Anti-adhesion purification device for LC grade diethyltoluenediamine
By designing an anti-adhesive purification device for LC-grade diethyl toluene diamine, using components such as spoiler units and flow guide shells, the scaling problem caused by impurities precipitation during distillation and purification is solved, and the effect of improving heat exchange efficiency and extending the running time of the device is achieved.
Patent Information
- Application Number
- CN202510475414.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-04-16
- Publication Date
- 2025-06-06
- Estimated Expiration
- 2045-04-16
AI Technical Summary
In the existing distillation and purification technology, crystals are precipitated by trace impurities during high-temperature evaporation, resulting in a decrease in heat transfer efficiency, and the device is scaled, affecting continuous production efficiency.
An anti-adhesion purification device for LC-grade diethyl toluene diamine is designed, and the distillation tank, heating parts, spoiler units and other components are used to increase the solution flow rate and shear force through the rotation of the first rectangular plate and the design of the flow guide shell, and peel off the loose crystals attached to the inner wall, delaying the scaling rate.
It effectively extends the continuous operation time of the device, improves heat exchange efficiency, reduces heat transfer thermal resistance, and ensures production efficiency.
Smart Images

Figure CN119971531B_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of chemical purification, in particular to an anti-adhesion purification device for LC-grade diethyltoluenediamine. Background Art
[0002] Diethyltoluenediamine (DETDA) is a key chain extender and antioxidant for polyurethane materials, and its purity directly affects the performance stability of downstream products. At present, the industry generally uses distillation purification technology to purify diethyltoluenediamine vapor from the organic phase solution after the alkylation reaction. It evaporates by heating to the boiling point of DETDA and then condenses to recover high-purity components. However, this process has significant defects in actual operation: trace impurities in the base solution (such as unreacted monomers or by-product salts) precipitate crystals due to a sudden change in solubility during high-temperature evaporation. These crystals are deposited on the inner wall of the distillation device with high adhesion, forming a dense insulation layer, resulting in an exponential decay in heat transfer efficiency.
[0003] As the thermal resistance increases, the heating unit needs to continuously increase energy consumption to maintain the system temperature. However, due to the hysteresis effect of heat conduction, the temperature of the solution will still deviate from the set boiling point, causing a sudden drop in the evaporation rate or even process interruption. More seriously, crystal deposition is cumulative. After multiple productions, the thickness of the scale on the inner wall can reach millimeters, forcing the device to be frequently shut down for cleaning, greatly reducing the efficiency of continuous production. Summary of the invention
[0004] The object of the present invention is to provide an anti-sticking purification device for LC-grade diethyltoluenediamine to solve the problems raised in the above-mentioned background technology.
[0005] The technical scheme of the present invention is: an anti-adhesion purification device for LC-grade diethyltoluenediamine, comprising a distillation tank, on which uniformly distributed heating elements are arranged, the lower part of the distillation tank is connected with a liquid injection pipe and a liquid discharge pipe, the upper part of the distillation tank is connected with a first exhaust pipe and a second exhaust pipe, and a flow disturbance unit is arranged in the distillation tank;
[0006] The spoiler unit includes a rotating sleeve, which is sealingly rotatably connected in the distillation tank, the rotating sleeve is provided with a through hole, the rotating sleeve and the distillation tank form an annular cavity, the distillation tank is equipped with a driving motor, the output shaft of the driving motor penetrates the distillation tank and is sealingly rotatably connected thereto, the output shaft of the driving motor and the rotating sleeve are driven by a gear set, the rotating sleeve is fixedly connected to a fixing frame, the fixing frame is fixedly connected to a first fixing rod, the first fixing rod is provided with a first rectangular plate, and there is a gap between the first rectangular plate and the distillation tank.
[0007] Preferably, the first rectangular plate is arranged to be inclined, and the first rectangular plate is used to drive the liquid to flow toward the middle of the distillation tank.
[0008] Preferably, it also includes:
[0009] A guide shell is fixedly connected to the rotating sleeve, and the upper surface of the guide shell is connected to the lower edge of the through hole;
[0010] The first fixed shell is fixedly connected to the distillation tank, and the first fixed shell is located outside the guide shell.
[0011] Preferably, it also includes:
[0012] A second fixing rod, fixedly connected to the fixing frame;
[0013] The second rectangular plate is arranged on the second fixing rod, and the second rectangular plate is used for stirring the solution in the annular cavity.
[0014] Preferably, an annular baffle is fixedly connected inside the distillation tank, the annular baffle is located below the fixing frame, and the inner side of the annular baffle is lower than the outer side thereof.
[0015] Preferably, a section of the rotating sleeve facing the first rectangular plate is a diameter-reducing section, and the diameter of the diameter-reducing section of the rotating sleeve gradually decreases from top to bottom.
[0016] Preferably, it also includes:
[0017] A sliding frame is slidably arranged on the fixed frame, the first fixing rod is rotatably connected to the first rectangular plate, the second fixing rod is rotatably connected to the second rectangular plate, the first rectangular plate and the second rectangular plate are both provided with horizontal grooves, and the horizontal grooves of the first rectangular plate and the horizontal grooves of the second rectangular plate are both slidably connected to the sliding frame;
[0018] A rotating frame, rotatably disposed on the distillation tank, the rotating frame is provided with a guide groove, and the sliding frame is located in the guide groove of the rotating frame and slides;
[0019] A rotating ring, rotatably disposed on the rotating frame, and rotatably connected to the distillation tank, wherein the distillation tank is provided with a vertical groove, and the rotating ring and the rotating frame are both used to cover the vertical groove on the distillation tank;
[0020] The driving member is fixedly connected to the outer side of the distillation tank and is used for driving the rotating ring to move.
[0021] Preferably, the first rectangular plate is provided with a plurality of evenly distributed first flow guide holes, and the second rectangular plate is provided with a plurality of evenly distributed second flow guide holes.
[0022] Preferably, it also includes:
[0023] A second fixed shell is fixedly connected to the upper part of the rotating sleeve, the injection pipe and the first exhaust pipe are both connected to the interior of the rotating sleeve, the discharge pipe and the second exhaust pipe are both connected to the annular cavity, and a plurality of connecting rods are arranged on the outer side of the second fixed shell;
[0024] A fixing sleeve is fixedly connected to all the connecting rods, an upper surface of the fixing sleeve is in contact with the distillation tank, and a lower edge of the fixing sleeve is lower than a lower edge of the through hole.
[0025] Preferably, the second fixing shell is fixedly connected to a third fixing shell, and the third fixing shell is located above the connecting rod.
[0026] Compared with the prior art, the present invention has the following advantages: 1. The present invention allows the solution to quickly pass through the gap between the first rectangular plate and the distillation tank by rotating the first rectangular plate. According to the continuity equation, due to the narrowness of the gap, the flow rate of the solution passing through the gap is significantly increased, and the loose crystal deposits attached to the inner wall are peeled off by the shearing action during the flow of the solution, which effectively slows down the scaling rate. This helps to reduce the heat transfer resistance, improve the heat exchange efficiency, extend the effective continuous operation time of the device, and ensure production efficiency;
[0027] 2. The present invention increases the surface area of the solution and improves the purification efficiency by guiding the flow through the guide shell and the first fixed shell;
[0028] 3. The present invention controls the swing angles of the first rectangular plate and the second rectangular plate through the operation of the driving member, changes the movement mode of the solution in the annular cavity, controls the temperature of the solution in the annular cavity to be consistent, improves the distillation and purification efficiency, and at the same time, changes the rotation direction of the solution to accelerate and guide the discharge of crystallized impurities;
[0029] 4. The present invention slowly heats the newly injected solution through the separation of the rotating sleeve to avoid affecting the evaporation and purification efficiency of the solution at a suitable temperature. The second fixed shell and the fixed sleeve are used for diversion to separate the inner cavity of the rotating sleeve from the annular cavity, and the water vapor is pre-separated from the solution in the inner cavity of the rotating sleeve, thereby reducing the workload of the subsequent condenser and improving the overall efficiency. BRIEF DESCRIPTION OF THE DRAWINGS
[0030] Figure 1 It is a schematic diagram of the three-dimensional structure of the present invention;
[0031] Figure 2 It is a schematic diagram of the three-dimensional structure of the guide shell and the first fixed shell of the present invention;
[0032] Figure 3 It is a cross-sectional view of the distillation tank and the rotating sleeve of the present invention;
[0033] Figure 4 It is a schematic diagram of the three-dimensional structure of the first rectangular plate and the second rectangular plate of the present invention;
[0034] Figure 5 It is a cross-sectional view of the fixed frame and the rotating frame of the present invention;
[0035] Figure 6 An exploded view of the second rectangular plate and the sliding frame of the present invention;
[0036] Figure 7 It is a cross-sectional view of the rotating sleeve and the fixed sleeve of the present invention;
[0037] Figure 8 It is a cross-sectional view of the second fixed shell and the third fixed shell of the present invention.
[0038] In the figure: 1. distillation tank, 2. injection pipe, 3. discharge pipe, 4. first exhaust pipe, 5. second exhaust pipe, 6. rotating sleeve, 601, through hole, 602, annular cavity, 7. drive motor, 9. fixed frame, 10. first fixed rod, 11. first rectangular plate, 1101, first guide hole, 12. guide shell, 13. first fixed shell, 14. second fixed rod, 15. second rectangular plate, 1501, second guide hole, 16. annular baffle, 17. sliding frame, 18. rotating frame, 19. rotating ring, 20. driving member, 21. second fixed shell, 22. connecting rod, 23. fixed sleeve, 24. third fixed shell. DETAILED DESCRIPTION
[0039] In order to make the purpose, technical solution and advantages of the present invention more clearly understood, the present invention is further described in detail below in conjunction with the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not used to limit the present invention. Example 1
[0040] This embodiment discloses an anti-sticking purification device for LC-grade diethyltoluenediamine, which is used to extract the diethyltoluenediamine component from the organic phase solution (hereinafter referred to as the solution) after the alkylation reaction.
[0041] The specific structure and connection relationship of the purification device are as follows:
[0042] like Figure 1-Figure 3 As shown, the purification device includes a distillation tank 1, which is fixedly connected to and communicates with an injection pipe 2, a discharge pipe 3, a first exhaust pipe 4 and a second exhaust pipe 5, wherein the injection pipe 2 and the discharge pipe 3 are located at the lower part of the distillation tank 1, the first exhaust pipe 4 and the second exhaust pipe 5 are located at the upper part of the distillation tank 1, a plurality of evenly distributed heating elements are arranged on the outer side surface of the distillation tank 1, and a turbulence unit is arranged inside the distillation tank 1.
[0043] like Figure 1-Figure 3As shown, the spoiler unit includes a rotating sleeve 6, which is sealed and rotatably connected to the distillation tank 1. The rotating sleeve 6 is provided with four through holes 601 equidistantly distributed in the circumferential direction (the number is the number shown in the figure, and the actual number can be set accordingly according to needs. The subsequent number is expressed in the same way. The parts expressed in the following increased number can also work when there is one of them). The through hole 601 is located at the upper part of the rotating sleeve 6 and is used to increase the retention time of the injected solution in the distillation tank 1. The rotating sleeve 6 and the distillation tank 1 form an annular cavity 602. The through hole 601 is used to connect the interior of the rotating sleeve 6 with the annular cavity 602 The distillation tank 1 is equipped with a driving motor 7, the output shaft of the driving motor 7 penetrates the distillation tank 1 and is sealed and rotatably connected thereto, the output shaft of the driving motor 7 and the rotating sleeve 6 are driven by a gear set, the lower part of the rotating sleeve 6 is fixedly connected with two fixing frames 9, the fixing frames 9 are located below the through hole 601, the two fixing frames 9 are commonly fixedly connected with four first fixing rods 10 equidistantly distributed in the circumferential direction, the first fixing rods 10 are provided with a first rectangular plate 11, there is a gap between the first rectangular plate 11 and the distillation tank 1, the first rectangular plate 11 is arranged in an inclined shape, when the four first rectangular plates 11 rotate clockwise (with the first rectangular plate 11 being attached to the distillation tank 1), the first rectangular plate 11 is arranged in an inclined shape, and when the four first rectangular plates 11 rotate clockwise (with the first rectangular plate 11 being attached to the distillation tank 1), the first rectangular plate 11 is arranged in an inclined shape, and when the four first rectangular plates 11 rotate clockwise (with the first rectangular plate 11 being attached to the distillation tank 1), the first rectangular plate 11 is arranged in an inclined shape, and the first rectangular plate 11 is arranged in an inclined shape, when the ... Figure 2 (viewed from top to bottom in the middle direction), the four first rectangular plates 11 are used to drive the solution to flow toward the middle of the distillation tank 1.
[0044] The working process of the purification device in this embodiment is as follows:
[0045] Purification preparation:
[0046] The conduit and the pump body are placed adjacent to the injection pipe 2, the discharge pipe 3 is connected to the pipeline where the control valve is installed, and the first exhaust pipe 4 and the second exhaust pipe 5 are connected to the condenser through pipelines respectively.
[0047] Purification starts:
[0048] The pump body, condenser, heater and drive motor 7 are started, wherein the heater works to create the evaporation temperature of diethyltoluenediamine in the distillation tank 1, and then the pump body works to inject the solution into the rotating sleeve 6 through the injection pipe 2. When the liquid level of the solution in the rotating sleeve 6 reaches the through hole 601, the solution flows downward from the through hole 601 and fills the annular cavity 602, wherein the control valve is first in a closed state. During this process, the temperature in the distillation tank 1 causes the diethyltoluenediamine in the solution to evaporate. After evaporation, the diethyltoluenediamine vapor flows upward and enters the condenser through the first exhaust pipe 4 and the second exhaust pipe 5. The condenser works to condense the diethyltoluenediamine vapor into liquid, and then after the remaining existing treatments, the purification operation of diethyltoluenediamine is finally completed.
[0049] During the solution injection process, when the liquid level of the solution in the annular cavity 602 exceeds the uppermost fixed frame 9, the control valve is opened so that the volume of the solution discharged from the discharge pipe 3 is the same as the volume of the solution injected into the injection pipe 2, and the solution at the bottom of the annular cavity 602 is discharged through the discharge pipe 3 for the remaining existing treatment. During this process, the liquid level of the solution in the annular cavity 602 remains relatively unchanged, and this process forms a continuous flow of the solution, thereby realizing a continuous purification operation.
[0050] During the continuous flow of the solution, the output shaft of the driving motor 7 drives the rotating sleeve 6, the fixing frame 9, the first fixing rod 10 and the first rectangular plate 11 to rotate clockwise (with the attached Figure 2 Taking the middle direction as an example and looking from top to bottom), the first rectangular plate 11 rotates to stir the solution in the annular cavity 602 to rotate, so that the temperature of the solution in the annular cavity 602 remains relatively uniform and consistent. At the same time, according to the continuity equation, the flow rate of the solution passing through the gap between the first rectangular plate and the distillation tank will increase significantly. At this time, the shear force generated during the rapid flow of the solution is used to peel off the loose crystal deposits attached to the inner wall, effectively delaying the scaling rate, extending the effective continuous operation time of the device, and ensuring production efficiency. Example 2
[0051] This embodiment discloses an anti-sticking purification device for LC-grade diethyltoluenediamine, which is further improved on the basis of Example 1.
[0052] The structure, connection relationship, and working process of the purification device in Example 1 will not be described in detail, and the working principle of the following structure will be explained in detail, and the same applies to the subsequent embodiments.
[0053] like Figure 2 and Figure 3 As shown, a guide shell 12 is fixedly connected to the side wall of the rotating sleeve 6, and the upper surface of the guide shell 12 is connected to the lower edge of the through hole 601; a first fixed shell 13 is fixedly connected to the distillation tank 1, and the first fixed shell 13 is located on the outside of the guide shell 12. The first fixed shell 13 and the guide shell 12 make the solution discharged from the through hole 601 be deflected multiple times.
[0054] The working process of this embodiment is similar to that of Embodiment 1, and is described in detail as follows:
[0055] After the solution flows out from the through hole 601, the solution flows downward along the upper surface of the guide shell 12, and then the solution flows to the first fixed shell 13 and continues to flow downward along its surface. The subsequent solution flows in the annular cavity 602 in a water curtain shape, increasing the contact area between the solution and the high-temperature gas in the annular cavity 602, making it easier for the diethyltoluenediamine vapor in the solution to float up quickly and gather at the upper part of the annular cavity 602, further improving the purification efficiency. Example 3
[0056] This embodiment discloses an anti-sticking purification device for LC-grade diethyltoluenediamine, which is further improved on the basis of Example 1.
[0057] like Figure 3-Figure 5 As shown, four second fixing rods 14 equidistantly distributed in the circumferential direction are all fixed to the two fixing frames 9, and the four second fixing rods 14 are located on the inner sides of the four first fixing rods 10; four second rectangular plates 15 equidistantly distributed in the circumferential direction are respectively arranged on adjacent second fixing rods 14, and when the four second rectangular plates 15 are in the working state, the four second rectangular plates 15 rotate clockwise (with the attached Figure 2 Looking downward from the middle direction, the described state is not the state shown in the accompanying drawings), four second rectangular plates 15 are used to drive the solution to flow near the side wall of the distillation tank 1; an annular baffle 16 is fixedly connected to the distillation tank 1, the annular baffle 16 is located below the fixed frame 9, and the inner side of the annular baffle 16 is lower than the outer side thereof, and the annular baffle 16 is used to intercept suspended impurities in the solution in the annular cavity 602; a section of the rotating sleeve 6 facing the first rectangular plate 11 is a diameter-reducing section, and the diameter of the diameter-reducing section of the rotating sleeve 6 gradually decreases from top to bottom.
[0058] The working process of this embodiment is similar to that of Embodiment 1, and is described in detail as follows:
[0059] During the rotation of the fixed frame 9, the fixed frame 9 simultaneously drives the second rectangular plate 15 to rotate clockwise through the second fixed rod 14. At this time, the rotation of the four second rectangular plates 15 will drive the solution in the annular cavity 602 to flow outward. At the same time, affected by the gap between the second rectangular plates 15 and the rotating sleeve 6, the liquid flow reduces the crystalline impurities attached to the rotating sleeve 6, thereby ensuring that the diethyltoluenediamine component in the solution is quickly separated and floated in the form of vapor, thereby accelerating the purification efficiency. Example 4
[0060] This embodiment discloses an anti-sticking purification device for LC-grade diethyltoluenediamine, which is further improved on the basis of Example 3.
[0061] like Figure 1-Figure 6 As shown, four sliding frames 17 equidistantly distributed in the circumferential direction are all slidably arranged on the fixed frame 9, the first fixed rod 10 is rotatably connected to the first rectangular plate 11, the second fixed rod 14 is rotatably connected to the second rectangular plate 15, and in the initial state, the four first rectangular plates 11 are attached Figure 2 In the state shown in FIG. 1 , both ends of the four second rectangular plates 15 are located on a circular trajectory with the central axis of the rotating sleeve 6 as the center. Figure 2 and attached Figure 4In the state, the upper part of the first rectangular plate 11 and the upper part of the second rectangular plate 15 are both provided with horizontal grooves, and the horizontal grooves of the first rectangular plate 11 and the second rectangular plate 15 are both slidably connected with the sliding frame 17, and the sliding frame 17 covers the horizontal grooves; the rotating frame 18 is rotatably arranged on the distillation tank 1, and the rotating frame 18 is provided with four groups of guide grooves, and the four sliding frames 17 are respectively slidably connected with the adjacent guide grooves on the rotating frame 18, and the four groups of guide grooves are separated from each other from top to bottom; the rotating ring 19 is rotatably arranged on the rotating frame 1 8, and is rotatably connected to the distillation tank 1, a vertical groove is provided at the front of the distillation tank 1, and the rotating ring 19 and the rotating frame 18 are both used to cover the vertical groove on the distillation tank 1; a driving member 20 is fixedly connected to the outer side of the distillation tank 1, and the driving member 20 is an electric push rod. When the electric push rod stops working, its telescopic end is in a stationary state, the telescopic end of the driving member 20 is located in the vertical groove of the distillation tank 1, and the telescopic end of the driving member 20 is fixedly connected to the rotating frame 18, and the driving member 20 is used to drive the rotating ring 19 to move up and down.
[0062] The above arrangement can realize the control of the tilt state of the first rectangular plate 11 and the second rectangular plate 15 during the working rotation. When the driving motor 7 drives the rotating sleeve 6 and the fixing frame 9 to rotate, the first rectangular plate 11 and the second rectangular plate 15 are in the adjacent Figure 2 At this time, the rotation of the second rectangular plate 15 will not drive the solution too much, and the first rectangular plate 11 drives the liquid to flow inward under the tilting effect, while reducing the adhesion of impurities on the inner wall of the distillation tank 1, and under the driving effect of the first rectangular plate 11, the impurities in the solution are gathered toward the rotating sleeve 6, and at the same time, due to the guiding effect of the variable diameter section on the rotating sleeve 6, the precipitated crystalline impurities in the solution are gathered toward the lower part of the rotating sleeve 6.
[0063] After working in the above state for a set time, the driving member 20 starts working, and the telescopic end of the driving member 20 drives the rotating ring 19 and the rotating frame 18 to move upward. The rotating frame 18 moves upward so that the guide groove on it squeezes the four sliding frames 17, so that the four sliding frames 17 are close to each other, and the sliding frames 17 move to squeeze the adjacent first rectangular plates 11 and the adjacent second rectangular plates 15 to swing. When the four first rectangular plates 11 swing to the point where their two ends are located on a circular trajectory with the central axis of the rotating sleeve 6 as the center, the four second rectangular plates 15 swing to an inclined state (at this time with the attached Figure 4 For example, the second rectangular plate 15 will swing to the adjacent Figure 4The symmetrical state of the first rectangular plate 11 in the distillation tank 1 is shown in FIG. 1 ), and the driving member 20 stops working. At this time, the second rectangular plate 15 rotates to drive the solution to flow outward. Under this trend, the crystalline impurities in the solution gather to the lower part of the annular baffle 16, reducing the amount of suspended crystalline impurities in the solution. Subsequently, at a set time, the two working states are switched to keep the solution temperature relatively uniform, and also reduce the amount of crystalline impurities attached to the distillation tank 1 and the rotating sleeve 6, thereby ensuring the stability of the purification efficiency.
[0064] The device can also control the first rectangular plate 11 and the second rectangular plate 15 to work in a state of driving the liquid to rotate, as described in the third embodiment. Example 5
[0065] This embodiment discloses an anti-sticking purification device for LC-grade diethyltoluenediamine, which is further improved on the basis of Example 4.
[0066] like Figure 2 and Figure 5 As shown, the first rectangular plate 11 is provided with a plurality of first guide holes 1101 evenly distributed in the vertical direction, and the second rectangular plate 15 is provided with a plurality of second guide holes 1501 evenly distributed in the vertical direction, and the distance between the two first guide holes 1101 (or second guide holes 1501) located on the same horizontal plane on the two centrally symmetrical first rectangular plates 11 (or second rectangular plates 15) gradually decreases from top to bottom.
[0067] The working process of this embodiment is similar to that of Embodiment 4, and is described in detail as follows:
[0068] During the process of the first rectangular plate 11 rotating to drive the solution, the first guide hole 1101 drives the liquid to flow upward, accelerating the floating of the diethyltoluenediamine vapor in the solution. During the process of the second rectangular plate 15 rotating to drive the solution, the second guide hole 1501 drives the liquid to flow downward, so that the impurities accumulated in the solution are gathered to the lower part of the annular baffle 16, so as to facilitate the subsequent rapid discharge of the crystal impurities from the drain pipe 3. Example 6
[0069] The present embodiment discloses an anti-adhesion purification device for LC-grade diethyltoluenediamine, which, based on the embodiment 1, also has the function of pre-separating water vapor.
[0070] like Figure 2 , Figure 7 and Figure 8As shown, it also includes: a second fixed shell 21, fixedly connected to the upper part of the rotating sleeve 6, the diameter of the lower surface of the second fixed shell 21 gradually increases from top to bottom, the injection pipe 2 and the first exhaust pipe 4 are both connected to the inside of the rotating sleeve 6, the discharge pipe 3 and the second exhaust pipe 5 are both connected to the annular cavity 602, the first exhaust pipe 4 is used to discharge water vapor (if the heat of water vapor is directly used, the condenser connected to the first exhaust pipe 4 can be controlled not to work), the second exhaust pipe 5 is used to discharge diethyltoluenediamine vapor, and a plurality of connecting rods 22 are arranged on the outer side of the second fixed shell 21; a fixed sleeve 23, fixedly connected to the outer ends of all the connecting rods 22, the upper surface of the fixed sleeve 23 is in contact with the distillation tank 1, and the lower edge of the fixed sleeve 23 is lower than the lower edge of the through hole 601; a third fixed shell 24 is fixedly connected to the upper side of the second fixed shell 21, and the third fixed shell 24 is located above the connecting rod 22.
[0071] The working process of this embodiment is similar to that of Embodiment 5, and is described in detail as follows:
[0072] As the solution is continuously injected into the rotating sleeve 6, after the solution contacts the second fixed shell 21, the solution flows upward from the middle of the second fixed shell 21. When the liquid level of the solution exceeds the upper surface of the second fixed shell 21, the solution flows along the third fixed shell 24. The solution that leaves the third fixed shell 24 flows downward in a water curtain shape. The subsequent solution fills the gap between the second fixed shell 21 and the rotating sleeve 6. In this process, after the liquid level of the solution exceeds the through hole 601, the above-mentioned operation of the solution flowing in the annular cavity 602 will be repeated.
[0073] At this time, due to the separation effect of the fixed sleeve 23, the internal chamber of the second fixed shell 21 is separated from the annular cavity 602. Since it takes time for the heat generated by the heating element to be transferred inward, the temperature of the solution in the rotating sleeve 6 is slightly lower than the boiling point of diethyltoluenediamine. However, at this time, the internal temperature of the solution in the rotating sleeve 6 is higher than 100°C. At this time, the water in the solution boils and becomes steam, and the water vapor is discharged through the first exhaust pipe 4, while the diethyltoluenediamine vapor in the annular cavity 602 is discharged from the second exhaust pipe 5, reducing the existing processing steps for the steam discharged from the second exhaust pipe 5. At the same time, under the separation effect of the rotating sleeve 6, the newly injected solution can only contact with the solution in the rotating sleeve 6, reducing the large amount of mixing of the new solution with the solution in the annular cavity 602, which affects the purification efficiency of the solution in the annular cavity 602.
[0074] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should be included in the protection scope of the present invention.
Claims
1. Anti-adhesion purification device for LC-grade diethyltoluenediamine, characterized in that: It comprises a distillation tank (1) on which evenly distributed heating elements are arranged, the lower part of the distillation tank (1) is connected to a liquid injection pipe (2) and a liquid discharge pipe (3), the upper part of the distillation tank (1) is connected to a first exhaust pipe (4) and a second exhaust pipe (5), and a flow disturbance unit is arranged inside the distillation tank (1); The spoiler unit comprises a rotating sleeve (6), the rotating sleeve (6) is connected to the distillation tank (1) in a sealed and rotatable manner, the rotating sleeve (6) is provided with a through hole (601), the rotating sleeve (6) and the distillation tank (1) form an annular cavity (602), the distillation tank (1) is provided with a driving motor (7), the output shaft of the driving motor (7) penetrates the distillation tank (1) and is connected to the distillation tank (1) in a sealed and rotatable manner, the output shaft of the driving motor (7) and the rotating sleeve (6) are driven by a gear set, the rotating sleeve (6) is fixedly connected to a fixing frame (9), the fixing frame (9) is fixedly connected to a first fixing rod (10), the first fixing rod (10) is provided with a first rectangular plate (11), and a gap exists between the first rectangular plate (11) and the distillation tank (1); A second fixing rod (14) fixedly connected to the fixing frame (9); a second rectangular plate (15) disposed on the second fixing rod (14), the second rectangular plate (15) being used to stir the solution in the annular cavity (602); a sliding frame (17) slidably disposed on the fixed frame (9), the first fixed rod (10) and the first rectangular plate (11) being rotatably connected, the second fixed rod (14) and the second rectangular plate (15) being rotatably connected, the first rectangular plate (11) and the second rectangular plate (15) being both provided with horizontal grooves, the horizontal grooves of the first rectangular plate (11) and the horizontal grooves of the second rectangular plate (15) being both slidably connected to the sliding frame (17); A rotating frame (18) is rotatably mounted on the distillation tank (1), the rotating frame (18) being provided with a guide groove, and the sliding frame (17) is located in the guide groove of the rotating frame (18) and slides therein; a rotating ring (19) rotatably mounted on the rotating frame (18) and rotatably connected to the distillation tank (1); the distillation tank (1) is provided with a vertical groove; the rotating ring (19) and the rotating frame (18) are both used to cover the vertical groove on the distillation tank (1); A driving member (20) is fixedly connected to the outside of the distillation tank (1) and is used to drive the rotating ring (19) to move.
2. The anti-adhesion purification device for LC-grade diethyltoluenediamine according to claim 1, characterized in that: The first rectangular plate (11) is arranged to be inclined, and the first rectangular plate (11) is used to drive the liquid to flow toward the middle of the distillation tank (1).
3. The anti-adhesion purification device for LC-grade diethyltoluenediamine according to claim 2, characterized in that: Also included are: A guide shell (12) is fixedly connected to the rotating sleeve (6), and the upper surface of the guide shell (12) is connected to the lower edge of the through hole (601); The first fixed shell (13) is fixedly connected to the distillation tank (1), and the first fixed shell (13) is located outside the flow guide shell (12).
4. The anti-adhesion purification device for LC-grade diethyltoluenediamine according to claim 1, characterized in that: An annular baffle (16) is fixedly connected inside the distillation tank (1), the annular baffle (16) is located below the fixing frame (9), and the inner side of the annular baffle (16) is lower than the outer side thereof.
5. The anti-adhesion purification device for LC-grade diethyltoluenediamine according to claim 4, characterized in that: A section of the rotating sleeve (6) facing the first rectangular plate (11) is a diameter-reducing section, and the diameter of the diameter-reducing section of the rotating sleeve (6) gradually decreases from top to bottom.
6. The anti-adhesion purification device for LC-grade diethyltoluenediamine according to claim 1, characterized in that: The first rectangular plate (11) is provided with a plurality of evenly distributed first flow guide holes (1101), and the second rectangular plate (15) is provided with a plurality of evenly distributed second flow guide holes (1501).
7. The anti-adhesion purification device for LC-grade diethyltoluenediamine according to claim 6, characterized in that: Also included are: a second fixed shell (21) fixedly connected to the upper part of the rotating sleeve (6); the liquid injection pipe (2) and the first exhaust pipe (4) are both in communication with the interior of the rotating sleeve (6); the liquid discharge pipe (3) and the second exhaust pipe (5) are both in communication with the annular cavity (602); and a plurality of connecting rods (22) are provided on the outer side surface of the second fixed shell (21); A fixing sleeve (23) is fixedly connected to all the connecting rods (22), the upper surface of the fixing sleeve (23) is in contact with the distillation tank (1), and the lower edge of the fixing sleeve (23) is lower than the lower edge of the through hole (601).
8. The anti-adhesion purification device for LC-grade diethyltoluenediamine according to claim 7, characterized in that: The second fixing shell (21) is fixedly connected to a third fixing shell (24), and the third fixing shell (24) is located above the connecting rod (22).
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