Parafluorotoluene automated production line
By designing a p-fluorotoluene automated production line and using frozen crystallization technology for moisture separation, the problem of lack of automated control and low moisture separation efficiency of p-fluorotoluene production line in the existing technology is solved, and an efficient and economical production process is achieved.
Patent Information
- Application Number
- CN202411754754.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-03
- Publication Date
- 2025-03-04
- Estimated Expiration
- 2044-12-03
AI Technical Summary
The existing p-fluorotoluene production line lacks automated control, resulting in difficult temperature control during the reaction process, uneven material addition, and low moisture separation efficiency, which increases production and time costs.
An automated production line of parafluorotoluene is designed, including a salt-forming processing area, a diazotization processing area, a thermal decomposition processing area, a water-washing neutralization area and a distillation area, and is equipped with an automated control system. The moisture is separated by freezing crystallization technology, and the amount of steam required for distillation is reduced by crushing the ice crystals to collect the p-fluorotoluene liquid.
It improves the degree of automation of the parafluorotoluene production process, reduces manual intervention and safety accidents, reduces production costs and time costs, and improves production efficiency and economic benefits.
Smart Images

Figure CN119236832B_ABST
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of production and processing of p-fluorotoluene, and in particular relates to an automated production line for p-fluorotoluene. Background Art
[0002] Parafluorotoluene is an important organic fluoride that is widely used in medicine, pesticides, dyes, fluoroplastics and other fields.
[0003] At present, the preparation method of p-fluorotoluene includes the following steps: 1. Salt-forming step: anhydrous hydrofluoric acid and p-toluidine are mixed, and a mixture ① is prepared after reaction; 2. Diazotization step: sodium nitrite is added to the mixture ①, and a mixture ② is prepared after reaction; 3. Thermal decomposition step: the mixture ② is heated and decomposed; 4. Water washing and neutralization: the product obtained after thermal decomposition is allowed to stand for stratification, the upper layer of crude p-fluorotoluene is collected for water washing, and the lower layer of wastewater solution is discarded for neutralization; 5. Distillation: the crude p-fluorotoluene after water washing and neutralization is subjected to steam distillation and atmospheric distillation respectively, and the obtained fractions are the p-fluorotoluene finished product.
[0004] The above-mentioned preparation method has the following disadvantages: the reaction process in each of the above-mentioned steps needs to be temperature controlled, and the addition amount of each material has a certain ratio. Considering that there is a certain connection between the addition of materials and their reaction time, in the prior art, for example, the addition of aniline materials and sodium nitrite materials needs to be uniformly added dropwise within ten hours, which requires that the material inventory and its feed rate are related. In the conventional p-fluorotoluene production line, there is often a lack of control over these processing procedures, and the automated production process is limited. In addition, in step 4, after the crude p-fluorotoluene is washed with water for many times, the product contains a large amount of water. When p-fluorotoluene is refined, step 5 is often used to carry out distillation to remove the water. However, directly distilling the crude p-fluorotoluene will consume a large amount of steam, increase time cost, and the refining time is long, consuming relatively high time cost, consuming a lot of resources, affecting the production efficiency in the factory, and unable to meet the use requirements of production and processing. Summary of the invention
[0005] In view of the technical problems existing in the production process of p-fluorotoluene mentioned above, the present invention proposes a method with reasonable design, simple structure, convenient processing and supporting automatic control system installed in the production and processing process of p-fluorotoluene, which can reduce labor costs to a certain extent, reduce production safety accidents, improve production efficiency, and ensure the economic benefits of production and processing in the factory. At the same time, the water in the p-fluorotoluene is frozen and crystallized to discharge the p-fluorotoluene to complete the water separation, especially to fully crush the p-fluorotoluene retained in the crystals, and make the p-fluorotoluene liquid fall and be exported, and the frozen crystals can also flow back to the production line, which plays a role in saving production costs and effectively meets the use requirements of the p-fluorotoluene automatic production line.
[0006] In order to achieve the above-mentioned purpose, the technical solution adopted by the present invention is an automated production line for parafluorotoluene, comprising a salt-forming processing area, a diazotization processing area, a thermal decomposition processing area, a water washing and neutralization area and a distillation area sequentially arranged along the parafluorotoluene production line, the salt-forming processing area comprising a salt-forming kettle with a stirring function, a coil refrigeration temperature adjustment group is arranged on the outside of the salt-forming kettle, an aniline metering tank with a weighing and metering module is arranged on one side of the salt-forming kettle, and is connected to the salt-forming kettle, a first metering control system is arranged on the outside of the weighing and metering module of the aniline metering tank, the diazotization processing area comprises a diazotization kettle with a temperature display component and a temperature adjustment function, a sodium nitrite metering silo with a gas metering component is arranged above the diazotization kettle, and the nitrite metering silo is provided with a sodium nitrite metering silo. A sodium nitrite gas delivery system is provided at the feed inlet of the sodium acid metering silo, a second metering control system is provided outside the gas metering component of the sodium nitrite metering silo, the thermal decomposition processing area includes thermal decomposition tanks R1-R4 with heating function and arranged in sequence, a temperature rise control system is provided on one side of the thermal decomposition processing area, the water washing and neutralization area includes a static separation tank for receiving the crude para-fluorotoluene product to achieve static stratification, a water washing tank is provided on one side of the static separation tank, a moisture separation tank for pre-treating the crude para-fluorotoluene after water washing is provided on one side of the water washing tank, the distillation area includes a distillation tower for receiving the material exported from the moisture separation tank, and a distillation supply group for heat supply is provided on one side of the distillation tower.
[0007] Preferably, the output control end of the first metering control system is respectively connected to the feed regulating valve of the coil refrigeration temperature control group and the discharge regulating valve of the aniline metering tank, the signal end of the second metering control system is connected to the temperature display component of the diazotization kettle, and the output end of the second metering control system is connected to the feed regulating valve of the sodium nitrite metering silo of the diazotization kettle.
[0008] Preferably, the moisture separation tank includes a tank body designed in an M shape, the tank body includes a freezing tank body and an ice crystal treatment tank body designed in an arc shape and arranged in a mirror image with respect to the freezing tank body, support frames are arranged below the freezing tank body and the ice crystal treatment tank body, a coil freezing assembly is arranged on the periphery of the freezing tank body, a drive shaft is arranged inside the freezing tank body, a material transfer assembly, a conveying assembly and an ice breaking assembly are arranged on the outside of the drive shaft from top to bottom, a partition is arranged above the freezing tank body, a driving gear is arranged on the outside of the drive shaft above the partition, two symmetrically arranged driven gears are arranged on the outside of the driving gear, an adjusting screw is arranged inside the driven gear, a lifting plate is arranged on the outside below the two adjusting screws, and a plurality of one-way valves are evenly distributed inside the lifting plate.
[0009] Preferably, the material shifting assembly includes a mounting frame connected to the driving shaft, a horizontal frame is arranged on the outer sides of the upper and lower mounting frames, a vertical plate is arranged between the two horizontal frames, and the conveying assembly includes a sleeve connected to the driving shaft, and an auger blade is arranged on the outer periphery of the sleeve.
[0010] Preferably, the ice-breaking assembly includes a ring disk, a carrying disk is arranged below the ring disk, a mounting disk is arranged at the geometric center of the carrying disk, a rotating blade is arranged below the mounting disk, a rotating disk is arranged on the outer side of the mounting disk, an arc groove is opened in the rotating disk, a key groove is opened in the carrying disk, a moving rod is arranged in the key groove and matched with the arc groove, a breaking tooth is arranged below the moving rod, an adjusting groove is arranged on one side of the ring disk, an adjusting rod is arranged in the adjusting groove and connected to the rotating disk, and a locking bolt is arranged above the ring disk.
[0011] Preferably, the one-way valve includes a valve sleeve with an L-shaped cross-section, a limiting sleeve is arranged at the bottom of the valve sleeve, and a valve body with a double-conical shape is arranged in the valve sleeve above the limiting sleeve, the taper and height of the lower half of the valve body are greater than the taper and height of the upper half, and a limiting plate is arranged on the outside of the valve body, the outer side of the limiting plate is designed in a stepped shape, and the top of the limiting plate is adapted to the inner diameter of the valve sleeve.
[0012] Preferably, the ice crystal processing tank body is provided with a rotating shaft running through it, a toggle rod is provided on the lower outer side of the rotating shaft, a loading tray with a flying saucer shape is provided at the lower part of the ice crystal processing tank body, a cleaning assembly is provided above the loading tray, and discharge ports are staggered up and down in the ice crystal processing tank body on both sides of the lower end of the loading tray, a drainage hood with a right-angled trapezoidal cross-section is provided on the periphery of the ice crystal processing tank body located outside the discharge port, a collecting hood with a conical table shape is provided below the drainage hood, a drain pipe is provided below the collecting hood, and a sealing plate that can realize vertical lifting and lowering is provided on the drainage hood, and corresponds to the discharge port located above.
[0013] Preferably, the cleaning assembly includes a rotating rod connected to the loading tray, the rotating rod is provided with an arc rod on one side of the rotating rod, a vertical rod is provided on the lower outer side of the arc plate, a material-discharging plate designed in a chain concave shape is provided on the inner side of the arc plate, and a cover body designed in a hollow L shape is provided on the other side of the rotating rod, one end face of the cover body is designed in an arc shape and is adapted to the outer periphery of the loading tray, a plurality of vertical plates are evenly distributed in the cover body, and the cover body is divided into a plurality of cleaning areas, a lifting rod is provided on the cover body, a cleaning plate is provided at the lower end of the lifting rod, a key-shaped plate is provided on the outer periphery of the lifting rod, a fixing rod is provided on the cover body and passes through the key-shaped plate, a spring is provided on the outer periphery of the fixing rod located between the cover body and the key-shaped plate, and a wedge-shaped stop block is provided above the lifting rod.
[0014] Preferably, a production method of a p-fluorotoluene automated production line, using the p-fluorotoluene automated production line, comprises the following steps:
[0015] S1: Salt-forming step: anhydrous hydrofluoric acid is transported to the salt-forming kettle, and the aniline metering tank is opened to uniformly add the aniline to the salt-forming kettle, and the reaction temperature is adjusted and the reaction time is controlled to fully react to obtain a mixture ①;
[0016] Among them, in step S1: the weighing and metering module in the aniline metering tank weighs the aniline material in real time, and feeds back the remaining material weight information to the first metering control system. According to the setting of the reaction temperature and reaction time in the salt-forming step by the first metering control system, its output control end acts on the feed regulating valve of the coil refrigeration temperature control group and the feed regulating valve of the aniline metering tank respectively, so as to realize the automatic control of the reaction temperature and reaction time;
[0017] S2: Diazotization step: input the mixture ① into the diazotization kettle, open the sodium nitrite metering bin, add all the materials to the diazotization kettle at a uniform speed, control the reaction temperature and reaction time, and obtain the mixture ② after sufficient reaction;
[0018] Wherein, in step S2: first, the sodium nitrite gas delivery system delivers a certain amount of sodium nitrite gas to the sodium nitrite metering silo, the gas metering component of the sodium nitrite metering silo feeds back the gas delivery amount in real time, and feeds back the metering information to the second metering control system, and the sodium nitrite gas is delivered to the diazotization kettle to be condensed first and then react with the mixture ①; secondly, the temperature display component in the diazotization kettle detects the internal temperature in real time, and feeds back the temperature information to the second metering control system, and then according to the setting of the reaction temperature and reaction time in the diazotization step in the second metering control system, its output control end acts on the feed regulating valve of the sodium nitrite metering silo to realize the feed control of the material amount, thereby realizing the real-time control and feedback of the temperature;
[0019] S3: Thermal decomposition step: The mixture ② is transported to the thermal decomposition tanks R1-R4 in the thermal decomposition processing area to correspond to four thermal decomposition stages, wherein the temperature control system sets the reaction temperatures of the four thermal decomposition tanks in turn at the corresponding stages, and realizes one-key temperature increase operation control at the beginning of the thermal decomposition step;
[0020] S4: Standing separation step: the product obtained in step S3 is input into a standing separation tank to stand and separate into layers, and the upper layer obtained is crude p-fluorotoluene, and the lower layer is waste acid;
[0021] S5: Water washing and neutralization step: collecting the lower layer of wastewater and transferring it to a neutralization tank, adding an alkaline solution thereto for neutralization reaction to make the mixed solution neutral, collecting the upper layer of crude p-fluorotoluene into a water washing tank, and washing the crude p-fluorotoluene with water for multiple times;
[0022] S6: Water separation step: the washed crude parafluorotoluene is conveyed to the water separation tank, the coil freezing component is controlled to operate to freeze the material in the water separation tank, and after the freezing is completed, the ice breaking component is controlled to operate to crush the frozen material. At this time, the lifting plate drives the material to rise. On the one hand, the ice crystals generated by the crushing are conveyed to the ice crystal processing tank body under the cooperation of the conveying component and the material shifting component, and on the other hand, the parafluorotoluene liquid flows downward through the one-way valve of the lifting plate to complete the separation;
[0023] Among them, in step S6: the ice crystals transported to the ice crystal treatment tank fall on the loading plate, and the cleaning component is controlled to rotate the ice crystals. While collecting and cleaning all the ice crystals, the ice crystals can also be further broken to transform them into ice water. The treated ice crystal water is then fed back to the coil freezing temperature control group and the diazotization reactor;
[0024] S7: Distillation step: The crude p-fluorotoluene after water separation is transported to a distillation tower, and is first heated to perform reduced pressure distillation, and then heated to perform atmospheric pressure distillation, to obtain a distillation fraction p-fluorotoluene finished product.
[0025] Compared with the prior art, the advantages and positive effects of the present invention are:
[0026] 1. The present invention provides an automated production line for p-fluorotoluene. The first metering control system and the second metering control system are used to automatically control the temperature and the amount of material added during the reaction process based on the reaction time of each reaction stage, thereby improving the production and processing system of p-fluorotoluene products and effectively improving the degree of automation. The water separation tank is used to freeze the washed crude p-fluorotoluene material based on a freezing crystallization method, and then the ice crystals are crushed. At the same time, the p-fluorotoluene liquid can be collected in a centralized manner, the water separation work is completed, the work progress is guaranteed, and the ice crystal material can be put into the production line for subsequent processing, saving resources. The device has reasonable design, simple structure, convenient processing and is equipped with an automatic control system in the production and processing of p-fluorotoluene, which can reduce labor costs to a certain extent, reduce production safety accidents, improve production efficiency, and ensure the economic benefits of production and processing in the factory. At the same time, the water in p-fluorotoluene is frozen and crystallized to discharge the p-fluorotoluene to complete the water separation, especially to fully crush the p-fluorotoluene retained in the crystal, and make the p-fluorotoluene liquid fall and be exported, and the frozen crystals can also flow back to the production line, which plays a role in saving production costs and effectively meets the use needs. BRIEF DESCRIPTION OF THE DRAWINGS
[0027] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the following briefly introduces the drawings required for use in the description of the embodiments. Obviously, the drawings described below are some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without creative work.
[0028] Figure 1 It is a structural schematic diagram of the automated production line of p-fluorotoluene;
[0029] Figure 2 It is a structural schematic diagram of a moisture separation tank;
[0030] Figure 3 It is a structural front view of the moisture separation tank;
[0031] Figure 4 It is a schematic diagram of some internal structures in the freezing tank;
[0032] Figure 5 This is a schematic diagram of part of the internal structure of the ice-breaking component;
[0033] Figure 6 It is a schematic diagram of a partial internal structure of the ice-breaking assembly from above;
[0034] Figure 7 It is a schematic diagram of part of the internal structure of the one-way valve;
[0035] Figure 8 It is a front view of the internal structure of the one-way valve;
[0036] Fig. 9 This is a schematic diagram of part of the internal structure of the ice crystal treatment tank;
[0037] Fig.10 It is a front view of part of the internal structure of the ice crystal treatment tank;
[0038] In the above figures, 1, salt-forming kettle; 2, coil refrigeration temperature control group; 3, aniline metering tank; 4, first metering control system; 5, diazotization kettle; 6, sodium nitrite metering silo; 7, sodium nitrite gas delivery system; 8, second metering control system; 9, thermal decomposition tank; 10, temperature control system; 11, static separation tank; 12, water washing tank; 13, moisture separation tank; 131, support frame; 132, freezing tank body; 13 3. Ice crystal treatment tank; 1331. Feeding port; 14. Distillation tower; 15. Distillation supply group; 16. Coil freezing assembly; 17. Material shifting assembly; 171. Mounting frame; 172. Horizontal frame; 173. Vertical plate; 18. Conveying assembly; 181. Casing; 182. Auger blade; 19. Ice breaking assembly; 191. Ring plate; 1911. Adjustment groove; 192. Carrying plate; 1921. Key groove; 193. Installation disc; 194, rotating blade; 195, rotating disc; 1951, arc groove; 196, moving rod; 197, crushing tooth; 198, adjusting rod; 199, locking bolt; 20, partition; 21, driving shaft; 22, driving gear; 23, driven gear; 24, adjusting screw; 25, lifting disc; 26, one-way valve; 261, valve sleeve; 262, limit sleeve; 263, valve body; 2631, limit plate; 27 , rotating shaft; 28, toggle rod; 29, loading tray; 30, cleaning assembly; 301, rotating rod; 302, arc rod; 303, vertical rod; 304, material discharge plate; 305, cover body; 306, vertical plate; 307, lifting rod; 308, cleaning plate; 309, key plate; 310, fixing rod; 311, spring; 312, stop block; 31, drainage cover; 32, collecting cover; 33, drain pipe; 34, sealing plate. DETAILED DESCRIPTION
[0039] In order to more clearly understand the above-mentioned purpose, features and advantages of the present invention, the present invention is further described below in conjunction with the accompanying drawings and embodiments. It should be noted that the embodiments of the present application and the features in the embodiments can be combined with each other without conflict.
[0040] In the following description, many specific details are set forth to facilitate a full understanding of the present invention. However, the present invention may also be implemented in other ways than those described herein. Therefore, the present invention is not limited to the specific embodiments of the following disclosure.
[0041] Examples, such as Figure 1 to Figure 10As shown, an automated production line for parafluorotoluene includes a salt-forming processing area, a diazotization processing area, a thermal decomposition processing area, a water washing and neutralization area, and a distillation area arranged in sequence along the parafluorotoluene production line. The salt-forming processing area includes a salt-forming kettle 1 with a stirring function. Two feeding inlets are arranged outside the salt-forming kettle 1, one is an anhydrous hydrofluoric acid feeding inlet, and the other is an aniline feeding inlet. This design is used to ensure the smooth progress of the feeding work. A coil refrigeration temperature control group 2 is arranged on the outside of the salt-forming kettle 1. This component includes a spiral-disk-shaped pipe body and a regulating valve for material inlet and outlet. The inlet receives cold water medium, and the outlet outputs the changed medium. The specific control temperature is controlled according to the reaction. Of course, this design is also an existing mature and commonly used technical means, which uses the conveying of refrigerated water medium to achieve the kettle body. In order to control the internal temperature, an aniline metering tank 3 with a weighing and metering module is arranged on one side of the salt-forming kettle 1 and is connected to the salt-forming kettle 1. For the materials pre-placed in the aniline metering tank 3, the weighing and metering module can weigh the weight in real time, and record and feed back the weight information. A first metering control system 4 is arranged on the outside of the weighing and metering module of the aniline metering tank 3. The diazotization processing area includes a diazotization kettle 5 with a temperature display component and a temperature control function. A coil refrigeration and temperature control group 2 is also arranged on the outside of the diazotization kettle 5 for realizing the control of the reaction temperature in the kettle. The temperature display component on the diazotization kettle 5 can measure the temperature in the kettle in real time, and feed back the temperature information to the control system. A gas metering component is arranged on the top of the diazotization kettle 5. Sodium nitrite metering silo 6, the gas metering component is used to detect the output of the material in the sodium nitrite metering silo 6 in real time, and a sodium nitrite gas delivery system 7 is arranged at the feed inlet of the sodium nitrite metering silo 6. This design takes into account the low reaction temperature in the diazotization reactor 5. For the method of transporting materials in a gaseous state, it can not only ensure the precise regulation of the delivery amount, but also rely on the reaction temperature to condense the material into a liquid to participate in the reaction, saving costs while improving the convenience of the production and processing process. A second metering control system 8 is arranged outside the gas metering component of the sodium nitrite metering silo 6. The thermal decomposition processing area includes a thermal decomposition tank 9 with a heating function and arranged in sequence. R1-R4, the four thermal decomposition tanks 9 correspond to the thermal decomposition working area respectively. The four stages in the thermal decomposition processing zone each have their own functions and do not interfere with each other. A temperature control system 10 is provided on one side of the thermal decomposition processing zone. The temperature control system 10 has a one-key temperature increase program, that is, it can perform one-key control on the temperature in the tank body at different thermal decomposition stages, and the temperature increase process is also different due to the influence of different stages, that is, the temperature increase process corresponds to the action time of the previous stage. The water washing and neutralization zone includes a standing separation tank 11 for receiving the crude p-fluorotoluene product and realizing standing stratification. The obtained upper layer is crude p-fluorotoluene, and the lower layer is waste acid, which is neutralized with a sodium hydroxide solution. A water washing tank 12 is provided on one side of the standing separation tank 11, and a water separation tank 13 for pre-treating the crude p-fluorotoluene after water washing is provided on one side of the water washing tank 12.The distillation area includes a distillation tower 14 for receiving the material discharged from the water separation tank 13. The distillation working principle is effectively known to those skilled in the art, and the details are not repeated here. A distillation supply group 15 for heat supply is provided on one side of the distillation tower 14. The distillation supply group 15 can ensure the continuous supply of heat in the distillation tower 14, providing convenient conditions for the distillation work.
[0042] In order to further improve the rationality of the establishment of the device, the output control end of the first metering control system 4 is respectively connected to the feed regulating valve of the coil refrigeration temperature control group 2 and the discharge regulating valve of the aniline metering tank 3, the signal end of the second metering control system 8 is connected to the temperature display component of the diazotization kettle 5, and the output end of the second metering control system 8 is connected to the feed regulating valve of the sodium nitrite metering silo 6 of the diazotization kettle 5.
[0043] In order to effectively improve the degree of automation in the production and processing of p-fluorotoluene, a production method of a p-fluorotoluene automated production line is provided, comprising the following steps:
[0044] S1: Salt-forming step: anhydrous hydrofluoric acid is transported to the salt-forming kettle 1, and the aniline metering tank 3 is opened to uniformly add the anhydrous hydrofluoric acid to the salt-forming kettle 1, and the reaction temperature and reaction time are adjusted to fully react to obtain a mixture ①;
[0045] Among them, in step S1: the weighing and metering module in the aniline metering tank 3 weighs the aniline material in real time, and feeds back the remaining material weight information to the first metering control system 4. According to the setting of the reaction temperature and reaction time in the salt-forming step by the first metering control system 4, its output control end acts on the feed regulating valve of the coil refrigeration temperature control group 2 and the feed regulating valve of the aniline metering tank 3 respectively, so as to realize the automatic control of the reaction temperature and reaction time;
[0046] S2: Diazotization step: input the mixture ① into the diazotization kettle 5, open the sodium nitrite metering silo 6, add all the materials to the diazotization kettle 5 at a uniform speed, control the reaction temperature and reaction time, and obtain the mixture ② after sufficient reaction;
[0047] Wherein, in step S2: first, the sodium nitrite gas delivery system 7 delivers a certain amount of sodium nitrite gas to the sodium nitrite metering silo 6, the gas metering component of the sodium nitrite metering silo 6 feeds back the gas delivery amount in real time, and feeds back the metering information to the second metering control system 8, and the sodium nitrite gas is delivered to the diazotization kettle 5 to be condensed first and then react with the mixture ①; secondly, the temperature display component in the diazotization kettle 5 detects the internal temperature in real time, and feeds back the temperature information to the second metering control system 8, and then according to the setting of the reaction temperature and reaction time in the diazotization step in the second metering control system 8, its output control end acts on the feed regulating valve of the sodium nitrite metering silo 6 to realize the feed control of the material amount, thereby realizing the real-time control and feedback of the temperature;
[0048] S3: Thermal decomposition step: the mixture ② is transported to the thermal decomposition tanks 9R1-R4 in the thermal decomposition processing area to correspond to four thermal decomposition stages, wherein the temperature control system 10 sets the reaction temperature of the corresponding stages for the four thermal decomposition tanks 9 in turn, and realizes one-key temperature increase operation control at the beginning of the thermal decomposition step;
[0049] S4: static separation step: the product obtained in step S3 is input into a static separation tank 11 to be statically separated and separated, and the obtained upper layer is crude p-fluorotoluene, and the lower layer is waste acid;
[0050] S5: Water washing and neutralization step: collecting the lower layer of wastewater and conveying it to a neutralization tank, adding an alkaline solution thereto for neutralization reaction, so that the mixed solution reaches neutrality, collecting the upper layer of crude p-fluorotoluene into a water washing tank 12, and washing the crude p-fluorotoluene with water for multiple times;
[0051] S6: Water separation step: The washed crude parafluorotoluene is conveyed to the water separation tank 13, and the coil freezing assembly 16 is controlled to operate to freeze the material in the water separation tank 13. After the freezing is completed, the ice breaking assembly 19 is controlled to operate to crush the frozen material. At this time, the lifting plate 25 drives the material to rise. On the one hand, the ice crystals generated by the crushing are conveyed to the ice crystal processing tank body 133 under the cooperation of the conveying assembly 18 and the material shifting assembly 17. On the other hand, the parafluorotoluene liquid passes through the one-way valve 26 of the lifting plate and flows downward to complete the separation;
[0052] Among them, in step S6: the ice crystals transported to the ice crystal processing tank 133 fall on the loading plate 29, and the cleaning component 30 is controlled to rotate the ice crystals. While collecting and cleaning all the ice crystals, the ice crystals can also be further broken to transform them into ice water. The treated ice crystal water is then fed back to the coil freezing temperature control group 2 and the diazotization kettle 5;
[0053] S7: Distillation step: transporting the crude p-fluorotoluene after water separation to the distillation tower 14, first heating and distilling under reduced pressure, then heating and distilling under normal pressure to obtain a distillation fraction p-fluorotoluene finished product;
[0054] In the above process: the first metering control system 4 and the second metering control system 8 are used to automatically control the temperature and the amount of material added in the reaction process based on the reaction time of each reaction stage, thereby improving the production and processing system of the p-fluorotoluene product and effectively improving the degree of automation; the water separation tank 13 is used to freeze the washed crude p-fluorotoluene material based on the freezing crystallization method, and then the ice crystals are crushed, and at the same time, the p-fluorotoluene liquid can be collected centrally, the water separation work is completed, and the work progress is guaranteed. The ice crystal material can be put into the production line after subsequent processing, saving resource costs. The economic benefits of production in the factory are guaranteed and the use requirements are met. The device has a reasonable design, a simple structure, and is easy to process. In addition, an automatic control system is installed in the production and processing of p-fluorotoluene, which reduces labor costs to a certain extent, reduces production safety accidents, improves production efficiency, and guarantees the economic benefits of production and processing in the factory. At the same time, the water in p-fluorotoluene is frozen and crystallized, and the p-fluorotoluene is discharged to complete the water separation, especially the p-fluorotoluene retained in the crystal is fully crushed, and the p-fluorotoluene liquid is made to fall and be exported, and the frozen crystals can also flow back to the production line, which plays a role in saving production costs and effectively meets the use requirements.
[0055] In order to ensure that the device has a good establishment effect, the moisture separation tank 13 includes a tank body designed in an M shape, which can separate the two operating procedures, realize one device to complete two operating processes, and fully improve the functionality of the device. Further, the tank body includes a freezing tank body 132 and an ice crystal processing tank body 133 designed in an arc shape and arranged in a mirror image with respect to the freezing tank body 132. A material inlet is set on the rear side of the freezing tank body 132. It should be further explained that: for the material amount transported to the freezing tank body 132, the upper interface is lower than the ice breaking component 19 to ensure the smooth progress of the crushing work. A support frame 131 is arranged below the freezing tank body 132 and the ice crystal processing tank body 133, which can ensure the stability of the equipment establishment. The freezing tank body 1 A coil freezing assembly 16 is arranged on the periphery of the freezing tank 132, and its function is to cool and freeze the freezing tank body 132 so that the washed materials are frozen, providing a prerequisite for the subsequent processing work. A driving shaft 21 is arranged in the freezing tank body 132, and a material shifting assembly 17, a conveying assembly 18 and an ice breaking assembly 19 are arranged on the outside of the driving shaft 21 from top to bottom. The operation of the ice breaking assembly 19 can crush the frozen materials and separate the p-fluorotoluene liquid from the ice crystals. The conveying assembly 18 and the material shifting assembly 17 cooperate to guide the crushed ice crystals to the outside, so as to ensure the smooth progress of the subsequent processing work. A partition 20 is arranged above the freezing tank body 132, and a driving gear 22 is arranged on the outside of the driving shaft 21 above the partition 20. Two symmetrically arranged driven gears 23 are arranged on the outside of the driving gear 22, and an adjusting screw 24 is arranged inside the driven gear 23. The lower end of the adjusting screw 24 is rotatably connected to the bottom of the freezing tank body 132, and a lifting plate 25 is arranged on the lower outside of the two adjusting screws 24, wherein an external thread is provided below the outer periphery of the adjusting screw 24, and the external threads on the two adjusting screws 24 are in opposite directions. In this way, the lifting plate 25 can be driven to rise and fall in the vertical direction by the rotation of the adjusting screw 24, thereby driving the frozen material to move upward to ensure the continuous progress of the ice breaking work. In addition, considering that the material may affect the movement of the external thread of the adjusting screw 24 when frozen, a pipe sleeve can be set on the outer periphery of the adjusting screw 24 (in the figure Not shown), wherein the length of the tube sleeve is greater than the opening distance of the external thread and less than half the overall length of the adjusting screw 24, and the outer periphery of the tube sleeve is fixedly connected to the lifting plate, and a lead screw nut is provided inside to ensure that the lifting plate and the tube sleeve can be lifted and moved vertically with the help of the cooperation between the lead screw nut and the adjusting screw 24. Of course, the upper end of the tube sleeve is closed, and a sealing assembly is provided at the geometric center of its upper end and cooperates with the outer periphery of the adjusting screw 24. That is to say, when the lifting plate 25 is at the bottom, the lower end of the tube sleeve is precisely matched with the lower inner wall of the freezing tank body, and in order to prevent liquid from entering, the lower end face of the tube sleeve and the upper end face are closed structures and sealed, and the upper liquid level of the maximum amount of material in the freezing tank body 132 is lower than the upper end face of the tube sleeve,And when the lifting plate 25 rises to near the ice-breaking assembly 19, the upper end of the pipe sleeve is also on the upper inner side of the freezing tank body 132. The purpose of this design is to ensure the smoothness of the operation of the adjusting screw 24, avoid the frozen material from hindering its operation, and improve the convenience of the device during use, prevent interference, and ensure the working process; a plurality of one-way valves 26 are evenly arranged in the lifting plate 25, which are specifically described as follows: when the drive shaft 21 is driven by the external drive assembly, the material-dispensing assembly 17, the conveying assembly 18 and the ice-breaking assembly 19 are all in operation, and the ice-breaking assembly 19 crushes the frozen material. At the same time, the driving gear 22 rotates with the drive shaft 21 and acts on the driven gear 23. When the driven gear 23 rotates, it can drive the adjusting screw 24 to rotate, and the lifting plate 25 can slowly rise vertically relative to the adjusting screw 24, and the p-fluorotoluene liquid can flow downward from the one-way valve 26. When the lifting plate 25 drives the frozen material to move upward, the material can also be transported to the ice-breaking component to ensure the effective implementation of the crushing work and meet the use requirements. Further, after the crude p-fluorotoluene after water washing is first frozen, then crushed, and finally precipitated, the water content in the p-fluorotoluene product is greatly reduced. When the subsequent distillation work is carried out, it plays a role in saving distillation steam, which can effectively save production costs to a certain extent and ensure the production efficiency in the factory.
[0056] In order to facilitate the conveying of the crushed ice crystals into the ice crystal processing tank body 133 to improve the progress of subsequent processing work, the material-dispensing assembly 17 includes a mounting frame 171 connected to the drive shaft 21, and a horizontal frame 172 is arranged on the outer side of the upper and lower mounting frames 171, and a vertical plate 173 is arranged between the two horizontal frames 172, wherein the cross section of the mounting frame 171 is designed in an L shape, which provides convenient installation conditions for the establishment of the horizontal frame 172, and the establishment of the vertical plate 173 is arranged in an inclined state. When the drive shaft 21 rotates, the material-dispensing assembly 17 is driven to rotate, and the ice crystals conveyed upward by the conveying assembly 18 are pushed outward, so that they move toward the connection between the freezing tank body 132 and the ice crystal processing tank body 133, and then fall into the ice crystal processing tank In the body 133, in order to fully enable the crushed ice crystals to be transported upward, the conveying component 18 includes a sleeve 181 connected to the drive shaft 21, and the outer periphery of the sleeve 181 is provided with an auger blade 182, that is to say: the ice breaking component will crush the frozen material on the one hand, and on the other hand, it will throw it outward with the help of centrifugal effect, and the direction of its throwing corresponds to the inlet of the ice crystal processing tank body 133. For the ice crystals that splash in the vertical direction, the auger blade 182 will receive it and realize the upward conveying trend with its rotation, and then with the cooperation of the material shifting component 17, the ice crystals are smoothly transported to the ice crystal processing tank body 133, ensuring that the subsequent ice crystal materials are further processed and the work progress is improved.
[0057] In order to effectively complete the crushing process of frozen materials, the ice breaking assembly 19 includes an annular disk 191, and a carrier disk 192 is arranged below the annular disk 191, and the two are connected by bolts. A mounting disk 193 is arranged at the geometric center of the carrier disk 192, which is also connected to the carrier disk 192 by bolts. A rotating blade 194 is arranged below the mounting disk 193, and an axle rod (not shown in the figure) is set above the rotating blade 194 and connected to the mounting disk 193 to ensure that the rotating blade 194 has good stability. A rotating disk 195 is arranged on the outer side of the mounting disk 193, and a notch designed in an L shape is arranged near the corner of the mounting disk 193, which realizes its position to a certain extent. The rotating disk 195 is sleeved on the outside of the mounting disk 193 and located on the inside of the ring disk 191, and can rotate relative to the mounting disk 193 and the ring disk 191, wherein the rotation of the adjusting rod 198 can be used to adjust the position of the rotating disk 195, an arc groove 1951 is provided in the rotating disk 195, a key groove 1921 is provided in the carrier disk 192, a moving rod 196 is provided in the key groove 1921, and is adapted to the arc groove 1951, the moving rod 196 passes through the key groove 1921, and a limiting sleeve 262 is provided at the outer periphery thereof close to the key groove 1921, which not only ensures the stability of the moving rod 196, but also ensures the smoothness of the moving process, and the moving rod 19 6 is provided with a crushing tooth 197, the inner side surface of the crushing tooth 197 is designed in an arc shape, which can act on the frozen ice crystals to complete the pre-processing. In addition, in order to further improve the functionality of the device, a limit installation block designed in a fan shape is set between two adjacent crushing teeth 197. On the premise of limiting the installation position of the workpiece, it can also ensure that it is smoother and more convenient during the movement. An adjustment groove 1911 is provided on one side of the ring disk 191, and an adjustment rod 198 is provided in the adjustment groove 1911, and is connected to the rotating disk 195. A locking bolt 199 is provided on the top of the ring disk 191. The specific description is: according to the specifications of the freezing tank body 132, the adjustment rod 198 is adjusted in the adjustment Rotation adjustment is carried out in the section groove 1911. Of course, a process hole is opened above the ring disk 191 which conforms to the arc of the adjustment groove 1911. When the adjusting rod 198 is rotated, it drives the rotating disk 195 to rotate, and under the limitation of the arc groove 1951, when the moving rod 196 and the crushing tooth 197 move inward or outward relative to the key groove 1921, they will also be adjusted by the limit of the rotating disk 195. When the position is determined, a locking bolt 199 is installed in the process hole and screwed into the adjusting rod 198 to complete the locking of its position. In this way, the ice breaking assembly rotates circumferentially with the drive shaft 21, and the crushing of the frozen material can be completed under the action of the crushing tooth 197 to ensure the working progress.
[0058] In order to allow the p-fluorotoluene liquid to flow out conveniently, the one-way valve 26 includes a valve sleeve 261 with an L-shaped cross section. A process hole with a conical shape is provided on the upper inner side of the valve sleeve 261 and corresponds to the large head of the valve body 263. A limiting sleeve 262 is provided at the lower part of the valve sleeve 261. The cross section of the limiting sleeve 262 is also L-shaped. A sealing ring can be added between the notch on the outer side of the limiting sleeve 262 and the valve sleeve 261. While ensuring its sealing effect, it can also improve the stability of the equipment. The valve sleeve 26 located above the limiting sleeve 262 1 is provided with a valve body 263 designed in a double cone shape, the taper and height of the lower half of the valve body 263 are greater than the taper and height of the upper half thereof, wherein the outer periphery below the valve body 263 is in a streamline shape, which increases the contact area to a certain extent, and a limiting plate 2631 is provided on the outer side of the valve body 263, the outer side of the limiting plate 2631 is in a stepped design, and the upper side thereof is adapted to the inner diameter of the valve sleeve 261, specifically described as follows: when installing the one-way valve 26, the limiting sleeve 262 is kept in the downward direction for installation, and when liquid flows down from the lifting plate 25, it will flow from the valve The upper part of the sleeve 261 flows downward, and then flows downward through the gap between the two limit plates 2631. In this embodiment, it provides convenience for the centralized collection of the p-fluorotoluene liquid. When all the ice crystals are broken, the water in the crude p-fluorotoluene is almost separated along with the extraction of the ice crystals. In this way, the p-fluorotoluene liquid can be extracted to the outside. During the extraction process, the valve of the pipeline below the freezing tank body 132 is opened so that the p-fluorotoluene liquid can flow out through the management. In order to ensure that the material is extracted more thoroughly, the driving shaft 21 is controlled to run in the reverse direction, and the screw is adjusted. 24 drives the lifting plate 25 downward with the cooperation of the gears. At this time, considering the pressure conditions in the freezing tank body 132, the valve body 263 and the limit plate 2631 will be pushed upward until the upper half of the valve body 263 blocks the upper opening of the valve sleeve 261. In this process, the lifting plate 25 tends to be a sealed plate body. As the lifting plate 25 descends, the parafluorotoluene liquid at the bottom of the freezing tank body 132 can be pressed, especially so that it can be discharged outward through the pipeline, which improves the discharge process to a certain extent, ensures the thoroughness of material discharge, and meets the use requirements.
[0059] In order to further process the ice crystals introduced from the freezing tank 132 into the ice crystal processing tank 133, a rotating shaft 27 is provided in the ice crystal processing tank 133 and a driving motor can be provided on the outside of the ice crystal processing tank 133 to provide driving power to the rotating shaft 27. A toggle rod 28 is provided on the lower outside of the rotating shaft 27. A loading tray 29 in the shape of a flying saucer is provided at the bottom of the ice crystal processing tank 133 for receiving the introduced ice crystals. A cleaning component 30 is provided above the loading tray 29 for not only cleaning the materials adhering to the loading tray 29 but also for further grinding the materials so as to make the ice crystals more hygroscopic. It is converted from fragments or powder to ice water. The ice crystal processing tank body 133 located on both sides of the lower end of the loading plate 29 is staggered with discharge ports 1331. This design can not only ensure the stability of the device and equipment, ensure that it has good use strength, but also provide a prerequisite for the smooth export of materials, improve the working process, and the outer periphery of the ice crystal processing tank body 133 located outside the discharge port 1331 is provided with a drainage hood 31 with a right-angle trapezoidal cross-section. A collection hood 32 with a conical table-like design is provided below the drainage hood 31. A drainage pipe 33 is provided below the collection hood 32. A sealing plate that can be lifted and lowered vertically is provided on the drainage hood 31. 34, and corresponds to the discharge port 1331 located at the top, wherein the sealing plate 34 can be raised and lowered in the vertical direction relative to the drainage cover 31, and in order to realize the degree of automation of the equipment, a driving cylinder can be set on the outside of the ice crystal processing tank body 133, and its extension or contraction is used to complete the convenient opening operation of the discharge port 1331 located at the top, which is specifically described as follows: the crushed ice crystal material is input from the freezing tank body to the ice crystal processing tank body 133, and falls on the loading plate 29, and the rotation of the control shaft 27 is controlled to act on the cleaning component 30. Under the action of the cleaning component 30, on the one hand, it can clean the material on the loading plate 29 downward, and on the other hand On the one hand, the ice crystal material can be further shattered to accelerate its melting process, thereby converting it into an ice water state. The treated ice water material is temporarily stored above the lower half of the loading tray 29 until the ice crystals are completely broken and post-processed under the action of the cleaning component 30. The external cylinder is controlled to run, driving the sealing plate 34 to rise, so that the material is discharged through the discharge port 1331, and under the action of the drainage hood 31, it is guided to the collection hood 32 through the discharge port 1331 below, and finally discharged from the drain pipe 33 and transported to the equipment that needs to be temperature controlled in the production line. To a certain extent, resource costs can be saved and economic benefits can be guaranteed.
[0060] In order to complete the cleaning and further crushing of the ice crystals adhered to the loading tray 29, the cleaning component 30 includes a rotating rod 301 connected to the loading tray 29, which can rotate relative to the loading tray 29. An arc rod 302 is arranged on one side of the rotating rod 301, and a vertical rod 303 is arranged on the lower outer side of the arc plate. A receiving block with a material having deformation and recovery functions, such as rubber or silicone material, is set on the upper part of the vertical rod 303. When the rotating shaft 27 rotates, it will drive the toggle rod 28 to rotate together, and then act on the receiving block. In this way, the vertical rod 303 and the arc rod 302 can rotate with the rotating rod 301 under the above-mentioned driving power. A material separation plate 304 designed in a chain concave shape is arranged on the inner side of the arc plate. When the material separation plate 304 rotates with the arc plate, it relies on its designed shape to collect the materials on the loading tray 29 in sections, thereby providing a prerequisite for the subsequent cleaning and crushing of the cleaning plate 308.Furthermore, a cover body 305 with a hollow L-shape is provided on the other side of the rotating rod 301, and one end face of the cover body 305 is designed in an arc shape and is adapted to the outer periphery of the material loading tray 29. A plurality of vertical plates 306 are evenly arranged in the cover body 305, and the cover body 305 is divided into a plurality of cleaning areas, wherein a plurality of cleaning areas are provided, which can correspond to the gaps between the material discharging plates 304. A lifting rod 307 is provided on the cover body 305, and the lengths of the plurality of lifting rods 307 increase from the inside to the outside. A cleaning plate 308 is provided at the lower end of the lifting rod 307, and the spacing between the cleaning plate 308 and the outer periphery of the material loading tray 29 is approximately the same, so that the driving power of the toggle rod 28 acts on the lifting rod 307. When the toggle rod 28 is on the rod 307, it has an equal descending distance. A key plate 309 is arranged on the periphery of the lifting rod 307, and a fixing rod 310 is arranged on the cover body 305 and penetrates the key plate 309. A spring 311 is arranged on the periphery of the fixing rod 310 between the cover body 305 and the key plate 309. A wedge-shaped abutment 312 is arranged above the lifting rod 307. When the toggle rod 28 rotates, the toggle rod 28 on one side acts on the vertical rod 303 to provide driving power for it, and the toggle rod 28 on the other side acts on the abutment 312 to provide driving power. When and only when the toggle rod 28 is close to the receiving block and the abutment 312 at the same time, relying on its rotational inertia, it will drive the cleaning The component 30 rotates in the circumferential direction until the driving force is greater than the deformation resistance of the receiving block, the receiving block deforms, and the toggle rod 28 passes the position of the vertical rod 303. The receiving block returns to its original state after passing. At the same time, the toggle rod 28 on the other side will act on each stop block 312 in turn. Due to the shape design of the stop block 312, it will press the lifting rod 307 downward under the action of the driving force, and move the cleaning plate 308 toward the outer periphery of the loading tray 29. In this process, the cleaning plate 308 can not only have a tendency to rotate in the circumferential direction for cleaning, but also press downward in the vertical direction, especially acting on the ice crystal material to further crush it, thereby enhancing the crushing effect to a certain extent. In order to accelerate the melting process and make the transition to the ice water state more convenient, considering the reset of the toggle rod 28 after driving the lifting rod 307 to descend, the key plate 309 will also move downward relative to the fixed rod 310 when the lifting rod 307 descends, and compress the spring 311. When the toggle rod 28 passes over the stop block 312, the spring 311 expands and contracts and drives the lifting rod 307 to rise and reset. In this way, the cleaning component 30 can intermittently rotate in the circumferential direction, not only to divide it into parts, but also to crush the materials under the partitions, accelerate its melting process, and also to clean it to a certain extent, reduce the possibility of waste of resources, and improve the functionality of the device. ;
[0061] The above description is only a preferred embodiment of the present invention and does not limit the present invention in other forms. Any technician familiar with the profession may use the technical content disclosed above to change or modify it into an equivalent embodiment with equivalent changes and apply it to other fields. However, any simple modification, equivalent change and modification made to the above embodiment based on the technical essence of the present invention without departing from the content of the technical solution of the present invention still falls within the protection scope of the technical solution of the present invention.
Claims
1. An automated parafluorotoluene production line, comprising a salt-forming processing area, a diazotization processing area, a thermal decomposition processing area, a water washing and neutralization area and a distillation area arranged in sequence along the parafluorotoluene production line, characterized in that: The salt-forming processing area comprises a salt-forming kettle (1) with a stirring function, a coil refrigeration temperature control group (2) is arranged outside the salt-forming kettle (1), an aniline metering tank (3) with a weighing and metering module is arranged on one side of the salt-forming kettle (1) and is connected to the salt-forming kettle (1), a first metering control system (4) is arranged outside the weighing and metering module of the aniline metering tank (3), the diazotization processing area comprises a diazotization kettle (5) with a temperature display component and a temperature control function, a sodium nitrite metering silo (6) with a gas metering component is arranged above the diazotization kettle (5), a sodium nitrite gas delivery system (7) is arranged at the feed inlet of the sodium nitrite metering silo (6), and the gas of the sodium nitrite metering silo (6) is A second metering control system (8) is arranged outside the metering component. The thermal decomposition processing area includes thermal decomposition tanks (9) R1-R4 with heating functions and arranged in sequence. A temperature rise control system (10) is arranged on one side of the thermal decomposition processing area. The water washing and neutralization area includes a static separation tank (11) for receiving the crude para-fluorotoluene product to achieve static stratification. A water washing tank (12) is arranged on one side of the static separation tank (11). A water separation tank (13) for pre-treating the crude para-fluorotoluene after water washing is arranged on one side of the water washing tank (12). The distillation area includes a distillation tower (14) for receiving the material output from the water separation tank (13). A distillation supply group (10) for heat supply is arranged on one side of the distillation tower (14). 5), the output control end of the first metering control system (4) is respectively connected to the feed regulating valve of the coil freezing temperature control group (2) and the discharge regulating valve of the aniline metering tank (3), the signal end of the second metering control system (8) is connected to the temperature display component of the diazotization kettle (5), and the output end of the second metering control system (8) is connected to the feed regulating valve of the sodium nitrite metering silo (6) of the diazotization kettle (5), the moisture separation tank (13) includes a tank body designed in an M shape, the tank body includes a freezing tank body (132) and an ice crystal treatment tank body (133) designed in an arc shape and arranged in a mirror image with respect to the freezing tank body (132), and a support frame (132) is arranged below the freezing tank body (132) and the ice crystal treatment tank body (133). 31), a coil freezing assembly (16) is arranged on the outer periphery of the freezing tank body (132), a driving shaft (21) is arranged inside the freezing tank body (132), a material shifting assembly (17), a conveying assembly (18) and an ice breaking assembly (19) are arranged on the outer side of the driving shaft (21) from top to bottom, a partition (20) is arranged above the freezing tank body (132), a driving gear (22) is arranged on the outer side of the driving shaft (21) above the partition (20), two symmetrically arranged driven gears (23) are arranged on the outer side of the driving gear (22), an adjusting screw (24) is arranged inside the driven gear (23), and a lifting plate (25) is arranged on the lower outer side of the two adjusting screws (24),A plurality of one-way valves (26) are evenly distributed in the lifting plate (25).
2. The p-fluorotoluene automated production line according to claim 1, characterized in that: The material shifting assembly (17) comprises a mounting frame (171) connected to the driving shaft (21), a horizontal frame (172) is arranged outside the upper and lower mounting frames (171), and a vertical plate (173) is arranged between the two horizontal frames (172); the conveying assembly (18) comprises a sleeve (181) connected to the driving shaft (21), and an auger blade (182) is arranged on the outer periphery of the sleeve (181).
3. The p-fluorotoluene automated production line according to claim 2, characterized in that: The ice-breaking assembly (19) comprises an annular disk (191), a carrier disk (192) is arranged below the annular disk (191), a mounting disk (193) is arranged at the geometric center of the carrier disk (192), a rotating blade (194) is arranged below the mounting disk (193), a rotating disk (195) is arranged on the outer side of the mounting disk (193), an arc-shaped groove (1951) is provided in the rotating disk (195), and a key-shaped groove (1951) is provided in the carrier disk (192). A movable rod (196) is arranged in the key-shaped groove (1921) and is matched with the arc-shaped groove (1951); a crushing tooth (197) is arranged below the movable rod (196); an adjusting groove (1911) is arranged on one side of the ring disk (191); an adjusting rod (198) is arranged in the adjusting groove (1911) and is connected to the rotating disk (195); a locking bolt (199) is arranged above the ring disk (191).
4. The p-fluorotoluene automated production line according to claim 3, characterized in that: The one-way valve (26) comprises a valve sleeve (261) with an L-shaped cross section, a limiting sleeve (262) is arranged at the bottom of the valve sleeve (261), a valve body (263) with a double-conical shape is arranged in the valve sleeve (261) above the limiting sleeve (262), the taper and height of the lower half of the valve body (263) are greater than the taper and height of the upper half, a limiting plate (2631) is arranged at the outer side of the valve body (263), the outer side of the limiting plate (2631) is designed in a stepped shape, and the upper side thereof is adapted to the inner diameter of the valve sleeve (261).
5. The p-fluorotoluene automated production line according to claim 4, characterized in that: The ice crystal processing tank body (133) is provided with a rotating shaft (27) penetrating the rotating shaft, a toggle rod (28) is provided on the lower outer side of the rotating shaft (27), a material loading tray (29) in the shape of a flying saucer is provided on the lower side of the ice crystal processing tank body (133), a cleaning assembly (30) is provided on the upper side of the material loading tray (29), and material discharge ports (1331) are staggered in the upper and lower sides of the ice crystal processing tank body (133) located on both sides of the lower end of the material loading tray (29). A drainage hood (31) with a right-angled trapezoidal cross section is arranged on the outer periphery of the ice crystal treatment tank body (133) located outside the discharge port (1331), a collecting hood (32) with a conical table design is arranged below the drainage hood (31), a liquid discharge pipe (33) is arranged below the collecting hood (32), and a sealing plate (34) capable of vertical lifting is arranged on the drainage hood (31) and corresponds to the discharge port (1331) located above.
6. The p-fluorotoluene automated production line according to claim 5, characterized in that: The cleaning assembly (30) comprises a rotating rod (301) connected to the material loading tray (29), an arc-shaped rod (302) is arranged on one side of the rotating rod (301), a vertical rod (303) is arranged on the lower outer side of the arc-shaped plate, a material-discharging plate (304) designed in a chain concave shape is arranged on the inner side of the arc-shaped plate, a cover body (305) designed in a hollow L shape is arranged on the other side of the rotating rod (301), one end face of the cover body (305) is designed in an arc shape and is adapted to the outer periphery of the material loading tray (29), a plurality of vertical plates (306) are evenly arranged in the cover body (305), and The inside of the cover body (305) is divided into a plurality of cleaning areas. A lifting rod (307) is provided on the cover body (305). A cleaning plate (308) is provided at the lower end of the lifting rod (307). A key-shaped plate (309) is provided on the outer periphery of the lifting rod (307). A fixing rod (310) is provided on the cover body (305) and passes through the key-shaped plate (309). A spring (311) is provided on the outer periphery of the fixing rod (310) located between the cover body (305) and the key-shaped plate (309). A wedge-shaped stop block (312) is provided above the lifting rod (307).
7. A production method for an automated production line of p-fluorotoluene, characterized in that: The p-fluorotoluene automated production line as claimed in claim 6 comprises the following steps: S1: salt-forming step: anhydrous hydrofluoric acid is transported to the salt-forming kettle (1), and the aniline metering tank (3) is opened to uniformly add the anhydrous hydrofluoric acid to the salt-forming kettle (1), and the reaction temperature and reaction time are adjusted to allow the anhydrous hydrofluoric acid to react fully to obtain a mixture ①; S2: Diazotization step: the mixture ① is input into the diazotization kettle (5), the sodium nitrite metering bin (6) is opened, and all the materials are uniformly added dropwise into the diazotization kettle (5), and the reaction temperature and reaction time are controlled to obtain the mixture ② after sufficient reaction; S3: thermal decomposition step: the mixture ② is transported to the thermal decomposition tanks (9) R1-R4 in the thermal decomposition processing area to correspond to four thermal decomposition stages, wherein the temperature control system (10) sets the reaction temperatures of the corresponding stages for the four thermal decomposition tanks (9) in turn, and implements one-key temperature increase operation control at the beginning of the thermal decomposition step; S4: standing separation step: the product obtained in step S3 is input into a standing separation tank (11) to stand and separate layers, and the upper layer obtained is crude p-fluorotoluene, and the lower layer is waste acid; S5: Water washing and neutralization step: collecting the wastewater at the lower layer and transferring it to a neutralization tank, adding an alkaline solution thereto for neutralization reaction, so that the mixed solution reaches neutrality, collecting the crude p-fluorotoluene at the upper layer into a water washing tank (12), and washing the crude p-fluorotoluene with water for multiple times; S6: Water separation step: the washed crude parafluorotoluene is conveyed to the water separation tank (13), the coil freezing assembly (16) is controlled to operate to freeze the material in the water separation tank (13), and after the freezing is completed, the ice breaking assembly (19) is controlled to operate to crush the frozen material. At this time, the lifting plate (25) drives the material to rise. On the one hand, the ice crystals generated by the crushing are conveyed to the ice crystal processing tank (133) with the cooperation of the conveying assembly (18) and the material shifting assembly (17), and on the other hand, the parafluorotoluene liquid passes through the one-way valve (26) of the lifting plate and flows downward to complete the separation; S7: Distillation step: The crude p-fluorotoluene after water separation is transported to a distillation tower (14), where it is first heated and distilled under reduced pressure, and then heated and distilled under normal pressure to obtain a distillation fraction p-fluorotoluene product.
Citation Information
Patent Citations
Process for synthesizing methyl fluorobenzene by adopting hydrogen fluoride diazonium pyrolysis method
CN114874067A