Nitrotoluene rectifying still liquid steam entrainment distillation recovery device and method

Abstract

The invention relates to the technical field of chemical production, in particular to a nitrotoluene rectifying still liquid steam entrainment distillation recovery device and method.The nitrotoluene rectifying still liquid steam entrainment distillation recovery device comprises a distillation separation still, the top of the distillation separation still is connected with a condensation conveying pipe, and the nitrotoluene rectifying still liquid steam entrainment distillation recovery device further comprises a steam conveying pipe arranged at the center of the top of the distillation separation still; a center conveying pipe is slidably arranged on the inner side of the steam conveying pipe in an embedded mode, and the lower end of the center conveying pipe is connected with a floating conveying disc. High-temperature and high-pressure steam is conveyed to the sealed gas storage bin in the floating conveying disc through the steam conveying pipe and the central conveying pipe, and the floating conveying disc can circularly move up and down when conveying the steam so as to realize uniform release of the steam in liquid and stir the liquid to a certain extent, so that uniform distribution of the steam in distillation kettle liquid is ensured, and the quality of the distillation kettle liquid is improved. The phenomenon of local overheating or non-uniform distribution of steam in the traditional entrainment distillation process is avoided, and the entrainment distillation efficiency can be improved.

Description

Technical Field

[0001] The invention relates to the technical field of chemical production, and in particular to a nitrotoluene rectification kettle liquid steam entrainment distillation recovery device and method. Background Art

[0002] As an important chemical intermediate, nitrotoluene is widely used in the pharmaceutical, dye, pesticide and other industries. In the production process of nitrotoluene, distillation kettle liquid containing nitrotoluene, low-boiling impurities and high-boiling impurities is often produced. Toluidine distillation kettle liquid is toluidine-containing liquid discharged after the distillation of toluidine finished tower. These distillation kettle liquids usually contain a certain amount of nitrotoluene. If they are not recycled, it will not only cause waste of resources, but also increase the cost of treating these wastes.

[0003] The traditional treatment method is usually to treat the distillation kettle liquid as waste liquid, for example, it is barreled as tar and entrusted to a qualified manufacturer for treatment. However, this method not only increases the operating costs of the enterprise, but also poses the risk of environmental pollution. Therefore, it is urgent to find an economical and efficient recovery method. By treating the toluidine distillation kettle liquid by direct distillation or steam entrainment distillation to recover the toluidine in the toluidine distillation kettle liquid, the tar content can be effectively reduced and the treatment cost can be reduced.

[0004] However, due to the limitations of the steam transmission pipeline design in the current water vapor entrainment distillation processing equipment, the steam cannot be evenly distributed in the kettle liquid after entering the distillation kettle, which directly affects the contact efficiency between the steam and components such as nitrotoluene. The uneven steam distribution causes the nitrotoluene in certain areas to fail to be effectively entrained, thereby reducing the final recovery efficiency. In addition, in order to compensate for the impact of uneven steam distribution, the steam input needs to be increased, which undoubtedly increases energy consumption. Summary of the invention

[0005] In view of the above, the object of the present invention is to propose a device and method for steam entrainment distillation recovery of nitrotoluene distillation kettle liquid, so as to solve the problem that when the current water vapor entrainment distillation processing equipment is performing steam entrainment distillation recovery of nitrotoluene distillation kettle liquid, due to the limitations of the steam transmission pipeline design, the steam cannot be evenly distributed in the kettle liquid after entering the distillation kettle, which affects the contact efficiency between the steam and nitrotoluene and other components, thereby reducing the final recovery efficiency.

[0006] Based on the above purpose, the present invention provides a nitrotoluene rectification kettle liquid steam entrainment distillation recovery device, comprising a distillation separation kettle, the top of which is connected to a condensation delivery pipe, and further comprising:

[0007] A steam delivery pipe is arranged at the top center of the distillation separation kettle, a central delivery pipe is slidably arranged inside the steam delivery pipe, a floating delivery plate is connected to the lower end of the central delivery pipe, and the floating delivery plate is slidably connected to the steam delivery pipe through the central delivery pipe;

[0008] A sealed gas storage bin is arranged inside the floating conveying plate, a plurality of conveying openings are evenly arranged on the surface of the floating conveying plate, and the central conveying pipe is interconnected with all the conveying openings through the sealed gas storage bin;

[0009] A central linkage rod is connected and arranged at the bottom center of the floating conveying plate, a closed sliding sleeve is arranged at the bottom center of the distillation separation kettle, the central linkage rod is slidably connected to the distillation separation kettle through the closed sliding sleeve, and a switch trigger frame is fixedly connected and arranged at the bottom end of the central linkage rod;

[0010] A limit adjustment frame is symmetrically and vertically connected on the left and right sides at the bottom of the distillation separation kettle. An adjustment slide is arranged in the middle of the limit adjustment frame. A limit blocking frame is slidingly connected in the middle of the adjustment slide. A travel switch is installed on the adjacent side of the limit blocking frames arranged on the left and right sides. The travel switch and the switch trigger frame are arranged corresponding to each other. An electromagnetic switch valve is arranged on the top of the steam delivery pipe, and the travel switch and the electromagnetic switch valve are electrically connected.

[0011] Furthermore, the limit blocking frame is slidably connected to the limit adjustment frame through an adjusting slot, an adjusting screw is arranged in the middle of the adjusting slot, an adjusting motor is arranged at the axial end of the adjusting screw, an adjusting screw sleeve is arranged in the middle of the limit blocking frame, and the limit blocking frame is interconnected with the adjusting screw through the adjusting screw sleeve.

[0012] Furthermore, an annular stirring frame is arranged around the interior of the distillation separation kettle, a stirring connecting ring is arranged around the outer side of the annular stirring frame, the annular stirring frame is rotatably connected to the distillation separation kettle through the stirring connecting ring, spiral blades are symmetrically connected on the left and right sides of the annular stirring frame, and a plurality of stirring blades are evenly connected and arranged around the bottom of the annular stirring frame.

[0013] Furthermore, a guide sleeve is provided in the middle connection of the floating conveying plate, a vertical guide rod is fixedly provided inside the distillation separation kettle, the floating conveying plate is slidably connected to the vertical guide rod via the guide sleeve, a spiral drive groove is provided around the outer wall of the floating conveying plate, the spiral drive groove and the spiral blades are slidably connected with each other, and when the floating conveying plate moves up and down along the vertical guide rod, the annular stirring frame is driven to rotate synchronously through the spiral drive groove and the spiral blades.

[0014] Furthermore, a condensation separation cylinder is arranged above the distillation separation kettle, the condensation delivery pipe is located at the inner center of the condensation separation cylinder, an air collecting hood is arranged on the inner top of the distillation separation kettle, the bottom end of the condensation delivery pipe is connected to the air collecting hood, a plurality of inclined delivery pipes are evenly connected and arranged on the top of the condensation delivery pipe, a plurality of condensation delivery ports are evenly arranged in the middle of the inclined delivery pipe, a conical liquid guide plate is arranged around the bottom of the condensation separation cylinder, an annular liquid collecting trough is arranged around the bottom of the conical liquid guide plate, and a condensation output pipe is connected and arranged at the bottom of the annular liquid collecting trough.

[0015] Furthermore, a centrifugal separation cylinder is arranged around the inner side of the condensation separation cylinder, a conical guide wall is arranged around the inner side of the centrifugal separation cylinder, a plurality of inclined condensing fins are evenly connected and arranged in a circular shape on the inner side of the conical guide wall, the inclined condensing fins are located below the inclined conveying pipe, and a plurality of cooling pipes are evenly arranged in the middle of the inclined condensing fins.

[0016] Furthermore, a rotating connecting ring is arranged around the top of the centrifugal separation cylinder, and the centrifugal separation cylinder is rotatably connected to the condensation separation cylinder through the rotating connecting ring. A rotating gear ring is arranged around the outer side of the rotating connecting ring, and a rotating gear is meshingly connected to the outer side of the rotating gear ring. A rotating motor is connected to the shaft end of the rotating gear, and the rotating motor drives the centrifugal separation cylinder to rotate through the rotating gear and the rotating gear ring, and then drives all the inclined condensation fins to rotate synchronously through the centrifugal separation cylinder.

[0017] Furthermore, the top and bottom ends of the cooling pipe are connected with rotary joints, and the top and bottom ends of the cooling pipe are respectively connected with a circulation input pipe and a circulation output pipe through rotary joints. The cooling pipe is rotatably connected to the circulation input pipe or the circulation output pipe through the rotary joint, the outer ends of the circulation input pipe and the circulation output pipe are connected with finned radiators, and the middle of the circulation input pipe is connected with a circulation delivery pump.

[0018] Furthermore, a stratified separation cylinder is connected to the outer end of the condensation output pipe, a separation delivery pipe is vertically arranged at the center of the stratified separation cylinder, the condensation output pipe and the top of the separation delivery pipe are connected to each other, a delivery opening is arranged at the bottom end of the separation delivery pipe, a centrifugal turbine disk is arranged below the delivery opening, a centrifugal motor is connected to the axial end of the centrifugal turbine disk, a spacing separation cylinder is arranged around the inner upper side of the stratified separation cylinder, a heavy phase separation layer is arranged between the outer wall of the spacing separation cylinder and the inner wall of the stratified separation cylinder, a light phase separation layer is arranged between the inner wall of the spacing separation cylinder and the outer wall of the separation delivery pipe, and the tops of the heavy phase separation layer and the light phase separation layer are both connected to separation output pipes.

[0019] A method for using a nitrotoluene rectification kettle liquid steam entrainment distillation recovery device comprises the following steps:

[0020] S1: charging stage, adding the nitrotoluene rectification kettle liquid to be treated into the distillation separation kettle;

[0021] S2: Start steam delivery, open the electromagnetic switch valve at the top of the steam delivery pipe, so that high-temperature and high-pressure steam enters the central delivery pipe through the steam delivery pipe, and is transmitted to the sealed gas storage bin inside the floating delivery tray through the central delivery pipe;

[0022] S3: Steam is evenly distributed. The steam in the sealed gas storage bin is evenly distributed to the kettle liquid in the distillation separation kettle through multiple delivery openings. The steam forms an azeotropic mixture with substances such as nitrotoluene, which causes nitrotoluene to enter the gas phase. The recovered nitrotoluene is transported to the externally connected condensation equipment through the condensation delivery pipe connected to the top of the distillation separation kettle for condensation recovery.

[0023] S4: The floating conveyor plate moves. As the steam enters the sealed gas storage bin, the liquid in it is squeezed out. The floating conveyor plate rises due to the decrease in overall density, and the central linkage rod drives the switch trigger frame to move accordingly;

[0024] S5: Trigger the travel switch on the limit adjustment frame. When the floating conveying plate rises to a certain height, the switch trigger frame triggers the travel switch on the limit blocking frame to control the electromagnetic switch valve to close and stop steam delivery;

[0025] S6: Steam delivery is suspended. After losing steam pressure, the liquid flows back into the sealed gas storage bin, and the floating delivery plate sinks due to the increase in overall density;

[0026] S7: Trigger the travel switch on the limit adjustment frame again. When the floating conveying plate sinks to a certain position, the switch trigger frame triggers the travel switch on the limit blocking frame again to control the electromagnetic switch valve to open and continue to convey steam;

[0027] S8: The above steps are repeated repeatedly until the recovery of nitrotoluene is completed.

[0028] Beneficial effects of the present invention: As can be seen from the above description, a nitrotoluene rectification kettle liquid steam entrainment distillation recovery device provided by the present invention delivers high-temperature and high-pressure steam to the sealed gas storage bin inside the floating conveying plate through the steam conveying pipe and the central conveying pipe. When the floating conveying plate conveys steam inside, the liquid in the sealed gas storage bin is pressed out, so that the overall density of the floating conveying plate is reduced, and the floating conveying plate sunk at the bottom of the distillation separation kettle will gradually float upward. When the floating conveying plate floats upward for a certain distance, it will be linked to trigger the travel switch to control the closing of the electromagnetic switch valve. After losing the pressure of the steam, the liquid will naturally flow and be transported to the sealed gas storage bin inside the floating conveying plate, and its overall density will increase, and it will gradually move downward until it triggers another travel switch to reopen the electromagnetic switch valve, so that the floating conveying plate will cyclically move up and down when conveying steam to achieve uniform release of steam in the liquid, and turn over and stir the liquid to a certain extent, ensuring uniform distribution of steam in the distillation kettle liquid, avoiding the phenomenon of local overheating or uneven distribution of steam in the traditional entrainment distillation process, significantly improving the effective contact area between steam and target components such as nitrotoluene, and enhancing the entrainment effect. BRIEF DESCRIPTION OF THE DRAWINGS

[0029] In order to more clearly illustrate the technical solutions in the present invention or the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings in the following description are only for the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0030] Figure 1 It is a schematic structural diagram of a distillation separation kettle according to an embodiment of the present invention;

[0031] Figure 2 It is a schematic structural diagram of a condensation separation cylinder according to an embodiment of the present invention;

[0032] Figure 3 It is a schematic structural diagram of the front side of an embodiment of the present invention;

[0033] Figure 4 It is a structural schematic diagram of the back side of an embodiment of the present invention;

[0034] Figure 5 This is a schematic structural diagram of a central delivery pipe according to an embodiment of the present invention;

[0035] Figure 6 A schematic diagram of the internal structure of a distillation separation kettle according to an embodiment of the present invention;

[0036] Figure 7 It is a structural schematic diagram of a floating conveyor plate according to an embodiment of the present invention;

[0037] Figure 8A schematic diagram of the internal structure of a condensation separation cylinder according to an embodiment of the present invention;

[0038] Fig. 9 A schematic structural diagram of a centrifugal separation cylinder according to an embodiment of the present invention;

[0039] Fig.10 It is a schematic structural diagram of a layered separation cylinder according to an embodiment of the present invention.

[0040] The markings in the figure are:

[0041] 1. Distillation separation kettle; 101. Vertical guide rod; 102. Closed sleeve; 103. Gas collecting hood; 104. Feeding pipe; 105. Discharging pipe; 106. Steam delivery pipe; 107. Solenoid switch valve; 108. Central delivery pipe; 2. Limit adjustment frame; 201. Adjustment slide; 202. Adjustment screw; 203. Adjustment motor; 204. Limit blocking frame; 205. Travel switch; 206. Adjustment screw sleeve; 3. Floating conveying plate; 301. Guide sleeve; 302. Sealed gas storage bin; 303. One-way delivery valve; 304. Delivery opening; 305. Spiral drive groove; 306. Central linkage rod; 307. Switch trigger frame; 4. Annular stirring frame; 401. Stirring connecting ring; 402. Spiral blade; 403. Stirring blade; 5. Condensation separation cylinder; 50 1. Condensation delivery pipe; 502. Inclined delivery pipe; 503. Condensation delivery port; 504. Conical liquid guide plate; 505. Annular liquid collecting tank; 506. Condensation output pipe; 6. Centrifugal separation cylinder; 601. Conical guide wall; 602. Inclined condensation fins; 603. Rotating connecting ring; 604. Rotating gear ring; 605. Rotating gear; 606. Rotating motor; 7. Cooling pipeline; 701. Rotating joint; 702. Circulation input pipe; 703. Circulation output pipe; 704. Circulation delivery pump; 705. Finned radiator; 8. Layered separation cylinder; 801. Separation delivery pipe; 802. Delivery opening; 803. Centrifugal turbine disc; 804. Centrifugal motor; 805. Interval separation cylinder; 806. Heavy phase separation layer; 807. Light phase separation layer; 808. Separation output pipe. DETAILED DESCRIPTION

[0042] In order to make the objectives, technical solutions and advantages of the present invention more clearly understood, the present invention is further described in detail below in conjunction with specific embodiments.

[0043] It should be noted that, unless otherwise defined, the technical terms or scientific terms used in the present invention should be understood by people with ordinary skills in the field to which the present invention belongs. The "first", "second" and similar words used in the present invention do not indicate any order, quantity or importance, but are only used to distinguish different components. "Include" or "comprise" and similar words mean that the elements or objects appearing before the word include the elements or objects listed after the word and their equivalents, without excluding other elements or objects. "Connect" or "connected" and similar words are not limited to physical or mechanical connections, but may include electrical connections, whether direct or indirect. "Up", "down", "left", "right" and the like are only used to indicate relative positional relationships. When the absolute position of the described object changes, the relative positional relationship may also change accordingly.

[0044] like Figure 1 , Figure 2 , Figure 3 , Figure 4 , Figure 5 , Figure 6 , Figure 7 , Figure 8 , Fig. 9 , Fig.10 As shown, a nitrotoluene rectification kettle liquid steam entrainment distillation recovery device includes a distillation separation kettle 1, the top of the distillation separation kettle 1 is connected to a condensation delivery pipe 501, and also includes:

[0045] The steam delivery pipe 106 is arranged at the top center of the distillation separation kettle 1, and a central delivery pipe 108 is slidably arranged inside the steam delivery pipe 106, and a floating delivery plate 3 is connected to the lower end of the central delivery pipe 108, and the floating delivery plate 3 is slidably connected to the steam delivery pipe 106 through the central delivery pipe 108;

[0046] The sealed gas storage bin 302 is arranged inside the floating conveying plate 3. A plurality of conveying openings 304 are evenly arranged on the surface of the floating conveying plate 3. The central conveying pipe 108 is interconnected with all the conveying openings 304 through the sealed gas storage bin 302.

[0047] A central linkage rod 306 is connected and arranged at the bottom center of the floating conveying plate 3. A closed sliding sleeve 102 is arranged at the bottom center of the distillation separation kettle 1. The central linkage rod 306 is slidably connected to the distillation separation kettle 1 through the closed sliding sleeve 102. A switch trigger frame 307 is fixedly connected to the bottom end of the central linkage rod 306.

[0048] The limit adjustment frame 2 is symmetrically and vertically connected on the left and right sides at the bottom of the distillation separation kettle 1. An adjustment slide 201 is arranged in the middle of the limit adjustment frame 2. The middle sliding connection of the adjustment slide 201 is provided with a limit blocking frame 204. The adjacent side of the limit blocking frame 204 arranged on the left and right sides is installed with a travel switch 205. The travel switch 205 and the switch trigger frame 307 are arranged corresponding to each other. The top of the steam delivery pipe 106 is provided with an electromagnetic switch valve 107, and the travel switch 205 and the electromagnetic switch valve 107 are electrically connected.

[0049] In this embodiment, the device can transport high-temperature and high-pressure steam to the sealed gas storage bin 302 inside the floating transport plate 3 through the steam transport pipe 106 and the central transport pipe 108. The steam is evenly distributed and transported to the inside of the distillation separation kettle 1 through the transport opening 304, and the water vapor and the nitrotoluene in the liquid in the toluidine rectification kettle liquid contained in the distillation separation kettle 1 form an azeotropic mixture, so that the toluidine that is originally not volatile is carried into the gas phase by the water vapor, and floats upward and flows to gather at the top of the distillation separation kettle 1, and then is transported to the externally connected condensation device through the condensation transport pipe 501 connected to the top of the distillation separation kettle 1 The floating conveyor plate 3 is equipped with a central linkage rod 306, which drives the switch trigger frame 307 to move synchronously. When the floating conveyor plate 3 floats a certain distance upward, the central linkage rod 306 drives the switch trigger frame 307 to touch the upper position of the limit adjustment frame 2. The limit switch 205 on the limit blocking frame 204 is electrically connected to the electromagnetic switch valve 107 installed on the top of the steam delivery pipe 106, so that the electromagnetic switch valve 107 is closed by the limit switch 205 to stop the steam delivery. After losing the steam pressure, the liquid naturally flows to the sealed gas storage bin 302 inside the floating delivery tray 3, and its overall density increases, and it gradually moves downward until the central linkage rod 306 drives the switch trigger frame 307 to touch the limit switch 205 on the limit blocking frame 204 located at the lower position in the limit adjustment frame 2. At this time, it passes The travel switch 205 controls the opening of the electromagnetic switch valve 107, and the steam continues to be transported, pressing out the liquid, and the floating conveying plate 3 moves upward, so that the floating conveying plate 3 can be cyclically moved up and down to achieve uniform release of steam in the liquid, and to stir the liquid to a certain extent, so that the steam and liquid can be in uniform and sufficient contact, thereby improving the efficiency of entrainment distillation. At the same time, a one-way conveying valve 303 is provided at the connection between the central conveying pipe 108 and the floating conveying plate 3. The one-way conveying valve 303 allows the steam to be transported to the floating conveying plate 3 only through the central conveying pipe 108 to avoid reverse reflux of gas and liquid.

[0050] like Figure 1 , Figure 2 , Figure 3 , Figure 4 , Figure 5 , Figure 6 , Figure 7 , Figure 8 , Fig. 9 and Fig.10As shown, preferably, when the floating conveying plate 3 of the device moves up and down, the switch trigger frame 307 is driven to move synchronously through the central linkage rod 306, and then the travel switch 205 on the limit blocking frame 204 located at the upper and lower positions of the limit adjustment frame 2 is triggered by the switch trigger frame 307, and the limit blocking frame 204 is slidably connected with the limit adjustment frame 2 through the adjusting slide 201, and the middle connection of the adjusting slide 201 is provided with an adjusting screw 202, and the axial end of the adjusting screw 202 is connected with an adjusting motor 203, and the middle of the limit blocking frame 204 is provided with an adjusting screw sleeve 206, and the limit blocking frame 204 is connected to the adjusting screw 202 through the adjusting screw sleeve 206, so that the adjusting motor 203 can drive the corresponding limit blocking frame 204 to move up and down along the adjusting slide 201 through the adjusting screw 202 and the adjusting screw sleeve 206, and then adjust the position of the corresponding limit blocking frame 204, so that the trigger position and the circulation distance can be adjusted according to needs, such as the internal liquid level height of the distillation separation kettle 1, which is more flexible and convenient to use.

[0051] like Figure 1 , Figure 2 , Figure 3 , Figure 4 , Figure 5 , Figure 6 , Figure 7 , Figure 8 , Fig. 9 and Fig.10As shown, preferably, an annular stirring frame 4 is arranged around the inside of the distillation separation kettle 1 of the device, a stirring connection ring 401 is arranged around the outside of the annular stirring frame 4, the annular stirring frame 4 is rotatably connected to the distillation separation kettle 1 through the stirring connection ring 401, the left and right sides of the annular stirring frame 4 are symmetrically connected with spiral blades 402, a plurality of stirring blades 403 are evenly connected and arranged around the bottom of the annular stirring frame 4, and a guide sleeve 301 is arranged in the middle of the floating conveying plate 3, a vertical guide rod 101 is fixedly connected inside the distillation separation kettle 1, the floating conveying plate 3 is slidably connected to the vertical guide rod 101 through the guide sleeve 301, a spiral driving groove 305 is arranged around the outer wall of the floating conveying plate 3, the spiral driving groove 305 and the spiral blade 402 are mutually engaged and slidably connected, and the floating conveying plate 3 is arranged along the vertical guide When the rod 101 moves up and down, the floating conveying plate 3 can drive the annular stirring frame 4 to rotate synchronously through the spiral driving groove 305 and the spiral blade 402 when it moves up and down in a cycle, and then the annular stirring frame 4 can drive the spiral blade 402 and the stirring blade 403 to rotate synchronously to stir the toluidine distillation kettle liquid inside the distillation separation kettle 1, ensuring the uniform distribution of steam in the distillation kettle liquid, avoiding the phenomenon of local overheating or uneven distribution of steam during entrainment distillation, and at the same time, the floating conveying plate 3 is linked to drive the annular stirring frame 4 to rotate for stirring, so as to achieve the mutual coordination of steam conveying and stirring. When the steam conveying amount is high, the floating conveying plate 3 floats up quickly, and then the speed of driving the annular stirring frame 4 to rotate for stirring is also increased, which further improves the recovery efficiency of nitrotoluene and promotes the full contact between steam and liquid.

[0052] like Figure 1 , Figure 2 , Figure 3 , Figure 4 , Figure 5 , Figure 6 , Figure 7 , Figure 8 , Fig. 9 and Fig.10As shown, preferably, a condensation separation cylinder 5 is arranged above the distillation separation kettle 1 of the device, a condensation delivery pipe 501 is located at the inner center of the condensation separation cylinder 5, a gas collecting hood 103 is arranged on the inner top of the distillation separation kettle 1, the bottom end of the condensation delivery pipe 501 is connected to the gas collecting hood 103, a plurality of inclined delivery pipes 502 are evenly arranged and connected to the top of the condensation delivery pipe 501, a plurality of condensation delivery ports 503 are evenly arranged in the middle of the inclined delivery pipe 502, a conical liquid guide plate 504 is arranged around the bottom of the condensation separation cylinder 5, and a conical liquid guide plate 504 is arranged around the bottom of the conical liquid guide plate 504 An annular liquid collecting tank 505 is provided, and a condensation output pipe 506 is connected to the bottom of the annular liquid collecting tank 505, so that water vapor and nitrotoluene in the liquid form an azeotropic mixture, so that the toluidine that is originally not volatile is carried into the gas phase by the water vapor, and when it floats upward and flows and gathers on the top of the distillation separation kettle 1, it is gathered and transported to the condensation delivery pipe 501 through the gas collecting hood 103, and further transported to multiple inclined delivery pipes 502, and then uniformly transported to the inside of the condensation separation cylinder 5 through the condensation delivery port 503, and the inner side of the condensation separation cylinder 5 is surrounded by a centrifugal separation cylinder 6, and the centrifugal separation cylinder 6 is surrounded by a conical guide wall 601, and the inner side of the conical guide wall 601 is evenly connected and connected with a plurality of inclined condensing fins 602 in a circular shape. The inclined condensing fins 602 are located below the inclined conveying pipe 502, so after the mixed gas is conveyed to the inside of the condensation separation cylinder 5, it contacts with the plurality of inclined condensing fins 602, and a plurality of cooling pipes 7 are evenly arranged in the middle of the inclined condensing fins 602. The top and bottom ends of the cooling pipes 7 are connected with rotary joints 701, and the top and bottom ends of the cooling pipes 7 are respectively connected with rotary joints 701. The circulation input pipe 702 and the circulation output pipe 703, the cooling pipeline 7 is rotatably connected to the circulation input pipe 702 or the circulation output pipe 703 through a rotary joint 701, the outer ends of the circulation input pipe 702 and the circulation output pipe 703 are connected with a finned radiator 705, and the middle connection of the circulation input pipe 702 is provided with a circulation delivery pump 704, so that the circulation delivery pump 704 can circulate the cooling medium through the circulation input pipe 702, the circulation output pipe 703 and the cooling pipeline 7, and then the mixed gas is condensed into liquid through the inclined condensation fins 602 to recover toluidine.

[0053] like Figure 1 , Figure 2 , Figure 3 , Figure 4 , Figure 5 , Figure 6 , Figure 7 , Figure 8 , Fig. 9 and Fig.10As shown, preferably, a rotating connection ring 603 is arranged around the top of the centrifugal separation cylinder 6 of the device, and the centrifugal separation cylinder 6 is rotatably connected to the condensation separation cylinder 5 through the rotating connection ring 603. A rotating gear ring 604 is arranged around the outer side of the rotating connection ring 603, and a rotating gear 605 is arranged on the outer side of the rotating gear ring 604 in meshing connection. A rotating motor 606 is connected to the shaft end of the rotating gear 605, so that the centrifugal separation cylinder 6 and the multiple inclined condensation fins 602 connected thereto not only constitute a cooling structure, but also constitute a turbine structure. When the rotating motor 606 drives the centrifugal separation cylinder 6 to rotate through the rotating gear 605 and the rotating gear ring 604, and then drives all the inclined condensation fins 602 to rotate synchronously through the centrifugal separation cylinder 6, a certain suction structure is formed. The gas can be pumped and gathered through the gas collecting hood 103 to the condensation delivery pipe 501, and further delivered to multiple inclined delivery pipes 502, and then evenly delivered to the inside of the condensation separation cylinder 5 through the condensation delivery port 503. The gas is directly in contact with the turbine structure composed of the centrifugal separation cylinder 6 and the multiple inclined condensation fins 602 connected thereto, so that the gas can be cooled while being pumped, thereby avoiding the problem of condensation of the gas in the pump and reduced recovery rate when an additional gas delivery pump is used. When the gas condenses on the surface of the inclined condensation fins 602, it is naturally thrown outward to the conical guide wall 601 by the rotating centrifugal force, and is transported along the conical guide wall 601 to converge to the annular liquid collecting tank 505, and then discharged from the condensation output pipe 506.

[0054] like Figure 1 , Figure 2 , Figure 3 , Figure 4 , Figure 5 , Figure 6 , Figure 7 , Figure 8 , Fig. 9 and Fig.10As shown, preferably, the outer end of the condensation output pipe 506 of the device is connected to a stratified separation cylinder 8, a separation delivery pipe 801 is vertically arranged at the center of the stratified separation cylinder 8, the condensation output pipe 506 and the top of the separation delivery pipe 801 are connected to each other, and a delivery opening 802 is arranged at the bottom end of the separation delivery pipe 801, so that the condensed mixed liquid is output from the delivery opening 802, and a centrifugal turbine disk 803 is arranged below the delivery opening 802, and a centrifugal motor 804 is connected to the axial end of the centrifugal turbine disk 803, and the centrifugal motor 804 drives the centrifugal turbine disk 803 to rotate at a high speed to centrifuge the mixed liquid delivered to the stratified separation cylinder 8, and a spacing separation cylinder 805 is arranged around the upper side of the interior of the stratified separation cylinder 8, and the spacing separation cylinder 805 has a A heavy phase separation layer 806 is arranged between the outer wall and the inner wall of the stratified separation cylinder 8, a light phase separation layer 807 is arranged between the inner wall of the spacing separation cylinder 805 and the outer wall of the separation conveying pipe 801, and the tops of the heavy phase separation layer 806 and the light phase separation layer 807 are connected to the separation output pipe 808. Through centrifugation, the liquid with higher density gathers in the heavy phase separation layer 806 on the outside, i.e., between the outer wall of the spacing separation cylinder 805 and the inner wall of the stratified separation cylinder 8, while the liquid with lower density gathers in the light phase separation layer 807 between the inner wall of the spacing separation cylinder 805 and the outer wall of the separation conveying pipe 801, and then the two liquids are respectively output through the separation output pipe 808, thereby realizing the continuous separation of the mixed liquid after the entrainment distillation and condensation of the nitrotoluene distillation kettle liquid vapor.

[0055] When in use, the corresponding pipelines of the device are connected, and then aniline distillation kettle liquid is added through the feeding pipe 104 connected to the top of the side wall of the distillation separation kettle 1, and then high-temperature and high-pressure steam is transported to the sealed gas storage bin 302 inside the floating conveying plate 3 through the steam conveying pipe 106 and the central conveying pipe 108. The steam is evenly distributed and transported to the inside of the distillation separation kettle 1 through the conveying opening 304, and the water vapor and the nitrotoluene in the liquid form an azeotropic mixture in the toluidine distillation kettle liquid contained in the distillation separation kettle 1, so that the toluidine that is originally not easy to volatilize is carried into the gas phase by the water vapor, and floats upward and converges on the top of the distillation separation kettle 1, and then converges and transports to the condensation conveying pipe 501 through the gas collecting hood 103, and is further transported to multiple inclined conveying pipes 502. Then it is evenly transported to the inside of the condensation separation cylinder 5 through the condensation delivery port 503. After the mixed gas is transported to the inside of the condensation separation cylinder 5, it contacts with multiple inclined condensation fins 602 and condenses into liquid. The rotating motor 606 drives the centrifugal separation cylinder 6 to rotate through the rotating gear 605 and the rotating gear ring 604, and then drives all the inclined condensation fins 602 to rotate synchronously through the centrifugal separation cylinder 6. The gas is cooled while being pumped. When the gas condenses on the surface of the inclined condensation fins 602, it is naturally thrown outward to the conical guide wall 601 by the centrifugal force of rotation, and is transported along the conical guide wall 601 to converge to the annular liquid collecting tank 505, and then transported to the separation delivery pipe 801 by the condensation output pipe 506. The condensed mixed liquid is then transported to the separation delivery pipe 801 by the delivery opening The centrifugal motor 804 drives the centrifugal turbine disc 803 to rotate at a high speed to centrifuge the mixed liquid transported to the stratified separation cylinder 8. Through centrifugation, the liquid with higher density gathers in the heavy phase separation layer 806 between the outer wall of the spacing separation cylinder 805 and the inner wall of the stratified separation cylinder 8, while the liquid with lower density gathers in the light phase separation layer 807 between the inner wall of the spacing separation cylinder 805 and the outer wall of the central delivery pipe 108. Then the two liquids are respectively output through the separation output pipe 808, so as to realize the continuous separation of the mixed liquid after the distillation and condensation of the nitrotoluene distillation kettle liquid steam entrainment. When the floating delivery disc 3 transports steam inside, the liquid in the sealed gas storage bin 302 is pressed out by the steam, and a part of the steam is transported, thereby The liquid in the sealed gas storage bin 302 will gradually decrease, and the overall density will decrease, so that the floating conveying plate 3 sunk at the bottom of the distillation separation kettle 1 will gradually float upward and release steam at the same time. When the floating conveying plate 3 moves, it will drive the switch trigger frame 307 to move synchronously through the central linkage rod 306. When the floating conveying plate 3 floats upward for a certain distance, the central linkage rod 306 drives the switch trigger frame 307 to touch the travel switch 205 on the upper limit blocking frame 204 in the limit adjustment frame 2. At this time, the electromagnetic switch valve 107 is controlled to be closed through the travel switch 205 to stop conveying steam. After losing the steam pressure, the liquid will naturally flow and be transported to the sealed gas storage bin 302 inside the floating conveying plate 3. Its overall density increases, and it gradually moves downward.Until the central linkage rod 306 drives the switch trigger frame 307 to touch the travel switch 205 on the lower limit blocking frame 204 in the limit adjustment frame 2, at this time, the travel switch 205 controls the opening of the electromagnetic switch valve 107, and the steam continues to be transported to press the liquid out, and the floating conveying plate 3 moves upward, so that the floating conveying plate 3 can be cyclically moved up and down to achieve uniform release of steam in the liquid. At the same time, when the floating conveying plate 3 moves up and down in a cycle, the spiral driving groove 305 and the spiral blade 402 drive the annular stirring frame 4 to rotate synchronously, and then the annular stirring frame 4 drives the spiral blade 402 and the stirring blade 403 to rotate synchronously to stir the toluidine rectification kettle liquid inside the distillation separation kettle 1, so that the steam and the liquid are evenly and fully contacted, and the efficiency of entrained distillation is improved.

[0056] A method for using a nitrotoluene rectification kettle liquid steam entrainment distillation recovery device comprises the following steps:

[0057] S1: feeding stage, adding the nitrotoluene rectification kettle liquid to be treated into the distillation separation kettle 1;

[0058] S2: Start steam delivery, open the electromagnetic switch valve 107 at the top of the steam delivery pipe 106, so that the high-temperature and high-pressure steam enters the central delivery pipe 108 through the steam delivery pipe 106, and is transmitted to the sealed gas storage bin 302 inside the floating delivery tray 3 through the central delivery pipe 108;

[0059] S3: The steam is evenly distributed. The steam in the sealed gas storage bin 302 is evenly distributed to the kettle liquid in the distillation separation kettle 1 through multiple delivery openings 304. The steam forms an azeotropic mixture with substances such as nitrotoluene, which causes nitrotoluene to enter the gas phase. The recovered nitrotoluene is transported to an externally connected condensation device through a condensation delivery pipe 501 connected to the top of the distillation separation kettle 1 for condensation recovery;

[0060] S4: The floating conveying plate 3 moves. As the steam enters the sealed gas storage bin 302, the liquid therein is squeezed out. The floating conveying plate 3 rises due to the decrease in overall density, and the central linkage rod 306 drives the switch trigger frame 307 to move accordingly.

[0061] S5: Trigger the travel switch 205 on the limit adjustment frame 2. When the floating conveying plate 3 rises to a certain height, the switch trigger frame 307 triggers the travel switch 205 on the limit blocking frame 204, controls the electromagnetic switch valve 107 to close, and stops steam delivery;

[0062] S6: Steam delivery is suspended. After losing steam pressure, the liquid flows back into the sealed gas storage bin 302, and the floating delivery plate 3 sinks due to the increase of overall density;

[0063] S7: Trigger the travel switch 205 on the limit adjustment frame 2 again. When the floating conveying plate 3 sinks to a certain position, the switch trigger frame 307 triggers the travel switch 205 on the limit blocking frame 204 again, controls the electromagnetic switch valve 107 to open, and continues to convey steam;

[0064] S8: The above steps are repeated repeatedly until the recovery of nitrotoluene is completed.

[0065] The nitrotoluene rectification kettle liquid steam entrainment distillation recovery device provided by the present invention delivers high-temperature and high-pressure steam to the sealed gas storage bin 302 inside the floating conveying plate 3 through the steam delivery pipe 106 and the central delivery pipe 108. When the steam is delivered inside the floating conveying plate 3, the liquid in the sealed gas storage bin 302 is pressed out, so that the overall density of the floating conveying plate 3 is reduced, and the floating conveying plate 3 sunk at the bottom of the distillation separation kettle 1 will gradually float upward. When the floating conveying plate 3 floats upward for a certain distance, it will link and trigger the travel switch 205 to control the closing of the electromagnetic switch valve 107. After losing the steam pressure, the liquid will be discharged by itself. The steam flows to the sealed gas storage bin 302 inside the floating conveying plate 3, where its overall density increases and it gradually moves downward until another travel switch 205 is triggered to reopen the electromagnetic switch valve 107. As a result, the floating conveying plate 3 moves up and down cyclically when conveying steam, so as to achieve uniform release of steam in the liquid and stir the liquid to a certain extent, thereby ensuring uniform distribution of steam in the distillation kettle liquid, avoiding local overheating or uneven distribution of steam in traditional entrainment distillation, significantly improving the effective contact area between steam and target components such as nitrotoluene, and enhancing the entrainment effect.

[0066] Those skilled in the art should understand that the discussion of any of the above embodiments is only exemplary and is not intended to imply that the scope of the present invention is limited to these examples; under the concept of the present invention, the technical features in the above embodiments or different embodiments can also be combined, the steps can be implemented in any order, and there are many other changes in different aspects of the present invention as described above, which are not provided in detail for the sake of simplicity. Any omissions, modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the scope of protection of the present invention.

Claims

1. A nitrotoluene rectification kettle liquid steam entrainment distillation recovery device, comprising a distillation separation kettle (1), wherein the top of the distillation separation kettle (1) is connected to a condensation delivery pipe (501), characterized in that: Also includes: A steam delivery pipe (106) is arranged at the top center of the distillation separation kettle (1), a central delivery pipe (108) is slidably arranged inside the steam delivery pipe (106), a floating delivery plate (3) is connected to the lower end of the central delivery pipe (108), and the floating delivery plate (3) is slidably connected to the steam delivery pipe (106) through the central delivery pipe (108); A sealed gas storage bin (302) is arranged inside the floating conveying plate (3), a plurality of conveying openings (304) are evenly arranged on the surface of the floating conveying plate (3), and the central conveying pipe (108) is interconnected with all the conveying openings (304) through the sealed gas storage bin (302); A central linkage rod (306) is connected and arranged at the bottom center of the floating conveying plate (3); a closed sliding sleeve (102) is arranged at the bottom center of the distillation separation kettle (1); the central linkage rod (306) is slidably connected to the distillation separation kettle (1) through the closed sliding sleeve (102); and a switch trigger frame (307) is fixedly connected to the bottom end of the central linkage rod (306); A limit adjustment frame (2) is symmetrically and vertically connected on the left and right sides at the bottom of the distillation separation kettle (1); an adjustment slide groove (201) is arranged in the middle of the limit adjustment frame (2); a limit blocking frame (204) is arranged in a sliding connection in the middle of the adjustment slide groove (201); a travel switch (205) is installed on the adjacent side of the limit blocking frame (204) arranged on the left and right sides; the travel switch (205) and the switch trigger frame (307) are arranged corresponding to each other; an electromagnetic switch valve (107) is arranged on the top of the steam delivery pipe (106); and the travel switch (205) and the electromagnetic switch valve (107) are electrically connected.

2. The nitrotoluene rectification kettle liquid steam entrainment distillation recovery device according to claim 1, characterized in that: The position-limiting blocking frame (204) is slidably connected to the position-limiting adjusting frame (2) via an adjusting slide groove (201); an adjusting screw rod (202) is connected in the middle of the adjusting slide groove (201); an adjusting motor (203) is connected at the shaft end of the adjusting screw rod (202); an adjusting screw sleeve (206) is arranged in the middle of the position-limiting blocking frame (204); and the position-limiting blocking frame (204) is connected to the adjusting screw rod (202) via the adjusting screw sleeve (206).

3. The nitrotoluene rectification kettle liquid steam entrainment distillation recovery device according to claim 1, characterized in that: The interior of the distillation separation kettle (1) is surrounded by an annular stirring frame (4), the outer side of the annular stirring frame (4) is surrounded by a stirring connection ring (401), the annular stirring frame (4) is rotatably connected to the distillation separation kettle (1) via the stirring connection ring (401), the left and right sides of the annular stirring frame (4) are symmetrically connected with spiral blades (402), and the bottom of the annular stirring frame (4) is evenly surrounded by a plurality of stirring blades (403).

4. The nitrotoluene rectification kettle liquid steam entrainment distillation recovery device according to claim 3, characterized in that: The floating conveying plate (3) is provided with a guide sleeve (301) in the middle of the floating conveying plate (3), and a vertical guide rod (101) is fixedly connected inside the distillation separation kettle (1). The floating conveying plate (3) is slidably connected to the vertical guide rod (101) through the guide sleeve (301). The outer wall of the floating conveying plate (3) is surrounded by a spiral driving groove (305). The spiral driving groove (305) and the spiral blade (402) are mutually engaged and slidably connected. When the floating conveying plate (3) moves up and down along the vertical guide rod (101), the spiral driving groove (305) and the spiral blade (402) drive the annular stirring frame (4) to rotate synchronously.

5. The nitrotoluene rectification kettle liquid steam entrainment distillation recovery device according to claim 1, characterized in that: A condensation separation cylinder (5) is arranged above the distillation separation kettle (1), and the condensation delivery pipe (501) is located at the inner center of the condensation separation cylinder (5). An air collecting hood (103) is arranged on the inner top of the distillation separation kettle (1), and the bottom end of the condensation delivery pipe (501) is connected to the air collecting hood (103). A plurality of inclined delivery pipes (502) are evenly arranged around the top of the condensation delivery pipe (501), and a plurality of condensation delivery ports (503) are evenly arranged in the middle of the inclined delivery pipe (502). A conical liquid guide plate (504) is arranged around the bottom of the condensation separation cylinder (5), and an annular liquid collecting trough (505) is arranged around the bottom of the conical liquid guide plate (504), and a condensation output pipe (506) is connected to the bottom of the annular liquid collecting trough (505).

6. The nitrotoluene rectification kettle liquid steam entrainment distillation recovery device according to claim 5, characterized in that: A centrifugal separation cylinder (6) is arranged around the inner side of the condensation separation cylinder (5), a conical guide wall (601) is arranged around the inner side of the centrifugal separation cylinder (6), a plurality of inclined condensing fins (602) are arranged evenly and connected around the inner side of the conical guide wall (601) in a circular shape, the inclined condensing fins (602) are located below the inclined conveying pipe (502), and a plurality of cooling pipes (7) are evenly arranged around the middle of the inclined condensing fins (602).

7. The nitrotoluene rectification kettle liquid steam entrainment distillation recovery device according to claim 6, characterized in that: A rotating connection ring (603) is arranged around the top of the centrifugal separation cylinder (6), and the centrifugal separation cylinder (6) is rotatably connected to the condensation separation cylinder (5) through the rotating connection ring (603). A rotating gear ring (604) is arranged around the outer side of the rotating connection ring (603), and a rotating gear (605) is arranged on the outer side of the rotating gear ring (604) in meshing connection. A rotating motor (606) is connected to the shaft end of the rotating gear (605). The rotating motor (606) drives the centrifugal separation cylinder (6) to rotate through the rotating gear (605) and the rotating gear ring (604), and then drives all the inclined condensation fins (602) to rotate synchronously through the centrifugal separation cylinder (6).

8. The nitrotoluene rectification kettle liquid steam entrainment distillation recovery device according to claim 7, characterized in that: The top and bottom ends of the cooling pipe (7) are both connected to a rotating joint (701), and the top and bottom ends of the cooling pipe (7) are respectively connected to a circulating input pipe (702) and a circulating output pipe (703) through the rotating joint (701). The cooling pipe (7) is rotatably connected to the circulating input pipe (702) or the circulating output pipe (703) through the rotating joint (701), and the outer ends of the circulating input pipe (702) and the circulating output pipe (703) are connected to a finned radiator (705), and the middle of the circulating input pipe (702) is connected to a circulating delivery pump (704).

9. The nitrotoluene rectification kettle liquid steam entrainment distillation recovery device according to claim 5, characterized in that: The outer end of the condensation output pipe (506) is connected to a stratified separation cylinder (8), a separation delivery pipe (801) is vertically arranged at the center of the stratified separation cylinder (8), the condensation output pipe (506) and the top end of the separation delivery pipe (801) are connected to each other, a delivery opening (802) is arranged at the bottom end of the separation delivery pipe (801), a centrifugal turbine disc (803) is arranged below the delivery opening (802), and a centrifugal motor (801) is connected to the shaft end of the centrifugal turbine disc (803). 804), a spacing separation cylinder (805) is arranged around the inner upper side of the stratified separation cylinder (8), a heavy phase separation layer (806) is arranged between the outer wall of the spacing separation cylinder (805) and the inner wall of the stratified separation cylinder (8), a light phase separation layer (807) is arranged between the inner wall of the spacing separation cylinder (805) and the outer wall of the separation conveying pipe (801), and the top ends of the heavy phase separation layer (806) and the light phase separation layer (807) are both connected with a separation output pipe (808).

10. A method for using the nitrotoluene rectification kettle liquid steam entrainment distillation recovery device according to any one of claims 1 to 9, characterized in that: The steps include: S1: a charging stage, in which the nitrotoluene rectification kettle liquid to be treated is added into the distillation separation kettle (1); S2: Start steam delivery, open the electromagnetic switch valve (107) at the top of the steam delivery pipe (106), so that high-temperature and high-pressure steam enters the central delivery pipe (108) through the steam delivery pipe (106), and is transmitted to the sealed gas storage bin (302) inside the floating delivery plate (3) through the central delivery pipe (108); S3: The steam is evenly distributed. The steam in the sealed gas storage bin (302) is evenly distributed to the kettle liquid in the distillation separation kettle (1) through a plurality of delivery openings (304). The steam forms an azeotropic mixture with substances such as nitrotoluene, which causes nitrotoluene to enter the gas phase. The recovered nitrotoluene is transported to an externally connected condensation device via a condensation delivery pipe (501) connected to the top of the distillation separation kettle (1) for condensation recovery. S4: The floating conveying plate (3) moves. As the steam enters the sealed gas storage bin (302), the liquid therein is squeezed out. The floating conveying plate (3) rises due to the decrease in overall density, and the central linkage rod (306) drives the switch trigger frame (307) to move accordingly. S5: triggering the travel switch (205) on the limit adjustment frame (2). When the floating conveying plate (3) rises to a certain height, the switch trigger frame (307) triggers the travel switch (205) on the limit blocking frame (204), controlling the electromagnetic switch valve (107) to close, thereby stopping steam delivery; S6: Steam delivery is suspended. After the steam pressure is lost, the liquid flows back into the sealed gas storage bin (302), and the floating delivery plate (3) sinks due to the increase in overall density; S7: The travel switch (205) on the limit adjustment frame (2) is triggered again. When the floating conveying plate (3) sinks to a certain position, the switch trigger frame (307) triggers the travel switch (205) on the limit blocking frame (204) again, and controls the electromagnetic switch valve (107) to open, and the steam is continuously conveyed; S8: The above steps are repeated repeatedly until the recovery of nitrotoluene is completed.

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