Apparatus and process for reactive distillation of isopropanol
Patent Information
- Application Number
- CN202511053478.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-07-30
- Publication Date
- 2026-09-11
- Estimated Expiration
- 2045-07-30
AI Technical Summary
由于铜基催化剂的活性中心依赖于高度分散的金属Cu0纳米颗粒,但其在80-150℃的反应温度下长期运行时,会因表面扩散效应引发Cu0颗粒团聚(即烧结现象),这导致催化剂粒径显著增大、比表面积骤降,活性位点数量锐减,进而严重削弱其在丙酮加氢反应中的催化效能,因此,工业生产中需定期更换失活催化剂,但该过程需经历反应器停机、开盖卸剂、新装填及氧气置换等复杂工序,尤其是氧气置换阶段,需确保系统氧含量降至安全阈值以下才能重新通入丙酮原料与氢气,这一系列操作会显著降低异丙醇的生产效率;
1.本发明通过设置换料箱,使得催化板能够在换料箱内进行预装填,具体而言,在反应器停机前,操作人员将新催化板预先装入换料箱内,并完成氮气置换以彻底排除换料箱内的氧气,从而在更换时,操作人员能够直接将预装填的催化板推入塔体进行更换,无需在停机后,对塔体内的氢气进行置换,减少了氢气的置换步骤,进而显著缩短了设备停机时间,提高了异丙醇的生产效率。
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Figure CN120679429B_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of isopropanol preparation technology, specifically to an apparatus and process for producing isopropanol by reactive distillation. Background Technology
[0002] Isopropanol, with the molecular formula (CH3)2CHOH, is a colorless, transparent, volatile liquid miscible with ethanol, ether, chloroform, and water. It is an excellent organic solvent, used not only as a solvent for shellac, nitrocellulose, alkaloids, rubber, and oils, but also as a raw material for the synthesis of glycerol, isopropyl acetate, and acetone. It has wide applications in pesticides, electronics, pharmaceuticals, coatings, daily chemicals, and organic synthesis. The main methods for synthesizing isopropanol include direct propylene hydration, indirect sulfuric acid hydration, acetone hydrogenation, isopropyl acetate hydrogenation, and isopropyl acetate transesterification. Among them, the acetone hydrogenation method uses a copper-based catalyst. The specific steps are as follows: first, acetone raw material is dehydrated and deoxygenated to obtain purified acetone. Then, the purified acetone is heated to obtain acetone vapor. The acetone vapor and hydrogen are sent into a hydrogenation reactor. At 80-200℃ and atmospheric pressure, the acetone vapor and hydrogen react to produce isopropanol. Because the active sites of copper-based catalysts depend on highly dispersed metallic Cu 0 Nanoparticles, but when operated for extended periods at reaction temperatures of 80-150℃, can induce Cu diffusion due to surface diffusion effects. 0 Particle agglomeration (i.e., sintering) leads to a significant increase in catalyst particle size, a sharp drop in specific surface area, and a drastic reduction in the number of active sites, which in turn severely weakens its catalytic efficiency in the hydrogenation reaction of acetone. Therefore, in industrial production, deactivated catalysts need to be replaced regularly. However, this process involves complex steps such as reactor shutdown, unloading, refilling, and oxygen replacement. In particular, during the oxygen replacement stage, it is necessary to ensure that the oxygen content in the system drops below the safe threshold before acetone feedstock and hydrogen can be reintroduced. This series of operations will significantly reduce the production efficiency of isopropanol. In view of this, in order to overcome the above-mentioned technical problems, the present invention proposes an apparatus and process for reactive distillation to produce isopropanol, which solves the above-mentioned technical problems. Summary of the Invention
[0003] To overcome the shortcomings of existing technologies, this invention proposes an apparatus and process for reactive distillation to produce isopropanol. This invention utilizes a feed changer box, allowing the catalyst plates to be pre-loaded within the box. Specifically, before reactor shutdown, operators pre-load new catalyst plates into the feed changer box and perform nitrogen purging to completely remove oxygen. This allows operators to directly push the pre-loaded catalyst plates into the column for replacement, eliminating the need for hydrogen purging after shutdown. This reduces the hydrogen purging steps, significantly shortens equipment downtime, and improves isopropanol production efficiency.
[0004] The technical solution adopted by the present invention to solve its technical problem is: the apparatus for producing isopropanol by reactive distillation according to the present invention includes a refining device, a preheater, a hydrogen filter, a hydrogen compressor, a buffer tank, a hydrogen heat exchanger, a hydrogenation reactor, a gas-liquid separator and a recovery tower. The hydrogenation reactor includes a tower body; the tower body includes an upper tower body and a lower tower body; the upper tower body has an inlet at its upper end; the lower tower body has a discharge port at its bottom; a catalytic plate is installed inside the upper tower body; a catalyst is installed inside the catalytic plate; a screw is installed above the catalytic plate; one end of the screw is helically connected to the catalytic plate, and the other end is rotatably connected to the inner wall of the upper tower body; a drive motor is fixedly installed on the outer wall of the upper tower body; a bevel gear shaft is installed at the output end of the drive motor; a bevel gear ring that meshes with the bevel gear shaft is fixedly connected to the upper end of the screw. A material changing box is fixedly connected to one side of the lower tower body; a door is installed at the lower end of the material changing box; connection ports are opened at both the upper and lower ends of the material changing box; a material changing port communicating with the material changing box is opened on the side wall of the lower tower body; a sealing plate is slidably connected to the inner wall of the tower body; the sealing plate is used to block the material changing port; an installation plate is slidably connected inside the material changing box; a through groove is opened in the center of the installation plate; the upper end of the installation plate is connected to the material changing box through a hydraulic push rod; a material changing module is installed at the lower end of the installation plate.
[0005] Preferably, the material changing module includes: A material changing plate; a groove is provided at the lower end of the mounting plate; the material changing plate is slidably connected in the groove; the material changing plate and the groove wall are connected by a connecting spring; a first bevel gear shaft is rotatably connected to the upper end of the mounting plate; the material changing plate and the first bevel gear shaft are connected by a steel wire rope; a second bevel gear shaft is rotatably and sealingly connected to the upper end of the material changing box; the first bevel gear shaft and the second bevel gear shaft mesh; a groove is provided at the upper end of the material changing plate; the catalytic plate is slidably connected in the groove. A lifting unit is installed in a groove; the lifting unit is used to push the catalytic plate to slide within the groove. A connecting unit; the connecting unit is located between the drive motor and the second bevel gear shaft; the drive motor drives the second bevel gear shaft to rotate through the connecting unit.
[0006] Preferably, the connecting unit includes a connecting rod; the output end of the drive motor has a connecting groove; the connecting rod is slidably connected in the connecting groove; a magnet is embedded at the end of the connecting rod near the bottom of the connecting groove; an electromagnetic plate is embedded at the bottom of the connecting groove; a bevel gear ring that meshes with the second bevel gear shaft is fixedly connected to the surface of the connecting rod; and a slot is provided at the end of the bevel gear shaft near the drive motor.
[0007] Preferably, the lifting unit includes an airbag; the airbag is embedded in the bottom of the groove; a hydraulic pump is installed at the upper end of the material changing box; the hydraulic pump is connected to the airbag through a spring hose.
[0008] Preferably, a slider is slidably connected to the inner wall of the sealing plate material exchange box; a metal rope is fixedly connected to the upper end of the slider; and the end of the metal rope away from the slider is fixedly connected to the sealing plate.
[0009] Preferably, the feed changing plate has a circular groove inside; a tilting plate is rotatably connected inside the circular groove; the groove is formed on the upper and lower end faces of the tilting plate; a servo motor is fixedly installed on the outer wall of the lower tower body; a rectangular groove is formed at the output end of the servo motor; a rectangular rod is slidably connected inside the rectangular groove; a slot that mates with the rectangular rod is formed at the end of the tilting plate near the servo motor; a rotating ring is rotatably sealed to the surface of the output shaft of the servo motor; an annular groove communicating with the rectangular groove is formed on the surface of the output shaft of the servo motor; a circular hole communicating with the annular groove is formed on the surface of the rotating ring; and the infusion pump is connected to the circular hole through an infusion pipe.
[0010] Preferably, the inner wall of the groove is provided with a fixing groove; the fixing groove is connected to the slot through an air passage; a solenoid valve is installed in the air passage; a fixing rod is slidably connected in the fixing groove; a slotted plate is slidably and sealingly connected in the slot; a support groove is provided on the side wall of the catalytic plate, which is directly opposite to the fixing groove; a support block is slidably connected in the support groove; the support block is connected to the bottom of the support groove through a support spring.
[0011] Preferably, the inner wall of the circular groove is provided with a positioning groove that communicates with the spring hose; a positioning rod is slidably and sealingly connected in the positioning groove; and a straight groove is provided on the side wall of the flip plate that is directly opposite the positioning groove.
[0012] A process for producing isopropanol by reactive distillation, applicable to the aforementioned apparatus for producing isopropanol by reactive distillation, comprising the following steps: S1: Acetone is dehydrated and deoxygenated through a refining device, and then the refined acetone is sent to a preheater to be heated to vaporization. At this time, the hydrogen in the hydrogen tank is filtered by a hydrogen filter, pressurized by a hydrogen compressor, buffered by a buffer tank after the hydrogen compressor, and finally heat exchanged by a hydrogen heat exchanger. S2: During the acetone refining process, switch the main inlet valve of the upper tower to allow nitrogen to enter the hydrogenation reactor through the inlet, pushing the internal air out of the discharge port of the lower tower to complete the air replacement of the reactor; then switch the main inlet valve to the preheater exhaust pipe, thereby mixing the heat-exchanged hydrogen with the vaporized acetone at a molar ratio of 3:1 and transporting it to the hydrogenation reactor. S3: As the acetone vapor and hydrogen mixture enter the hydrogenation reactor, the activated catalyst catalyzes the reaction between acetone and hydrogen. The isopropanol and unreacted raw materials produced by the reaction enter the gas-liquid separator from the bottom discharge port of the lower tower. The gas phase hydrogen and the liquid phase isopropanol and unreacted acetone are separated, and the liquid phase is transported to the recovery tower to recover acetone, finally obtaining a high-purity isopropanol product. S4: During the process of producing isopropanol in the hydrogenation reactor, the user opens the box door, first pre-installs the new catalyst plate on the tilting plate, and then replaces the oxygen in the feed exchange box. When the hydrogenation reactor is shut down and a new catalyst plate needs to be replaced, the tilting plate is controlled to drive the new catalyst plate into the lower tower through the feed exchange port. S5: After the tilting plate enters the lower tower body, control the tilting plate to tilt so that the empty groove below the tilting plate faces upward. This allows the screw to release the old catalyst plate into the empty groove. Control the fixing rod to fix the old catalyst plate in the empty groove. Then control the tilting plate to rotate so that the tilting plate drives the new catalyst plate to face upward. The new catalyst plate is then inserted into the screw under the push of the airbag. This causes the screw to drive the new catalyst plate to rise and seal it to the upper tower body, completing the replacement of the catalyst plate.
[0013] The beneficial effects of this invention are as follows: 1. This invention, by setting up a replacement tank, allows the catalyst plates to be pre-loaded within the tank. Specifically, before the reactor is shut down, the operator pre-loads new catalyst plates into the replacement tank and completes nitrogen purging to completely remove oxygen from the tank. Thus, during replacement, the operator can directly push the pre-loaded catalyst plates into the tower for replacement, eliminating the need to purge the hydrogen in the tower after shutdown. This reduces the hydrogen purging steps, significantly shortens equipment downtime, and improves the production efficiency of isopropanol.
[0014] 2. This invention controls the delivery of nitrogen gas from the connection port at the bottom of the replacement tank to the tank. This allows nitrogen gas to enter the tower body through the replacement port during the replacement of the catalyst plate, preventing residual reaction products in the tower from entering the replacement tank through the replacement port. It also prevents leakage of reaction products from the replacement tank when operators open the door to remove the old catalyst plate, reducing environmental pollution and protecting the health of operators. Attached Figure Description
[0015] The present invention will be further described below with reference to the accompanying drawings and embodiments.
[0016] Figure 1 This is a perspective view of the hydrogenation reactor used in this invention; Figure 2 This is a schematic diagram of the structure of the hydrogenation reactor used in this invention; Figure 3 yes Figure 2 Enlarged view of point A in the middle; Figure 4 yes Figure 2 Enlarged view of point B in the middle; Figure 5 This is a partial cross-sectional view of the material changing plate used in this invention; Figure 6 This is a perspective view of the transmission of the sealing plate used in this invention; Figure 7 This is a process flow diagram of the present invention; In the diagram: 1. Upper tower body; 11. Air inlet; 12. Catalytic plate; 121. Support groove; 122. Support block; 123. Support spring; 13. Screw; 131. Bevel gear ring; 14. Drive motor; 141. Bevel gear shaft; 142. Connecting groove; 143. Connecting rod; 144. Magnet; 145. Electromagnetic plate; 146. Bevel gear ring; 147. Slot; 2. Lower tower body; 21. Discharge port; 22. Material changing port; 221. Sealing plate; 23. Servo motor; 231. Rectangular groove; 232. Rectangular rod; 233. Slot; 24. Rotary ring; 241. Annular groove; 242. Circular hole; 243. 1. Infusion tube; 3. Material changing box; 31. Box door; 32. Connection port; 33. Mounting plate; 331. Through groove; 332. Hydraulic push rod; 333. Slide groove; 334. Connecting spring; 335. No. 1 bevel gear shaft; 336. Steel wire rope; 337. No. 2 bevel gear shaft; 34. Material changing plate; 341. Circular groove; 342. Positioning groove; 343. Positioning rod; 344. Straight groove; 35. Flipping plate; 351. Groove; 352. Airbag; 36. Hydraulic pump; 361. Spring hose; 37. Slider; 371. Metal rope; 38. Fixing groove; 381. Air passage; 382. Fixing rod; 383. Clamping plate. Detailed Implementation
[0017] To make the technical means, creative features, objectives and effects of this invention easier to understand, the invention will be further described below in conjunction with specific embodiments.
[0018] like Figures 1 to 7 As shown, the apparatus for producing isopropanol by reactive distillation according to the present invention includes a refining device, a preheater, a hydrogen filter, a hydrogen compressor, a buffer tank, a hydrogen heat exchanger, a hydrogenation reactor, a gas-liquid separator, and a recovery tower. The hydrogenation reactor includes a tower body; the tower body includes an upper tower body 1 and a lower tower body 2; the upper tower body 1 has an inlet 11 at its upper end; the lower tower body 2 has a discharge port 21 at its bottom; a catalyst plate 12 is disposed inside the upper tower body 1; a catalyst is installed inside the catalyst plate 12; a screw 13 is disposed above the catalyst plate 12; one end of the screw 13 is helically connected to the catalyst plate 12, and the other end is rotatably connected to the inner wall of the upper tower body 1; a drive motor 14 is fixedly installed on the outer wall of the upper tower body 1; a bevel gear shaft 141 is installed at the output end of the drive motor 14; a bevel gear ring 131 that meshes with the bevel gear shaft 141 is fixedly connected to the upper end of the screw 13; A material changing box 3 is fixedly connected to one side of the lower tower body 2; a box door 31 is installed at the lower end of the material changing box 3; connection ports 32 are opened at both the upper and lower ends of the material changing box 3; a material changing port 22 communicating with the material changing box 3 is opened on the side wall of the lower tower body 2; a sealing plate 221 is slidably connected to the inner wall of the tower body; the sealing plate 221 is used to cover the material changing port 22; an installation plate 33 is slidably connected inside the material changing box 3; a through groove 331 is opened in the center of the installation plate 33; the upper end of the installation plate 33 is connected to the material changing box 3 through a hydraulic push rod 332; a material changing module is installed at the lower end of the installation plate 33.
[0019] In one embodiment of the present invention, the material changing module includes: A material changing plate 34 is provided; a groove 333 is provided at the lower end of the mounting plate 33; the material changing plate 34 is slidably connected in the groove 333; the material changing plate 34 and the groove wall of the groove 333 are connected by a connecting spring 334; a first bevel gear shaft 335 is rotatably connected to the upper end of the mounting plate 33; the material changing plate 34 and the first bevel gear shaft 335 are connected by a steel wire rope 336; a second bevel gear shaft 337 is rotatably and sealingly connected to the upper end of the material changing box 3; the first bevel gear shaft 335 and the second bevel gear shaft 337 mesh; a groove 351 is provided at the upper end of the material changing plate 34; the catalyst plate 12 is slidably connected in the groove 351. A lifting unit is installed in the groove 351; the lifting unit is used to push the catalytic plate 12 to slide within the groove 351. A connecting unit is located between the drive motor 14 and the second bevel gear shaft 337. The drive motor 14 drives the second bevel gear shaft 337 to rotate through the connecting unit.
[0020] In one embodiment of the present invention, the connecting unit includes a connecting rod 143; the output end of the drive motor 14 is provided with a connecting groove 142; the connecting rod 143 is slidably connected in the connecting groove 142; a magnet 144 is embedded in one end of the connecting rod 143 near the bottom of the connecting groove 142; an electromagnetic plate 145 is embedded in the bottom of the connecting groove 142; a bevel gear ring 146 that meshes with the second bevel gear shaft 337 is fixedly connected to the surface of the connecting rod 143; and a slot 147 is provided in one end of the bevel gear shaft 141 near the drive motor 14.
[0021] In one embodiment of the present invention, the lifting unit includes an airbag 352; the airbag 352 is embedded in the bottom of the groove 351; a hydraulic pump 36 is installed on the upper end of the material changing box 3; the hydraulic pump 36 is connected to the airbag 352 through a spring hose 361.
[0022] In one embodiment of the present invention, a slider 37 is slidably connected to the inner wall of the material changing box 3 of the sealing plate 221; a metal rope 371 is fixedly connected to the upper end of the slider 37; and the end of the metal rope 371 away from the slider 37 is fixedly connected to the sealing plate 221.
[0023] In one embodiment of the present invention, a circular groove 341 is provided inside the material changing plate 34; a flipping plate 35 is rotatably connected inside the circular groove 341; a groove 351 is provided on the upper and lower end faces of the flipping plate 35; a servo motor 23 is fixedly installed on the outer wall of the lower tower body 2; a rectangular groove 231 is provided at the output end of the servo motor 23; a rectangular rod 232 is slidably connected inside the rectangular groove 231; a slot 233 that cooperates with the rectangular rod 232 is provided at the end of the flipping plate 35 near the servo motor 23; a rotating ring 24 is rotatably and sealingly connected to the surface of the output shaft of the servo motor 23; an annular groove 241 communicating with the rectangular groove 231 is provided on the surface of the output shaft of the servo motor 23; a circular hole 242 communicating with the annular groove 241 is provided on the surface of the rotating ring 24; and the infusion pump is connected to the circular hole 242 through an infusion pipe 243.
[0024] In one embodiment of the present invention, a fixing groove 38 is provided on the inner wall of the groove 351; the fixing groove 38 is connected to the slot 233 through the air passage 381; a solenoid valve is installed in the air passage 381; a fixing rod 382 is slidably connected in the fixing groove 38; a slot plate 383 is slidably and sealingly connected in the slot 233; a support groove 121 is provided on the side wall of the catalytic plate 12, which is directly opposite to the fixing groove 38; a support block 122 is slidably connected in the support groove 121; the support block 122 and the bottom of the support groove 121 are connected by a support spring 123.
[0025] In one embodiment of the present invention, the inner wall of the circular groove 341 is provided with a positioning groove 342 that communicates with the spring hose 361; a positioning rod 343 is slidably and sealingly connected in the positioning groove 342; and a straight groove 344 is provided on the side wall of the flip plate 35 that is directly opposite to the positioning groove 342.
[0026] During operation, the active sites of the copper-based catalyst depend on highly dispersed metallic Cu. 0 Nanoparticles, but when operated for extended periods at reaction temperatures of 80-150℃, can induce Cu diffusion due to surface diffusion effects. 0 Particle agglomeration (i.e., sintering) leads to a significant increase in catalyst particle size, a sharp decrease in specific surface area, and a drastic reduction in the number of active sites, which severely weakens its catalytic efficiency in the hydrogenation reaction of acetone. Therefore, in industrial production, deactivated catalysts need to be replaced regularly. However, this process involves complex steps such as reactor shutdown, unloading, refilling, and oxygen replacement. In particular, during the oxygen replacement stage, it is necessary to ensure that the oxygen content in the system drops below the safe threshold before acetone feedstock and hydrogen can be reintroduced. This series of operations will significantly reduce the production efficiency of isopropanol.
[0027] Therefore, by setting up a replacement tank 3, the present invention allows the catalyst plate 12 to be pre-filled in the replacement tank 3. Specifically, before the reactor is shut down, the operator pre-fills the new catalyst plate 12 into the replacement tank 3 and completes nitrogen purging to completely remove the oxygen in the replacement tank 3. Thus, when replacing the catalyst plate, the operator can directly push the pre-filled catalyst plate 12 into the tower for replacement, without the need to replace the hydrogen in the tower after shutdown. This reduces the hydrogen replacement steps, thereby significantly shortening the equipment downtime and improving the production efficiency of isopropanol.
[0028] Before preparing isopropanol, the user first feeds acetone raw material into a refining device (such as a molecular sieve adsorption tower) to dehydrate and deoxygenate the acetone raw material, obtaining the desired refined acetone. The refined acetone is then fed into a preheater for heating at a temperature of 80-120°C to vaporize the acetone. At the same time, the hydrogen in the hydrogen tank is filtered by a hydrogen filter, pressurized by a hydrogen compressor, buffered by a buffer tank after the hydrogen compressor, and finally heat-exchanged by a hydrogen heat exchanger. Since the exhaust pipe of the hydrogen heat exchanger is connected to the exhaust pipe of the preheater, the hydrogen supplied by the hydrogen heat exchanger can mix with the acetone vapor supplied by the preheater. At this time, the acetone vapor and hydrogen in the exhaust pipe of the preheater are mixed at a molar ratio of 1:3.
[0029] In the acetone refining process, the inlet 11 of the upper column 1 is connected to the nitrogen supply pipeline and the preheater exhaust pipeline via a T-shaped inlet manifold. During nitrogen purging, the user switches the valve in the inlet manifold to connect the inlet 11 at the upper end of the upper column 1 to the external nitrogen supply pipeline, allowing nitrogen to enter the hydrogenation reactor through inlet 11. The air in the hydrogenation reactor is then discharged from the discharge port at the lower end of the lower column 2 under the push of the nitrogen, thus replacing the air in the hydrogenation reactor. Then, the inlet 11 at the upper end of the upper column 1 is switched to connect to the preheater. The exhaust pipe connection allows the acetone vapor and hydrogen mixed in the preheater exhaust pipe to enter the upper tower 1 through the inlet 11. As the mixture of acetone vapor and hydrogen continuously enters the upper tower 1, the raw material gas mixed with acetone vapor and hydrogen flows downward to the catalytic plate 12. Because the surface of the catalytic plate 12 has pores, the raw material gas can pass through the pores and flow downward, allowing it to contact the catalyst inside the catalytic plate 12. This causes the copper-based catalyst to be activated by hydrogen (the copper-based catalyst is reduced to Cu). 0 The process involves hydrogenating the raw material gas under the action of an activated catalyst to produce isopropanol. The product after the reaction (containing isopropanol and a small amount of unreacted raw material) continues to flow downward and is finally discharged from the discharge port 21 at the bottom of the lower tower 2. Since the discharge port 21 is connected to the gas-liquid separator, the product after the reaction is transported to the gas-liquid separator can be separated into gas and liquid phases, resulting in the separation of the gas phase (hydrogen) and the liquid phase (isopropanol and unreacted acetone). The separated liquid phase is transported to the recovery tower to recover the unreacted acetone, and finally, high-purity isopropanol product is obtained.
[0030] In its initial state, the connection port 32 on one side of the material changing box 3 is connected to the external nitrogen supply pipeline. Before filling the tower with nitrogen, the user controls the hydraulic push rod 332 to move, causing the hydraulic push rod 332 to push the mounting plate 33 down. This causes the mounting plate 33 to drive the material changing plate 34 connected to its lower end down synchronously, causing the material changing plate 34 to move continuously towards the slider 37 until the material changing plate 34 contacts the slider 37. This allows the material changing plate 34 to push the slider 37 to slide down along the inner wall of the material changing box 3, allowing the descending slider 37 to pass through the nitrogen supply system. The sealing plate 221 is pulled upward along the inner wall of the lower tower body 2 by the metal rope 371, so that the sealing plate 221 slides and seals against the inner wall of the lower tower body 2 until the sealing plate 221 slides to the material exchange port 22, so that the sealing plate 221 seals and blocks the material exchange port 22. Therefore, when the raw material gas is transported into the tower body, the raw material gas and the reaction products located in the tower body will not enter the material exchange box 3 through the material exchange port 22. This ensures that the raw material gas can fully react in the tower body and that the reaction products can be completely discharged from the discharge port 21 and completely collected.
[0031] When pre-replacing the catalyst plate 12, the user needs to open the door 31 on one side of the replacement box 3, so that one side of the replacement box 3 is open, exposing the mounting plate 33 and the replacement plate 34. The user puts the catalyst plate 12 into the through groove 331 from the upper end of the mounting plate 33, so that the catalyst plate 12 falls into the groove 351 at the upper end of the replacement plate 34 under its own weight. In the initial state, the connection end of the positioning groove 342 and the spring hose 361 is also equipped with a solenoid valve. Therefore, by controlling the solenoid valve to open the hydraulic pump 36, hydraulic oil is delivered into the positioning groove 342, so that the positioning rod 343 in the positioning groove 342 will be pushed out of the positioning groove 342 and inserted into the straight groove 344 by the hydraulic oil, so that the flip plate 35 is fixedly connected to the replacement plate 34 through the positioning rod 343. Therefore, when the catalyst plate 12 is placed in the groove 351 at the upper end of the flip plate 35, the flip plate 35 can effectively support the catalyst plate 12.
[0032] After the pre-installation of the new catalyst plate 12 is completed, the door 31 on one side of the material exchange box 3 is opened. Since the connection port 32 at the lower end of the material exchange box 3 is connected to the external nitrogen supply pipeline, nitrogen is controlled to be supplied from the connection port 32 at the lower end of the material exchange box 3 to the material exchange box 3, so that the air in the material exchange box 3 is discharged through the connection port 32 at the upper end. After the air in the material exchange box 3 is completely discharged, the connection port 32 of the material exchange box 3 is covered.
[0033] When the catalyst needs to be replaced, the user controls the hydraulic push rod 332 to pull the mounting plate 33 upward, causing the mounting plate 33 to drive the replacement plate 34 upward synchronously. During the upward movement of the mounting plate 33, the mounting plate 33 no longer exerts a downward pushing force on the slider 37. At this time, the sealing plate 221, under its own gravity, pulls the slider 37 upward via the metal rope 371 until the mounting plate 33 drives the replacement plate 34 to the replacement port 22. At this time, the sealing plate 221 falls below the replacement port 22 under the action of gravity, and the replacement port 22 is now in the open state. Simultaneously, the first bevel gear shaft 335 and the second bevel gear shaft 337 at the upper end of the mounting plate 33 mesh. Since the second bevel gear shaft 337 is a double-headed bevel gear, and the electromagnetic plate 145 is initially de-energized, the magnet 144 generates magnetism on the bottom of the connecting groove 142. The attraction force causes the connecting rod 143 to be positioned in the connecting groove 142 under the magnetic force of the magnet 144. At this time, the connecting rod 143 drives the bevel gear ring 146 on the surface to mesh with the upper end of the second bevel gear shaft 337, controlling the drive motor 14 to run. The drive motor 14 can drive the bevel gear ring 146 to rotate through the connecting rod 143, so that the bevel gear ring 146 drives the second bevel gear shaft 337 that meshes with it to rotate, so that the second bevel gear shaft 337 drives the first bevel gear shaft 335 to rotate. During the rotation of the first bevel gear shaft 335, it can drive the steel wire rope 336 fixed to the surface to wrap around its surface. The end of the steel wire rope 336 away from the first bevel gear shaft 335 pulls the material changing plate 34 to stretch the connecting spring 334 to slide in the slide groove 333, so that the material changing plate 34 enters the lower tower body 2 through the material changing port 22.
[0034] As the material changing plate 34 enters the lower tower body 2, it continuously approaches the servo motor 23, causing the rectangular rod 232 at one end of the servo motor 23 to continuously approach the slot 233 until the material changing plate 34 contacts the inner wall of the lower tower body 2. At this point, the hydraulic pump 36 delivers hydraulic oil into the rectangular groove 231, allowing the hydraulic oil to push the rectangular rod 232 out of the groove and into the slot 233. This causes the plate 383 in the slot 233 to be pushed into the bottom of the slot by the rectangular rod 232. Since the slot 233 is filled with hydraulic oil, the plate 383 is pushed by the rectangular rod 232 into the bottom of the slot. The card plate 383 pushes the hydraulic oil in the card slot 233 into the air passage 381. By controlling the solenoid valve in the air passage 381, which is connected to the upper fixing slot 38 of the flip plate 35, the hydraulic oil in the card slot 233 can flow into the fixing slot 38 above the flip plate 35 through the air passage 381. The fixing rod 382 in the fixing slot 38 is pushed out of the fixing slot 38 by the hydraulic oil and inserted into the support slot 121 on the side wall of the catalyst plate 12. The support block 122 in the support slot 121 is pushed by the fixing rod 382 and squeezes the support spring 123 into the support slot 121. At this time, the catalyst plate 12 is fixed to the flip plate 35 by the support rod.
[0035] After the new catalyst plate 12 is fixed to the tilting plate 35 by the support rod, the hydraulic pump 36 is controlled to run, so that the hydraulic pump 36 draws out the hydraulic oil in the positioning groove 342 through the spring hose 361, so that the positioning rod 343 in the positioning groove 342 enters the positioning groove 342 under negative pressure, so that the tilting plate 35 is rotatably connected to the material changing plate 34. At this time, the servo motor 23 is controlled to run, so that the servo motor 23 drives the tilting plate 35 to rotate 180° through the rectangular rod 232, so that the tilting plate 35 drives the new catalyst plate 12 to rotate synchronously until the new catalyst plate 12 rotates and faces the bottom of the lower tower body 2. The hydraulic pump 36 is then controlled to deliver hydraulic oil into the positioning groove 342, so that the tilting plate 12 rotates synchronously. Plate 35 and material changing plate 34 are reconnected via positioning rod 343. At this time, the electromagnetic plate 145 in the control connecting groove 142 is energized, causing the magnetic poles generated by the electromagnetic plate 145 to be the same as the magnetic poles of magnet 144. Under the action of magnetic repulsion, magnet 144 pushes the connecting rod 143 connected to it out of the connecting groove 142. This causes the connecting rod 143 to move the bevel gear ring 146 away from the second bevel gear shaft 337, allowing the connecting rod 143 to insert into slot 147. This connects the drive motor 14 to the bevel gear shaft 141 via the connecting rod 143. Since the rectangular rod 232 is inserted into the slot 233, a sliding sealing contact is formed between the rectangular rod 232 and the slot 233. At this time, the rectangular rod 23... 2. The friction between the plate and the groove wall of slot 233 is greater than the restoring force of the connecting spring 334, making it impossible for the connecting spring 334 to pull the changing plate 34 away from the lower tower body 2. At this time, the drive motor 14 is controlled to run, so that the drive motor 14 can drive the bevel gear shaft 141 to rotate, so that the bevel gear shaft 141 can drive the bevel gear ring 131 meshing with it to rotate, so that the bevel gear ring 131 drives the screw 13 to rotate, so that the screw 13 can drive the old catalyst plate 12 connected to the surface spiral drive to descend. At the same time, the hydraulic pump 36 is controlled to deliver hydraulic oil through the spring hose 361 into the air bag 352, so that the air bag 352 is filled with hydraulic oil, causing the air bag 352 to expand, and the old catalyst plate 12 falling down. When the catalytic plate 12 passes the screw 13, the old catalytic plate 12 will fall on the upper end of the airbag 352. The hydraulic pump 36 is controlled to draw hydraulic oil from the airbag 352, causing the airbag 352 to contract. At this time, the old catalytic plate 12 located on the upper end of the airbag 352 descends with the airbag 352 until the old catalytic plate 12 falls into the groove 351. At this time, the solenoid valve near the groove 351 is opened and the solenoid plate near the new catalytic plate 12 is closed, so that the hydraulic pump 36 delivers hydraulic oil into the fixing groove 38 near the old catalytic plate 12. The fixing rod 382 in the fixing groove 38 is pushed by the hydraulic oil and inserted into the support groove 121 on the side wall of the old catalytic plate 12. At this time, the old catalytic plate 12 is connected to the flipping plate 35.
[0036] After the old catalyst plate 12 is connected to the flip plate 35, the hydraulic pump 36 is first controlled to draw hydraulic oil from the positioning groove 342, so that the support spring 123 pushes the positioning rod 343 into the positioning groove 342 through the support block 122, so that the flip plate 35 is rotatably connected to the material replacement plate 34. At this time, the servo motor 23 is controlled to drive the flip plate 35 to rotate 180°, so that the flip plate 35 drives the new catalyst plate 12 to face upward. Then, the flip plate 35 is controlled to connect to the material replacement plate 34 through the positioning rod 343. At this time, the solenoid valve near the new catalyst plate 12 is first controlled to open, and then the hydraulic pump 36 is controlled to draw hydraulic oil from the rectangular groove 231, so that part of the rectangular rod 232 extends out of the slot 233. At this time, the retaining plate 383 in the slot 233 fixes the spring. Pushing away from the bottom of the slot 233, the hydraulic oil in the fixing slot 38 flows back into the slot 233 through the opened solenoid valve, causing the fixing rod 382 near the new catalyst plate 12 to extend out of the support slot 121, so that the new catalyst plate 12 is no longer fixed to the flip plate 35. The solenoid valve near the new catalyst plate 12 closes, and then the hydraulic pump 36 is controlled to deliver hydraulic oil into the air bag 352, causing the air bag 352 to extend. The extended air bag 352 can push the new catalyst plate 12 up until the new catalyst plate 12 contacts the screw 13, so that the screw 13 is inserted into the threaded groove of the new catalyst plate 12. The drive motor 14 is controlled to drive the screw 13 to rotate, so that the screw 13 can drive the new catalyst plate 12 up, thereby completing the replacement of the catalyst plate 12.
[0037] After the catalytic converter plate 12 is replaced, the hydraulic pump 36 is first controlled to completely extract the hydraulic oil from the rectangular groove 231, so that the rectangular rod 232 is fully inserted into the rectangular groove 231. At this time, the rectangular rod 232 is separated from the flip plate 35. Then, the electromagnetic plate 145 is de-energized, so that the bevel gear ring 146 enters the connecting groove 142 under the drive of the connecting rod 143. This causes the connecting rod 143 to drive the bevel gear ring 146 to mesh with the second bevel gear shaft 337 again. At this time, the drive motor 14 is controlled to drive the second bevel gear shaft 337 in reverse. The rotation causes the No. 2 bevel gear shaft 337 to drive the No. 1 bevel gear shaft 335 to rotate in the opposite direction, causing the No. 1 bevel gear shaft 335 to release the steel wire rope 336 on its surface. This causes the connecting spring 334 to pull the material changing plate 34 out of the lower tower body 2 and into the material changing box 3. Then, the hydraulic push rod 332 is controlled to extend, causing the hydraulic push rod 332 to push the material changing plate 34 to the box door 31. At this time, the slider 37 located below the material changing plate 34 is pushed by the material changing plate 34 to pull the sealing plate 221 to reset, so that the material changing port 22 is sealed again.
[0038] During the replacement of catalyst plate 12, nitrogen gas is controlled to be delivered from the connection port 32 at the lower end of the replacement tank 3 into the replacement tank 3, so that the nitrogen gas can enter the tower body through the replacement port 22. This prevents the reaction products remaining in the tower from entering the replacement tank 3 through the replacement port 22, and prevents the leakage of reaction products into the replacement tank 3 when the operator opens the door 31 to take out the old catalyst plate 12 to be replaced in the replacement tank 3. This reduces environmental pollution and protects the health of the operators.
[0039] A process for producing isopropanol by reactive distillation, applicable to the aforementioned apparatus for producing isopropanol by reactive distillation, comprising the following steps: S1: Acetone is dehydrated and deoxygenated through a refining device, and then the refined acetone is sent to a preheater to be heated to vaporization. At this time, the hydrogen in the hydrogen tank is filtered by a hydrogen filter, pressurized by a hydrogen compressor, buffered by a buffer tank after the hydrogen compressor, and finally heat exchanged by a hydrogen heat exchanger. S2: During the acetone refining process, switch the main inlet valve of the upper column 1 to allow nitrogen to enter the hydrogenation reactor through the inlet 11, pushing the internal air out of the discharge port of the lower column 2 to complete the air replacement of the reactor; then switch the main inlet valve to the preheater exhaust pipe, thereby mixing the heat-exchanged hydrogen with the vaporized acetone at a molar ratio of 3:1 and transporting it to the hydrogenation reactor; S3: As the acetone vapor and hydrogen mixture enter the hydrogenation reactor, the activated catalyst catalyzes the reaction between acetone and hydrogen. The isopropanol and unreacted raw materials generated by the reaction enter the gas-liquid separator from the discharge port 21 at the bottom of the lower tower 2. The gas phase hydrogen and the liquid phase isopropanol and unreacted acetone are separated, and the liquid phase is sent to the recovery tower to recover acetone, finally obtaining a high-purity isopropanol product. S4: During the process of producing isopropanol in the hydrogenation reactor, the user opens the box door 31, first pre-installs the new catalyst plate 12 on the tilting plate 35, and then replaces the oxygen in the feed box 3. When the hydrogenation reactor is shut down and the new catalyst plate 12 needs to be replaced, the tilting plate 35 is controlled to drive the new catalyst plate 12 into the lower tower body 2 through the feed inlet 22. S5: After the tilting plate 35 enters the lower tower body 2, control the tilting plate 35 to tilt so that the empty groove 351 below the tilting plate 35 faces upward, so that the screw 13 releases the old catalyst plate 12 into the empty groove 351. Control the fixing rod 382 to fix the old catalyst plate 12 in the empty groove 351. Then control the tilting plate 35 to rotate so that the tilting plate 35 drives the new catalyst plate 12 to face upward, so that the new catalyst plate 12 is inserted into the screw 13 under the push of the air bag 352, so that the screw 13 drives the new catalyst plate 12 to rise and seal it to the upper tower body 1, thus completing the replacement of the catalyst plate 12.
[0040] The foregoing has shown and described the basic principles, main features, and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited to the above embodiments. The embodiments and descriptions in the specification are merely illustrative of the principles of the invention. Various changes and modifications can be made to the invention without departing from its spirit and scope, and all such changes and modifications fall within the scope of the present invention as claimed. The scope of protection of the present invention is defined by the appended claims and their equivalents.
Claims
1. An apparatus for producing isopropanol by reactive distillation, comprising a refining unit, a preheater, a hydrogen filter, a hydrogen compressor, a buffer tank, a hydrogen heat exchanger, a hydrogenation reactor, a gas-liquid separator, and a recovery tower; characterized in that: The hydrogenation reactor includes a tower body; the tower body includes an upper tower body (1) and a lower tower body (2); the upper tower body (1) has an air inlet (11) at its upper end; the lower tower body (2) has a discharge port (21) at its bottom; a catalyst plate (12) is provided inside the upper tower body (1); a catalyst is installed inside the catalyst plate (12); a screw (13) is provided above the catalyst plate (12); one end of the screw (13) is screw-driven to the catalyst plate (12), and the other end is rotatably connected to the inner wall of the upper tower body (1); a drive motor (14) is fixedly installed on the outer wall of the upper tower body (1); a bevel gear shaft (141) is installed at the output end of the drive motor (14); a bevel gear ring (131) that meshes with the bevel gear shaft (141) is fixedly connected to the upper end of the screw (13); A material exchange box (3) is fixedly connected to one side of the lower tower body (2); a box door (31) is installed at the lower end of the material exchange box (3); connection ports (32) are opened at both the upper and lower ends of the material exchange box (3); a material exchange port (22) communicating with the material exchange box (3) is opened on the side wall of the lower tower body (2); a sealing plate (221) is slidably connected to the inner wall of the tower body; the sealing plate (221) is used to cover the material exchange port (22); an installation plate (33) is slidably connected inside the material exchange box (3); a through groove (331) is opened in the center of the installation plate (33); the upper end of the installation plate (33) is connected to the material exchange box (3) through a hydraulic push rod (332); a material exchange module is installed at the lower end of the installation plate (33); The material changing module includes: A material changing plate (34); a groove (333) is provided at the lower end of the mounting plate (33); the material changing plate (34) is slidably connected in the groove (333); the material changing plate (34) and the groove wall of the groove (333) are connected by a connecting spring (334); a first bevel gear shaft (335) is rotatably connected to the upper end of the mounting plate (33); the material changing plate (34) and the first bevel gear shaft (335) are connected by a steel wire rope (336); a second bevel gear shaft (337) is rotatably and sealingly connected to the upper end of the material changing box (3); the first bevel gear shaft (335) and the second bevel gear shaft (337) mesh; a groove (351) is provided at the upper end of the material changing plate (34); the catalyst plate (12) is slidably connected in the groove (351); A lifting unit is installed in a groove (351); the lifting unit is used to push the catalytic plate (12) to slide within the groove (351); A connecting unit; the connecting unit is located between the drive motor (14) and the second bevel gear shaft (337); the drive motor (14) drives the second bevel gear shaft (337) to rotate through the connecting unit; The connecting unit includes a connecting rod (143); the output end of the drive motor (14) is provided with a connecting groove (142); the connecting rod (143) is slidably connected in the connecting groove (142); a magnet (144) is embedded in one end of the connecting rod (143) near the bottom of the connecting groove (142); an electromagnetic plate (145) is embedded in the bottom of the connecting groove (142); a bevel gear ring (146) that meshes with the second bevel gear shaft (337) is fixedly connected to the surface of the connecting rod (143); a slot (147) is provided in one end of the bevel gear shaft (141) near the drive motor (14); The lifting unit includes an airbag (352); the airbag (352) is embedded in the bottom of the groove (351); a hydraulic pump (36) is installed on the upper end of the material changing box (3); the hydraulic pump (36) is connected to the airbag (352) through a spring hose (361); The material changing plate (34) has a circular groove (341) inside; a flip plate (35) is rotatably connected inside the circular groove (341); a groove (351) is formed on the upper and lower end faces of the flip plate (35); a servo motor (23) is fixedly installed on the outer wall of the lower tower body (2); a rectangular groove (231) is formed at the output end of the servo motor (23); a rectangular rod (232) is slidably connected inside the rectangular groove (231); the flip plate (35) is close to the servo motor. One end of the servo motor (23) is provided with a slot (233) that mates with the rectangular rod (232); the output shaft surface of the servo motor (23) is rotatably sealed with a rotating ring (24); the output shaft surface of the servo motor (23) is provided with an annular groove (241) that communicates with the rectangular groove (231); the surface of the rotating ring (24) is provided with a circular hole (242) that communicates with the annular groove (241); the infusion pump is connected to the circular hole (242) through an infusion pipe (243); The inner wall of the groove (351) is provided with a fixing groove (38); the fixing groove (38) is connected to the slot (233) through the air passage (381); a solenoid valve is installed in the air passage (381); a fixing rod (382) is slidably connected in the fixing groove (38); a slot plate (383) is slidably and sealingly connected in the slot (233); a support groove (121) is provided on the side wall of the catalyst plate (12) opposite to the fixing groove (38); a support block (122) is slidably connected in the support groove (121); the support block (122) is connected to the bottom of the support groove (121) through a support spring (123).
2. A device for the reactive distillation of isopropanol according to claim 1, characterized in that The sealing plate (221) is slidably connected to the inner wall of the material changing box (3) by a slider (37); a metal rope (371) is fixedly connected to the upper end of the slider (37); the end of the metal rope (371) away from the slider (37) is fixedly connected to the sealing plate (221).
3. The apparatus for reactive distillation to produce isopropanol according to claim 1, characterized in that: The inner wall of the circular groove (341) is provided with a positioning groove (342) that communicates with the spring hose (361); a positioning rod (343) is slidably and sealed in the positioning groove (342); and a straight groove (344) is provided on the side wall of the flip plate (35) that is directly opposite to the positioning groove (342).
4. A process for reactive distillation to produce isopropanol, the process being applicable to the apparatus for reactive distillation to produce isopropanol as described in any one of claims 1-3, characterized in that: The steps of this process are as follows: S1: Acetone is dehydrated and deoxygenated through a refining device, and then the refined acetone is sent to a preheater to be heated to vaporization. At this time, the hydrogen in the hydrogen tank is filtered by a hydrogen filter, pressurized by a hydrogen compressor, buffered by a buffer tank after the hydrogen compressor, and finally heat exchanged by a hydrogen heat exchanger. S2: During the refining of acetone, switch the main inlet valve of the upper tower (1) so that nitrogen enters the hydrogenation reactor through the inlet (11) and pushes the internal air out of the discharge port of the lower tower (2) to complete the air replacement of the reactor; then switch the main inlet valve to the preheater exhaust pipe so that the heat exchanged hydrogen and the vaporized acetone are mixed at a molar ratio of 3:1 and transported to the hydrogenation reactor; S3: As the acetone vapor and hydrogen mixture enter the hydrogenation reactor, the activated catalyst catalyzes the reaction of acetone and hydrogen. The isopropanol and unreacted raw materials generated by the reaction enter the gas-liquid separator from the bottom discharge port (21) of the lower tower (2). The gas phase hydrogen and the liquid phase isopropanol and unreacted acetone are separated, and the liquid phase is transported to the recovery tower to recover acetone, and finally a high-purity isopropanol product is obtained. S4: During the process of producing isopropanol in the hydrogenation reactor, the user opens the box door (31), first pre-installs the new catalyst plate (12) on the tilting plate (35), and then replaces the oxygen in the feed box (3). When the hydrogenation reactor is shut down and the new catalyst plate (12) needs to be replaced, the tilting plate (35) is controlled to drive the new catalyst plate (12) into the lower tower body (2) through the feed inlet (22). S5: After the tilting plate (35) enters the lower tower body (2), control the tilting plate (35) to tilt so that the empty groove (351) below the tilting plate (35) faces upward, so that the screw (13) releases the old catalyst plate (12) into the empty groove (351), control the fixing rod (382) to fix the old catalyst plate (12) in the empty groove (351), and then control the tilting plate (35) to rotate so that the tilting plate (35) drives the new catalyst plate (12) to face upward, so that the new catalyst plate (12) is inserted into the screw (13) under the push of the air bag (352), so that the screw (13) drives the new catalyst plate (12) to rise and seal it to the upper tower body (1), thus completing the replacement of the catalyst plate (12).
Citation Information
Patent Citations
Process and device for increasing yield of acetone-hydrogenation isopropanol production
CN103449967A
Preparation method of 1-chloro-3, 3, 3-trifluoropropene
CN111848333A
Device for adding heterogeneous catalyst
CN214346309U