsulfuron-methyl nitrification reaction apparatus according to claim 1, characterized in that: The probe of the pH online detector (16) is embedded in the inner wall of the outlet (4) through a threaded sealing joint, and the electric shut-off valve (17) is connected to the probe signal to form a closed-loop control.

7. The metsulfuron-methyl nitrification reaction apparatus according to claim 1, characterized in that: The heating resistance wire (11) is evenly distributed in a spiral shape inside the heating jacket (10), and forms a PID temperature control circuit with the thermocouple (12).

Images