LC-level purification device and method for diethyltoluenediamine for progressively screening out impurities
Through the LC-grade diethyl toluene diamine purification device and method for sieving impurities, the continuous purification and purity improvement of the diethyl toluene diamine solution are achieved, the discontinuity and purity reduction of the evaporation process in the prior art are solved, the device life is extended and impurities are effectively screened.
Patent Information
- Application Number
- CN202310205804.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-03-06
- Publication Date
- 2025-07-11
- Estimated Expiration
- 2043-03-06
AI Technical Summary
The prior art cannot achieve continuous evaporation and purification of diethyl toluene diamine solution, and the addition of low-temperature solutions during evaporation will lead to temperature interference and a decrease in purity.
The LC-grade diethyl toluene diamine purification device that progressively screens impurities is used to heat the solution in the purification chamber evenly through the heating plate, and accelerate evaporation with the stirring leaf and baffle structure. The condensation and reflux tube in the cooling shell are used to achieve continuous replenishment of the solution and gradual screening of impurities.
Continuous purification of diethyl toluenediamine solution is achieved, purity is improved to LC level, the service life of the device is extended, and impurities are effectively screened, avoiding temperature interference and resource waste.
Smart Images

Figure CN116173522B_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of purification devices for diethyltoluenediamine, and in particular to an LC-grade diethyltoluenediamine purification device and method for gradually screening impurities. Background Art
[0002] Diethyltoluenediamine is mainly used as a curing agent, antioxidant, chain extender, lubricant, etc. Its boiling point is 301.4°C. Diethyltoluenediamine has a wide range of uses in the chemical industry. In the upstream of its production industrial chain, ethylene and toluenediamine are mostly used as raw materials. The boiling point of toluenediamine is 280°C. Ethylene is introduced into toluenediamine under certain temperature conditions, and a corresponding catalyst is used to complete the preparation of diethyltoluenediamine. After the preparation is completed, the finished product therein needs to be purified. LC is an indication of a high-purity solution.
[0003] Existing purification methods include a condensing tower and an evaporation and condensation method. The specific process is as follows: The solution is added to the reactor at one time and heated. When the solution temperature reaches the boiling point, the solution evaporates to form steam, and the steam is condensed and recovered. However, currently, when evaporating the diethyltoluenediamine solution, only a certain amount of the solution can be uniformly evaporated and purified, and the continuity of evaporation cannot be achieved, that is, the solution cannot be added during the evaporation process. The specific reason is that since the evaporation process requires a relatively high temperature, and the added solution has a lower temperature, it will interfere with the temperature of the original solution in the container. Moreover, the inside of the container is generally a cylindrical cavity. When heating the solution, the solution in the middle of the container is far from the inner wall of the container, and the temperature rises slowly, resulting in the solution near the inner wall of the container evaporating first. The evaporated steam will carry the original solution that has not evaporated, resulting in the solution containing unpurified solution during the subsequent condensation process, reducing the purity of the solution. If a low-temperature solution is added again during this process, this phenomenon will be aggravated. Summary of the Invention
[0004] In order to solve the above technical problems, the present invention provides an LC-grade diethyltoluenediamine purification device and method for uniformly heating and gradually screening impurities.
[0005] The technical solution is as follows: an LC-grade diethyltoluenediamine purification device for progressively screening impurities, including legs, the legs are fixedly connected with a first evaporation housing, the first evaporation housing is fixedly connected with a control terminal, the first evaporation housing is provided with a liquid outlet, and the liquid outlet is provided with a solenoid valve electrically connected to the control terminal. A second evaporation housing is fixedly connected inside the first evaporation housing. Heating plates electrically connected to the control terminal are embedded in both the first evaporation housing and the second evaporation housing. A purification cavity is formed by the cooperation between the first evaporation housing and the second evaporation housing. The first evaporation housing is fixedly connected with a connecting housing through a gas pipe. The connecting housing is provided with a liquid inlet, and a solenoid valve is arranged in the liquid inlet. The gas pipe is fixedly connected with a cooling housing located inside the second evaporation housing. The gas pipe connects the cooling housing and the purification cavity. A preheating cavity is formed by the cooperation between the second evaporation housing and the cooling housing. A liquid level gauge electrically connected to the control terminal is arranged in the preheating cavity. The second evaporation housing is provided with a through groove, and a check valve is arranged in the through groove of the second evaporation housing. The through groove of the second evaporation housing connects the purification cavity and the preheating cavity. The cooling housing is rotatably connected with a rotating sleeve. The first evaporation housing is fixedly connected with a drain pipe rotatably connected with the rotating sleeve. The rotating sleeve and the drain pipe are both provided with through holes distributed circumferentially. The through holes of the rotating sleeve and the drain pipe are both located inside the cooling housing. Stirring blades evenly distributed circumferentially at equal intervals are all located in the preheating cavity. The stirring blades are provided with through holes, and one end of the stirring blades is fixedly connected with the rotating sleeve. The first evaporation housing is provided with a purification mechanism for accelerating the evaporation of the diethyltoluenediamine solution in the purification cavity. The heating plates in the first evaporation housing and the second evaporation housing uniformly heat the solution in the purification cavity from inside and outside.
[0006] Preferably, the purification mechanism includes a servo motor. The servo motor is fixedly connected to the first evaporation housing through a support plate. The output shaft of the servo motor is fixedly connected with a first gear. A second gear is rotatably connected between the first evaporation housing and the connecting housing. The second gear meshes with the first gear. The first evaporation housing is rotatably connected with rotating rods evenly distributed circumferentially at equal intervals. The rotating rods are fixedly connected with third gears meshing with the second gear. The rotating rods are fixedly connected with spiral blades located in the purification cavity. The spiral blades are provided with through holes. A lifting component for increasing the contact area between the diethyltoluenediamine solution and air is arranged in the purification cavity.
[0007] Preferably, the lifting component includes an isolation ring, which is fixedly connected to the first evaporation housing. The isolation ring is located inside the purification cavity and is rotatably connected to the rotating rod. The isolation ring divides the purification cavity into a first annular cavity and a second annular cavity. The first evaporation housing is rotatably connected with a first gear ring located inside the purification cavity, and the second evaporation housing is rotatably connected with a second gear ring located inside the purification cavity. The rotating rod is fixedly connected with a fourth gear, and the fourth gear meshes with the first gear ring and the second gear ring. The second gear ring is fixedly connected with first connecting rods evenly distributed at circumferential intervals, and the first connecting rods are fixedly connected with a first baffle. The first gear ring is fixedly connected with second connecting rods evenly distributed at circumferential intervals, and the second connecting rods are fixedly connected with a second baffle. The first baffle and the second baffle are both provided with water spraying holes distributed at equal intervals, and the water spraying holes on the first baffle and the second baffle are all located on the upper side. The first baffle and the second baffle evenly distributed at circumferential intervals divide the second annular cavity into a first evaporation cavity and a second evaporation cavity distributed alternately. The isolation ring is provided with through holes evenly distributed at circumferential intervals, and the through holes of the isolation ring communicate the first annular cavity with the first evaporation cavity.
[0008] Preferably, both the first baffle and the second baffle are set to be arc-shaped for spraying the diethyltoluenediamine solution onto the spiral blades.
[0009] Preferably, one end of the stirring blades evenly distributed at circumferential intervals is fixed on the second gear.
[0010] Preferably, the cooling housing is provided with condensation plates evenly distributed at equal intervals. The condensation plates are provided with condensation holes evenly distributed at circumferential intervals, and an arc-shaped groove evenly distributed at circumferential intervals is arranged on one side of the condensation plate close to the inner wall of the cooling housing.
[0011] Preferably, the condensation plate is set to be an upwardly convex umbrella-shaped structure for guiding the condensed diethyltoluenediamine solution.
[0012] Preferably, the condensation holes of adjacent condensation plates are distributed alternately for intercepting the condensed diethyltoluenediamine solution.
[0013] Preferably, the condensation plates evenly distributed at equal intervals are fixedly connected with circumferentially distributed return pipes, and the return pipes are fixedly connected with the cooling housing. The return pipes communicate the interior of the cooling housing with the preheating cavity.
[0014] The purification method of the LC-level diethyltoluenediamine purification device for gradually screening impurities includes the following steps:
[0015] S1. The operator first connects the container storing the diethyltoluenediamine solution with the liquid inlet, and then adds the solution into the preheating cavity. The operator starts two heating plates to assist in the purification of the solution in the purification cavity;
[0016] S2. During the purification of the solution, the first baffle and the second baffle rotate to stir the solution in the second annular cavity to accelerate the evaporation rate of the solution;
[0017] S3. The material vapor and water vapor formed after evaporation enter the cooling housing through the air duct. The material vapor condenses in the cooling housing to form a solution, and the water vapor flows back into the preheating cavity through the return pipe.
[0018] S4. As the solution evaporates, the liquid level of the solution in the purification cavity decreases. The preheating cavity is timely replenished with the solution through the liquid inlet to continuously purify the solution.
[0019] S5. After all the solution is purified, the operator resets the device.
[0020] The beneficial effects of the present invention are as follows: The present invention uniformly heats the solution in the purification cavity through two heating plates, accelerates the rising speed of the solution in the purification cavity, ensures that the solution in the purification cavity quickly rises to the boiling point, thereby improving the purity of the solution to the LC level. The continuous evaporation and purification process is achieved by continuously replenishing the solution in the second annular cavity. The cooling housing continuously adds water vapor to the preheating cavity, keeping the inside of the device moist, avoiding the dry state inside the device, preventing the heating plate from directly dry-burning the inner wall of the device, and improving the service life of the device. The stirring blade scrapes the impurities on the inner wall of the preheating cavity, and the scraped impurities are located at the bottom of the purification cavity. Secondly, the impurities in the second annular cavity are scraped by the first baffle and the second baffle to screen the impurities in a progressive form. Description of the Drawings
[0021] Figure 1 It is a three-dimensional structure diagram of the present invention.
[0022] Figure 2 It is a three-dimensional structure diagram of the purification mechanism of the present invention.
[0023] Figure 3 It is a three-dimensional structure diagram of the rotating sleeve and the drain pipe of the present invention.
[0024] Figure 4 It is a three-dimensional structure diagram of the lifting component of the present invention.
[0025] Figure 5 It is a three-dimensional structure diagram of parts such as the cooling housing and the stirring blade of the present invention.
[0026] Figure 6 It is a three-dimensional structure diagram of the first evaporation housing and the isolation ring of the present invention.
[0027] Names of the reference numerals in the figure: 1 - outrigger, 2 - first evaporation housing, 201 - liquid outlet, 202 - purification chamber, 2021 - first annular chamber, 2022 - second annular chamber, 203 - first evaporation chamber, 204 - second evaporation chamber, 3 - second evaporation housing, 301 - one-way valve, 302 - preheating chamber, 4 - gas guide pipe, 5 - connection housing, 501 - liquid inlet, 6 - cooling housing, 7 - rotating sleeve, 8 - drain pipe, 901 - servo motor, 902 - first gear, 903 - second gear, 904 - rotating rod, 905 - third gear, 906 - spiral blade, 1001 - isolation ring, 1002 - first toothed ring, 1003 - second toothed ring, 1004 - fourth gear, 1005 - first connecting rod, 1006 - first baffle, 1007 - second connecting rod, 1008 - second baffle, 11 - stirring blade, 12 - condensation pan, 13 - reflux pipe. Detailed implementation manner
[0028] The technical solutions in the embodiments of the present invention will be described clearly and completely below. Obviously, the described embodiments are only partial embodiments of the present invention, rather than all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention. Embodiment 1
[0029] The LC-grade diethyltoluenediamine purification device for gradually screening impurities is as Figures 1-3As shown in the figure, it includes a support leg 1. The upper end of the support leg 1 is welded with a first evaporation housing 2. The right side of the first evaporation housing 2 is connected with a control terminal by bolts. On the left side of the lower surface of the first evaporation housing 2, there is a liquid outlet 201. An electromagnetic valve electrically connected to the control terminal is arranged at the liquid outlet 201. A second evaporation housing 3 is welded inside the first evaporation housing 2. The upper side of the second evaporation housing 3 contacts the top inside the first evaporation housing 2. Heating plates electrically connected to the control terminal are embedded in both the first evaporation housing 2 and the second evaporation housing 3. The heating plates are located on the side walls of the first evaporation housing 2 and the second evaporation housing 3, not at the bottom, and are used to heat the solution inside the second evaporation housing 3. A purification cavity 202 is formed by the cooperation between the inner side surface of the first evaporation housing 2 and the outer side surface of the second evaporation housing 3. The purification cavity 202 is annular. The heating plates inside the first evaporation housing 2 and the second evaporation housing 3 uniformly heat the solution inside the purification cavity 202 from inside and outside to ensure that the solution inside the purification cavity 202 quickly rises to the boiling point. The first evaporation housing 2 is fixedly connected with a connection housing 5 through a gas guide pipe 4. The gas guide pipe 4 is L-shaped and is located above the first evaporation housing 2. The connection housing 5 is provided with a liquid inlet 501. An electromagnetic valve is arranged inside the liquid inlet 501. The gas guide pipe 4 communicates with a cooling housing 6 located inside the second evaporation housing 3. The gas guide pipe 4 connects the upper part of the cooling housing 6 with the purification cavity 202. A preheating cavity 302 is formed by the cooperation between the second evaporation housing 3 and the cooling housing 6. The liquid inlet 501 communicates with the preheating cavity 302. A liquid level gauge electrically connected to the control terminal (not shown in the figure) is arranged inside the preheating cavity 302. The liquid level gauge is used to monitor the liquid level height inside the preheating cavity 302. On the left side of the bottom of the second evaporation housing 3, there is a through groove. A one-way valve 301 is arranged in the through groove of the second evaporation housing 3. The through groove of the second evaporation housing 3 connects the purification cavity 202 with the preheating cavity 302. The bottom of the cooling housing 6 is rotatably connected through a rotating sleeve 7 in a penetrating manner. The first evaporation housing 2 is fixedly connected with a drain pipe 8. The drain pipe 8 is located inside the rotating sleeve 7 and is rotatably connected with it. The rotating sleeve 7 and the drain pipe 8 are both provided with through holes distributed circumferentially. The through holes of the rotating sleeve 7 and the drain pipe 8 are both located inside the cooling housing 6. When the through holes of the rotating sleeve 7 and the drain pipe 8 are communicated, the solution inside the cooling housing 6 is discharged from the through holes of the rotating sleeve 7 and the drain pipe 8. The first evaporation housing 2 is provided with a purification mechanism for accelerating the evaporation of the diethyltoluenediamine solution inside the purification cavity 202.
[0030] As Figures 1-5As shown in the figure, the purification mechanism includes a servo motor 901. The servo motor 901 is welded to the upper part on the left side of the first evaporation shell 2 through a support plate. A first gear 902 is key-connected to the output shaft of the servo motor 901. A second gear 903 is rotatably connected between the first evaporation shell 2 and the connection shell 5. The second gear 903 meshes with the first gear 902. Six rotating rods 904 are rotatably connected to the first evaporation shell 2 and are circumferentially and equally spaced. A third gear 905 that meshes with the second gear 903 is key-connected to the rotating rod 904. A spiral blade 906 located in the purification cavity 202 is fixedly connected to the rotating rod 904. The spiral blade 906 is provided with through holes. The rotation of the spiral blade 906 lifts the solution in the purification cavity 202 upward, accelerating the discharge of steam in the solution and disturbing the solution at the same time, accelerating the evaporation of the solution. A lifting component for increasing the contact area between the diethyltoluenediamine solution and air is arranged in the purification cavity 202.
[0031] As Figures 2-6As shown, the lifting component includes an isolation ring 1001. The isolation ring 1001 is welded to the first evaporation housing 2. The isolation ring 1001 is located at the lower part inside the purification cavity 202. The isolation ring 1001 is rotatably connected to the lower end of the rotating rod 904. The isolation ring 1001 divides the purification cavity 202 into a first annular cavity 2021 and a second annular cavity 2022. The first annular cavity 2021 is located on the lower side of the second annular cavity 2022. The first annular cavity 2021 is formed by the cooperation of the bottom of the first evaporation housing 2 and the second evaporation housing 3. The second annular cavity 2022 is formed by the cooperation of the side walls of the first evaporation housing 2 and the second evaporation housing 3. The first evaporation housing 2 is rotatably connected with a first gear ring 1002 located inside the purification cavity 202. The second evaporation housing 3 is rotatably connected with a second gear ring 1003 located inside the purification cavity 202. Both the first gear ring 1002 and the second gear ring 1003 are located on the upper side of the purification cavity 202. The rotating rod 904 is key-connected with a fourth gear 1004. The fourth gear 1004 meshes with the first gear ring 1002 and the second gear ring 1003. Six first connecting rods 1005 are welded to the second gear ring 1003 and are circumferentially equally spaced. A first baffle 1006 is welded to the first connecting rods 1005. Six second connecting rods 1007 are fixedly connected to the first gear ring 1002 and are circumferentially equally spaced. A second baffle 1008 is welded to the second connecting rods 1007. Both the first baffle 1006 and the second baffle 1008 are located inside the purification cavity 202. The widths of the first baffle 1006 and the second baffle 1008 are equal to the spacing between the first evaporation housing 2 and the second evaporation housing 3. Both the first baffle 1006 and the second baffle 1008 are provided with equally spaced spray holes. The spray holes on the first baffle 1006 and the second baffle 1008 are all located on the upper side. The solution is sprayed out through the multiple spray holes and sprayed towards the lower side of the second evaporation cavity 204. The steam in the solution contacts the air and directly moves upward and overflows from the solution, accelerating the evaporation rate of the solution. Both the first baffle 1006 and the second baffle 1008 are arranged in an arc shape. The sides of the first baffle 1006 and the second baffle 1008 close to the spiral blade 906 are both arranged as arc-shaped concave surfaces for spraying the diethyltoluenediamine solution towards the spiral blade 906. The solution discharged from the spray holes will be sprayed onto the rotating spiral blade 906. The rotating spiral blade 906 disperses the solution, further accelerating the evaporation of the solution. The first baffles 1006 and the second baffles 1008 that are circumferentially equally spaced divide the second annular cavity 2022 into alternately distributed first evaporation cavities 203 and second evaporation cavities 204. The numbers of both the first evaporation cavities 203 and the second evaporation cavities 204 are 6. The isolation ring 1001 is provided with through holes that are circumferentially equally spaced. The through holes of the isolation ring 1001 connect the first annular cavity 2021 with the first evaporation cavity 203 for replenishing the solution into the first evaporation cavity 203.
[0032] As Figure 5 andFigure 6 As shown, the second gear 903 is welded with stirring blades 11 evenly distributed at equal intervals in the circumferential direction. The stirring blades 11 evenly distributed at equal intervals in the circumferential direction are all located in the preheating cavity 302. The stirring blades 11 are provided with through holes. The lower ends of the stirring blades 11 are fixedly connected to the rotating sleeve 7. The stirring blades 11 drive the rotating sleeve 7 to rotate, and the through holes of the rotating sleeve 7 and the drain pipe 8 are gradually displaced.
[0033] As Figure 3 and Figure 6 As shown, condensation trays 12 are arranged at equal intervals in the cooling housing 6. The condensation trays 12 are provided with condensation holes evenly distributed in the circumferential direction. An arc-shaped groove evenly distributed in the circumferential direction is arranged on one side of the condensation tray 12 close to the inner wall of the cooling housing 6. The water vapor and steam (material) entering the cooling housing 6 first come into contact with the uppermost condensation tray 12. Since the temperature in the preheating cavity 302 is lower than 280 °C, and the temperature in the cooling housing 6 will also be lower than 280 °C, but the temperature will not be lower than 100 °C. Therefore, the temperature of the steam (material) decreases and gradually condenses into a solution. The condensation tray 12 is arranged in an upward convex umbrella-shaped structure. Therefore, the condensed solution will flow along the upper side surface of the condensation tray 12 towards the inner wall of the cooling housing 6, and then be transported downward through the arc-shaped groove of the condensation tray 12. The condensation holes of adjacent condensation trays 12 are staggered, increasing the moving path of the steam (material) and the residence time on the upper side in the cooling housing 6, avoiding too short condensation time of the steam (material), and the uncondensed steam (material) directly discharging downward through the return pipe 13 into the preheating cavity 302, resulting in a decrease in the solution content in the cooling housing 6.
[0034] As Figure 3 and Figure 6 As shown, the condensation trays 12 evenly distributed at equal intervals are welded with return pipes 13 distributed in the circumferential direction. The return pipes 13 are welded to the cooling housing 6. The return pipes 13 communicate the inside of the cooling housing 6 with the preheating cavity 302. The water vapor in the cooling housing 6 enters the preheating cavity 302 through the return pipes 13 to preheat the solution in the preheating cavity 302, assisting the evaporation of the solution and avoiding waste of resources caused by directly discharging the water vapor.
[0035] When continuous purification of diethyltoluenediamine is required, the operator first connects the container storing the diethyltoluenediamine solution to the liquid inlet 501. Hereinafter, the diethyltoluenediamine solution is referred to as "solution". Subsequently, the operator opens the solenoid valve in the liquid inlet 501 through the control terminal. The solution enters the preheating cavity 302 through the liquid inlet 501 and contacts the stirring blade 11. Due to the addition of the solution, the pressure on the upper side of the check valve 301 increases, and the check valve 301 opens. The solution in the preheating cavity 302 enters the first annular cavity 2021 through the through groove of the second evaporation housing 3. The solution in the first annular cavity 2021 enters the adjacent first evaporation cavity 203 through the six through holes of the isolation ring 1001. When the liquid level of the solution in the first evaporation cavity 203 is higher than the water spray holes of the first baffle 1006 and the second baffle 1008, the solution in the first evaporation cavity 203 enters the adjacent second evaporation cavity 204 through the water spray holes of the first baffle 1006 and the second baffle 1008. The solution in the second evaporation cavity 204 contacts the spiral blade 906. In the initial state, the through hole of the rotating sleeve 7 and the through hole of the drain pipe 8 are communicated. The air in the purification cavity 202 is squeezed by the solution and enters the upper part of the cooling housing 6 through the air guide pipe 4, enters the drain pipe 8 through the through hole of the rotating sleeve 7 and the through hole of the drain pipe 8 and is discharged. Since the preheating cavity 302 and the purification cavity 202 are communicated, when the liquid level detected by the liquid level gauge in the preheating cavity 302 is between the first gear ring 1002 and the spiral blade 906, the control terminal closes the solenoid valve in the liquid inlet 501, and no more solution is added to the preheating cavity 302. The control terminal starts the servo motor 901. The servo motor 901 drives the first gear 902 to rotate. The first gear 902 drives the stirring blade 11 to rotate through the second gear 903. The stirring blade 11 drives the rotating sleeve 7 to rotate. When the through hole of the rotating sleeve 7 is misaligned with the through hole of the drain pipe 8, the control terminal closes the servo motor 901, and the gas in the cooling housing 6 no longer discharges through the through holes of the rotating sleeve 7 and the drain pipe 8.
[0036] After the through holes of the rotating sleeve 7 and the drain pipe 8 are misaligned, the control terminal activates the heating plates in the first evaporation housing 2 and the second evaporation housing 3. The two heating plates heat the solution. Since the second annular cavity 2022 is located between the two heating plates, and the preheating cavity 302 is only close to the heating plate in the second evaporation housing 3, the temperature in the second annular cavity 2022 is higher than that in the preheating cavity 302. By setting the power of the two heating plates, the temperature in the second annular cavity 2022 is controlled to be higher than 301.4 °C (the boiling point of the solution), and the temperature in the preheating cavity 302 is lower than 280 °C (diethyltoluenediamine is in a liquid state). After a period of time, the solution in the second annular cavity 2022 reaches the boiling point, and the solution in the second annular cavity 2022 forms steam (material). At the same time, since the temperature in the second annular cavity 2022 is higher than 301.4 °C, and the boiling point of water in the solution is 100 °C, the water in the solution will also evaporate to form water vapor. The water vapor and steam (material) enter the cooling housing 6 through the air duct 4. The water vapor and steam (material) entering the cooling housing 6 first contact the uppermost condensation disk 12. Since the temperature in the preheating cavity 302 is lower than 280 °C, and the temperature in the cooling housing 6 will also be lower than 280 °C, but the temperature will not be lower than 100 °C, the steam (material) temperature decreases and gradually condenses into a solution. At this time, the solution is the purified solution, and since the temperature in the preheating cavity 302 is still higher than the boiling point of water, the water still exists in the form of water vapor in the cooling housing 6.
[0037] With the continuous generation of steam (material) in the second annular cavity 2022, the steam (material) moving downward in the cooling housing 6 continuously contacts the condensation disk 12. Since the condensation disk 12 is arranged in an upwardly convex umbrella-shaped structure, the condensed solution will flow along the upper side surface of the condensation disk 12 towards the inner wall of the cooling housing 6, and then be conveyed downward through the arc-shaped groove of the condensation disk 12. Moreover, the condensation holes of adjacent condensation disks 12 are staggered, increasing the moving path of the steam (material) and the residence time on the upper side in the cooling housing 6, avoiding the steam (material) having too short a condensation time and the uncondensed steam (material) directly flowing downward through the return pipe 13 into the preheating cavity 302, resulting in a decrease in the solution content in the cooling housing 6 and a reduction in the solution purification efficiency.
[0038] As the amount of water vapor in the cooling housing 6 increases, the water vapor in the cooling housing 6 enters the upper part of the preheating cavity 302 through the return pipe 13. The water vapor entering the preheating cavity 302 preheats the solution that has not been purified. In summary, first, the solution is preheated in the preheating cavity 302 to raise the preheating temperature to near the boiling point, ensuring that the solution entering the second annular cavity 2022 is in a high-temperature state. Second, since the solution is added from the upper side of the preheating cavity 302 and discharged from the lower side, the solution is already close to the boiling point of the solution during the downward movement. The solution added to the preheating cavity 302 subsequently will not affect the temperature of the solution on the lower side, providing a preheating condition for the subsequent evaporation of the solution. In this way, the temperature is gradually increased to eliminate the temperature interference caused by the solution added subsequently to the solution during the evaporation process. The heat in the water vapor is used to preheat the solution that has not been purified to assist the evaporation of the solution and avoid wasting resources by directly discharging the water vapor.
[0039] During the evaporation of the solution in the second annular cavity 2022, the control terminal starts the servo motor 901, and the second gear 903 drives six third gears 905 to rotate. Taking one of the third gears 905 as an example, the third gear 905 drives the fourth gear 1004 to rotate counterclockwise through the rotating rod 904, the rotating rod 904 drives the spiral blade 906 to rotate, the fourth gear 1004 drives the first toothed ring 1002 to rotate counterclockwise, the fourth gear 1004 drives the second toothed ring 1003 to rotate clockwise, the first toothed ring 1002 drives the second baffle 1008 to rotate counterclockwise through the second connecting rod 1007, and the second toothed ring 1003 drives the first baffle 1006 to rotate clockwise through the first connecting rod 1005. The first baffle 1006 and the second baffle 1008 adjacent to the same spiral blade 906 move away from each other, the volume of the second evaporation cavity 204 increases, the volume of the first evaporation cavity 203 decreases, the pressure of the solution in the first evaporation cavity 203 gradually increases due to the extrusion force of the adjacent first baffle 1006 and second baffle 1008, and is discharged into the adjacent second evaporation cavity 204 through the water spraying holes of the first baffle 1006 and the second baffle 1008.
[0040] Since the water spray holes on the first baffle 1006 and the second baffle 1008 are located on the upper side, the solution is discharged from the upper sides of the first baffle 1006 and the second baffle 1008. The solution is ejected through a plurality of water spray holes and sprayed downward onto the second evaporation cavity 204. The steam in the solution contacts the air and moves directly upward, reducing the residence time of the steam in the solution and overflowing from the solution, which accelerates the evaporation of the solution. If the solution forms steam, the steam will evaporate and overflow from the uppermost side of the solution surface. However, the steam inside the solution needs to move to the upper side of the liquid surface, which slows down the overflow speed of the steam and affects the evaporation efficiency of the solution. Since the sides of the first baffle 1006 and the second baffle 1008 close to the spiral blade 906 are both set as arc-shaped concave surfaces, the solution discharged from the water spray holes will be sprayed onto the rotating spiral blade 906. The rotating spiral blade 906 disperses the solution, further accelerating the evaporation of the solution. Moreover, when the first baffle 1006 and the second baffle 1008 adjacent to the same spiral blade 906 approach each other, the first baffle 1006 and the second baffle 1008 wrap the spiral blade 906. Since the spiral blade 906 is spiral-shaped, the rotating blade will drive the solution to move upward, thereby turning the solution on the lower side to the upper side, facilitating the discharge of the steam attached to the solution inside. When the first connecting rod 1005 and the second connecting rod 1007 in the same first evaporation cavity 203 come into contact, the content of the solution in the second evaporation cavity 204 is greater than that in the first evaporation cavity 203. Subsequently, the control terminal reversely rotates the first gear 902 through the servo motor 901, and the first baffle 1006 and the second baffle 1008 gradually approach the spiral blade 906. The solution in the second evaporation cavity 204 enters the adjacent first evaporation cavity 203 through the water spray holes, further accelerating the evaporation of the solution in the second evaporation cavity 204.
[0041] During the clockwise rotation of the second gear 903, the second gear 903 drives the rotating sleeve 7 to rotate through the stirring blade 11. The through-hole of the rotating sleeve 7 gradually communicates with the through-hole of the drain pipe 8. When the through-hole of the rotating sleeve 7 gradually communicates with the through-hole of the drain pipe 8, the solution on the lower side in the cooling housing 6 is discharged from the through-holes of the rotating sleeve 7 and the drain pipe 8 and enters the drain pipe 8. The operator collects the solution discharged from the drain pipe 8, and part of the solution is purified. When the second gear 903 rotates clockwise, the through-hole of the rotating sleeve 7 is misaligned with the through-hole of the drain pipe 8. By periodically communicating the through-hole of the rotating sleeve 7 with the through-hole of the drain pipe 8, the discharge of the solution in the cooling housing 6 is assisted, ensuring that the height of the solution level in the cooling housing 6 is lower than that of the return pipe 13, and preventing the height of the solution level in the cooling housing 6 from being higher than the lower end of the return pipe 13 to block it, so that the subsequent water vapor cannot flow back into the preheating cavity 302 through the return pipe 13. If the through-hole of the rotating sleeve 7 is continuously communicated with the through-hole of the drain pipe 8 for a long time, the water vapor will be directly discharged through the drain pipe 8, resulting in waste of water vapor. Therefore, by intermittently communicating the through-hole of the rotating sleeve 7 with the through-hole of the drain pipe 8, while ensuring that the solution level in the cooling housing 6 is lower than the return pipe 13, the waste of water vapor is avoided.
[0042] Since some of the solution and water in the second annular cavity 2022 are evaporated, the content of the solution in the second annular cavity 2022 decreases. At this time, when the solution in the second annular cavity 2022 decreases to a certain amount, since the solution level in the second annular cavity 2022 is lower than the solution level in the preheating cavity 302, the pressure on the upper side of the one-way valve 301 is greater than that on its lower side, and the one-way valve 301 opens. At this time, the solution preheated in the preheating cavity 302 enters the first annular cavity 2021 through the through-groove of the second evaporation housing 3 and enters the first evaporation cavity 203 through the through-hole of the isolation ring 1001 to supplement the solution in the second annular cavity 2022. Since the solution in the preheating cavity 302 decreases, the liquid level gauge in the preheating cavity 302 detects that the liquid level has decreased, and the liquid level gauge transmits the data to the control terminal. The control terminal opens the solenoid valve at the liquid inlet 501 to supplement the solution in the preheating cavity 302. When the solution level in the preheating cavity 302 reaches the specified height, the control terminal closes the solenoid valve at the liquid inlet 501, and the continuous evaporation and purification process is realized by continuously supplementing the solution in the second annular cavity 2022.
[0043] The operator intermittently starts the servo motor 901, and the stirring blade 11 in the preheating cavity 302 will rotate intermittently, making the solution in the preheating cavity 302 evenly heated, so as to accelerate the evaporation of the solution. Since the temperature in the second annular cavity 2022 is provided by two heating plates and the second annular cavity 2022 is annular, the distance between the solution in the middle of the second annular cavity 2022 and the two heating plates is equal and short. Therefore, the solution in the second annular cavity 2022 will be evenly heated, ensuring that the solution in the second annular cavity 2022 is quickly raised to the boiling point, and the purity of the solution is successively raised to the LC level, avoiding the temperature in the middle of the solution being lower than the temperature near the inner wall of the container and unable to achieve uniform heating. Moreover, the solution containing the solution that has not reached the evaporation temperature will cause the steam formed by the solution that has reached the boiling point. During the process of the steam overflowing from the solution, some liquid components that have not reached the evaporation temperature will be carried away, resulting in some solutions being directly discharged without evaporation and purification, reducing the purity of the solution after subsequent purification. Since the added solution contains impurities, impurities will exist in both the second annular cavity 2022 and the preheating cavity 302, and some impurities will adhere to the inner walls of the second annular cavity 2022 and the preheating cavity 302. Therefore, first, the impurities on the inner wall of the preheating cavity 302 are scraped off by the stirring blade 11, and the scraped impurities are located at the bottom of the second annular cavity 2022. Secondly, the impurities in the second annular cavity 2022 are scraped off by the first baffle 1006 and the second baffle 1008. Through preheating and purification in the preheating cavity 302, some impurities are retained in the preheating cavity 302, and then evaporation and purification are carried out through the second annular cavity 2022. And the increase in temperature will reduce the adhesion of impurities. Therefore, during the process of gradual purification, the gradual separation of impurities is realized, and the impurities are screened in a progressive form to assist in the discharge of impurities in the solution.
[0044] Since the cooling housing 6 continuously adds water vapor into the preheating cavity 302, the inside of the device is kept in a moist state, avoiding the dry state inside the device, causing the heating plate to directly dry-burn the inner wall of the device, and improving the service life of the device. When the solution purification is completed, the control terminal turns off the two heating plates. After a period of time, the water vapor in the device forms liquid water, and the control terminal opens the solenoid valve at the liquid outlet 201, and the water in the device carries impurities and is discharged. After the device is used, the operator resets the device. Embodiment 2
[0045] Based on Embodiment 1, the purification method of the LC-level diethyltoluenediamine purification device for progressively screening impurities includes the following steps:
[0046] S1. First, the operator connects the container storing the diethyltoluenediamine solution to the liquid inlet 501, and then adds the solution into the preheating cavity 302. The operator starts the two heating plates to assist in the purification of the solution in the purification cavity 202;
[0047]
[0047] In the process of solution purification, the first baffle 1006 and the second baffle 1008 rotate to stir the solution in the second annular cavity 2022, accelerating the evaporation rate of the solution;
[0048]
[0048] The material vapor and water vapor formed after evaporation enter the cooling housing 6 through the gas guide pipe 4. The material vapor condenses into a solution in the cooling housing 6, and the water vapor returns to the preheating cavity 302 through the return pipe 13;
[0049]
[0049] As the solution evaporates, the liquid level of the solution in the purification cavity 202 decreases. The solution is timely replenished into the preheating cavity 302 through the liquid inlet 501 to continuously purify the solution;
[0050]
[0050] After all the solution is purified, the operator resets the device.
[0051] The above embodiments are provided for those skilled in the art to implement or use the present invention. Those skilled in the art can make various modifications or changes to the above embodiments without departing from the inventive concept of the present invention. Therefore, the protection scope of the present invention is not limited by the above embodiments, but should be the maximum scope that conforms to the innovative features mentioned in the claims.
Claims
1. An LC-grade diethyltoluenediamine purification device for gradually screening impurities, comprising legs (1), the legs (1) being fixedly connected to a first evaporation housing (2), the first evaporation housing (2) being fixedly connected to a control terminal, the first evaporation housing (2) being provided with a liquid outlet (201), and the liquid outlet (201) being provided with an electromagnetic valve electrically connected to the control terminal, characterized in that: A second evaporation housing (3) is fixedly connected inside the first evaporation housing (2). Heating plates electrically connected to the control terminal are embedded in both the first evaporation housing (2) and the second evaporation housing (3). A purification cavity (202) is formed by the cooperation between the first evaporation housing (2) and the second evaporation housing (3). The first evaporation housing (2) is fixedly connected to a connection housing (5) through a gas guide pipe (4). The connection housing (5) is provided with a liquid inlet (501), and a solenoid valve is arranged in the liquid inlet (501). The gas guide pipe (4) is fixedly connected to a cooling housing (6) located inside the second evaporation housing (3). The gas guide pipe (4) connects the cooling housing (6) and the purification cavity (202). A preheating cavity (302) is formed by the cooperation between the second evaporation housing (3) and the cooling housing (6). A liquid level gauge electrically connected to the control terminal is arranged in the preheating cavity (302). The second evaporation housing (3) is provided with a through groove, and a check valve (301) is arranged in the through groove of the second evaporation housing (3). The through groove of the second evaporation housing (3) connects the purification cavity (202) and the preheating cavity (302). The cooling housing (6) is rotatably connected to a rotating sleeve (7). The first evaporation housing (2) is fixedly connected to a drain pipe (8) rotatably connected to the rotating sleeve (7). The rotating sleeve (7) and the drain pipe (8) are both provided with through holes distributed circumferentially. The through holes of the rotating sleeve (7) and the drain pipe (8) are both located inside the cooling housing (6). Stirring blades (11) evenly distributed at equal circumferential intervals are all located inside the preheating cavity (302). The stirring blades (11) are provided with through holes, and one end of the stirring blades (11) is fixedly connected to the rotating sleeve (7). The first evaporation housing (2) is provided with a purification mechanism for accelerating the evaporation of the diethyltoluenediamine solution in the purification cavity (202). The heating plates inside the first evaporation housing (2) and the second evaporation housing (3) uniformly heat the solution in the purification cavity (202) from inside and outside; The purification mechanism includes a servo motor (901). The servo motor (901) is fixedly connected to the first evaporation housing (2) through a support plate. The output shaft of the servo motor (901) is fixedly connected to a first gear (902). A second gear (903) is rotatably connected between the first evaporation housing (2) and the connection housing (5). The second gear (903) meshes with the first gear (902). The first evaporation housing (2) is rotatably connected to rotating rods (904) evenly distributed at equal circumferential intervals. The rotating rods (904) are fixedly connected to third gears (905) meshing with the second gear (903). The rotating rods (904) are fixedly connected to spiral blades (906) located inside the purification cavity (202). The spiral blades (906) are provided with through holes. A lifting component for increasing the contact area between the diethyltoluenediamine solution and air is arranged inside the purification cavity (202); The lifting component includes an isolation ring (1001). The isolation ring (1001) is fixedly connected to the first evaporation housing (2). The isolation ring (1001) is located inside the purification cavity (202). The isolation ring (1001) is rotatably connected to the rotating rod (904). The isolation ring (1001) divides the purification cavity (202) into a first annular cavity (2021) and a second annular cavity (2022). The first evaporation housing (2) is rotatably connected to a first gear ring (1002) located inside the purification cavity (202). The second evaporation housing (3) is rotatably connected to a second gear ring (1003) located inside the purification cavity (202). The rotating rod (904) is fixedly connected to a fourth gear (1004). The fourth gear (1004) meshes with the first gear ring (1002) and the second gear ring (1003). The second gear ring (1003) is fixedly connected to first connecting rods (1005) that are circumferentially and equally spaced. The first connecting rods (1005) are fixedly connected to a first baffle (1006). The first gear ring (1002) is fixedly connected to second connecting rods (1007) that are circumferentially and equally spaced. The second connecting rods (1007) are fixedly connected to a second baffle (1008). Both the first baffle (1006) and the second baffle (1008) are provided with spray holes that are equally spaced. The spray holes on the first baffle (1006) and the second baffle (1008) are all located on the upper side. The circumferentially and equally spaced first baffles (1006) and second baffles (1008) divide the second annular cavity (2022) into an alternately distributed first evaporation cavity (203) and a second evaporation cavity (204). The isolation ring (1001) is provided with through holes that are circumferentially and equally spaced. The through holes of the isolation ring (1001) connect the first annular cavity (2021) with the first evaporation cavity (203).
2. The LC-level diethyltoluenediamine purification device for gradually screening impurities according to claim 1, characterized in that: Both the first baffle (1006) and the second baffle (1008) are set to be arc-shaped for spraying the diethyltoluenediamine solution onto the spiral blade (906).
3. The LC-level diethyltoluenediamine purification device for progressively screening impurities according to claim 2, wherein: One end of the stirring blades (11) that are circumferentially and equally spaced is fixed on the second gear (903).
4. The LC-level diethyltoluenediamine purification device for gradually screening impurities according to claim 3, wherein: The cooling housing (6) is internally provided with condensation trays (12) that are equally spaced. The condensation trays (12) are provided with condensation holes that are circumferentially and equally spaced. On one side of the condensation trays (12) close to the inner wall of the cooling housing (6), there are arc-shaped grooves that are circumferentially and equally spaced.
5. The LC-level diethyltoluenediamine purification device for gradually screening impurities according to claim 4, wherein: The condensation trays (12) are set to be an upwardly convex umbrella-like structure for guiding the condensed diethyltoluenediamine solution.
6. The LC-level diethyltoluenediamine purification device for gradually screening impurities according to claim 5, wherein: The condensation holes of adjacent condensation trays (12) are staggeredly distributed for intercepting the condensed diethyltoluenediamine solution.
7. The LC-level diethyltoluenediamine purification device for gradually screening impurities according to claim 6, characterized in that: The equally spaced condensation trays (12) are fixedly connected to circumferentially distributed return pipes (13). The return pipes (13) are fixedly connected to the cooling housing (6). The return pipes (13) connect the interior of the cooling housing (6) with the preheating cavity (302).
8. The purification method of the LC-grade diethyltoluenediamine purification device for gradually screening impurities according to claim 7, characterized in that: It includes the following steps: S1: The operator first connects the container storing the diethyltoluenediamine solution to the liquid inlet (501), and then adds the solution into the preheating cavity (302). The operator starts two heating plates to assist in the purification of the solution inside the purification cavity (202). S2: During the process of solution purification, the first baffle (1006) and the second baffle (1008) rotate to stir the solution in the second annular cavity (2022), accelerating the evaporation rate of the solution; S3: The material vapor and water vapor formed after evaporation enter the cooling housing (6) through the gas guide pipe (4). The material vapor condenses into a solution in the cooling housing (6), and the water vapor then returns to the preheating cavity (302) through the return pipe (13); S4: As the solution evaporates, the liquid level of the solution in the purification cavity (202) decreases. The solution is replenished into the preheating cavity (302) in a timely manner through the liquid inlet (501) to continuously purify the solution; S5: After all the solution is purified, the operator resets the device.
Citation Information
Patent Citations
Evaporation and purification circulating device applied to NMP (N-Methyl Pyrrolidone) recovery
CN215387594U