An apparatus and method for producing tetrahydrofuran

By designing a tetrahydrofuran preparation device with automatic catalyst replacement, and utilizing the synergistic operation of the drive and cleaning components, the problems of catalyst failure and caking in fixed-bed reactors were solved, thereby improving production efficiency and reducing costs.

CN115672199BActive Publication Date: 2026-02-13TAICANG HUSHI REAGENT
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Patent Information

Application Number
CN202211352788.3
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2022-10-31
Publication Date
2026-02-13
Estimated Expiration
2042-10-31

AI Technical Summary

Technical Problem

Catalyst failure, caking, and clogging in fixed-bed reactors lead to low production efficiency and increased costs, and uneven catalyst use results in waste.

Method used

A tetrahydrofuran preparation device was designed, which uses a drive component and a cleaning component to realize the automatic replacement and replenishment of catalyst. Through the coordinated work of components such as drive motor, rotating tube, gear and stirring rod, the device automatically cleans up the dead catalyst and replenishes the new catalyst, avoiding downtime.

Benefits of technology

The process enables automatic catalyst replacement and replenishment without downtime, reducing labor, improving production efficiency, lowering production costs, and preventing catalyst residue from affecting the reaction rate.

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Abstract

The application discloses a device and method for preparing tetrahydrofuran, and belongs to the technical field of chemical equipment. The device for preparing tetrahydrofuran comprises a kettle body, a gas outlet pipe and a liquid inlet pipe arranged at the top and bottom of the kettle body respectively, a fixing plate arranged in the kettle body, a reaction tube and a storage hopper arranged at the bottom of the fixing plate, the storage hopper being sleeved outside the reaction tube, a feeding slot being formed in the reaction tube, a partition assembly for plugging the feeding slot being arranged on the storage hopper, a working pipe being communicated with the bottom of the reaction tube, the liquid inlet pipe and the working pipe being interconnected, a cleaning assembly for cleaning the failed catalyst being arranged in the working pipe, a driving assembly for driving the cleaning assembly being arranged on the kettle body, and the driving assembly being connected with the partition assembly. The application can automatically replace the failed catalyst in the reaction kettle, and the production efficiency is greatly improved and the production cost is reduced without stopping the machine during the replacement.
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Description

Technical Field

[0001] This invention relates to the field of chemical equipment technology, and in particular to an apparatus and method for preparing tetrahydrofuran. Background Technology

[0002] Currently, the fixed-bed process remains the most mature and widely used technology in the preparation of tetrahydrofuran. Fixed-bed reactors are a common type of chemical reactor. They consist of a bed of granular solid catalysts or reactants, packed to a certain height. Gases or liquids flow through the static bed between the particles, simultaneously achieving a heterogeneous reaction. A key characteristic of this type of reactor is that the solid particles filling the reactor remain stationary, unlike moving beds and fluidized beds where the solid materials move within the reactor; hence, they are also known as packed-bed reactors.

[0003] In actual use, the catalyst inside a fixed bed gradually becomes ineffective, caking, and blocked, affecting the reaction progress of the materials. This requires staff to stop the machine to replace the catalyst, increasing the workload of the staff. In addition, the catalyst at the front end fails much faster than the catalyst at the back end during actual use. Replacing all the catalysts would also result in a lot of waste and increase production costs. Summary of the Invention

[0004] Purpose of the invention: The first purpose of this invention is to provide a tetrahydrofuran preparation apparatus that can automatically replace the depleted catalyst in the reactor.

[0005] A second objective of the present invention is to provide a method for preparation using the above-described apparatus.

[0006] Technical Solution: The tetrahydrofuran preparation apparatus of the present invention includes a vessel body, with an outlet pipe and a liquid inlet pipe respectively provided at the top and bottom of the vessel body. A fixing plate is provided inside the vessel body, and a reaction tube and a storage hopper are provided at the bottom of the fixing plate. The storage hopper is sleeved on the outside of the reaction tube. A feeding groove is provided on the reaction tube. A partition component for blocking the feeding groove is provided on the storage hopper. A working pipe is connected to the bottom of the reaction tube. The liquid inlet pipe is connected to the working pipe. A cleaning component for cleaning the degraded catalyst is provided inside the working pipe. A driving component for driving the cleaning component is provided on the vessel body, and the driving component is connected to the partition component.

[0007] Preferably, the drive assembly includes a drive motor fixed on the vessel body, the output end of the drive motor is connected to a drive shaft, the end of the drive shaft away from the drive motor passes through the vessel body and is rotatably mounted on the working tube, and an incomplete gear is connected to the drive shaft.

[0008] Preferably, the cleaning assembly includes a rotating tube rotatably mounted on a working tube, a first gear meshing with an incomplete gear on the rotating tube, a sleeve fixedly connected to the outside of the rotating tube, the sleeve being coaxially mounted with the working tube, and uniformly distributed baffles on the sleeve, with a placement groove formed between two adjacent baffles and the inner wall of the working tube.

[0009] Preferably, the working tube has an upper opening, a side opening, and a lower opening. The working tube is connected to the reaction tube through the upper opening. The side opening is connected to the interior of the vessel body and a filter screen is installed inside the side opening. The vessel body is provided with a surrounding plate that cooperates with the lower opening. A waste chamber is formed between the surrounding plate and the inner wall of the vessel body. The vessel body has a discharge port that communicates with the waste chamber.

[0010] Preferably, a fixing rod is fixedly connected to the inner wall of the vessel. The fixing rod is disposed inside the rotating tube and is coaxially arranged with the rotating tube. A protrusion is provided on the outer side of the fixing rod. A sliding rod is slidably connected to the rotating tube. The sliding rod abuts against the protrusion. A connecting plate is provided on the sliding rod. A first elastic element is sleeved on the sliding rod. The two ends of the first elastic element are respectively connected to the rotating tube and the connecting plate. A rubber ball is connected to the end of the sliding rod away from the protrusion. The rubber ball abuts against the sleeve.

[0011] Preferably, a reflux pipe is connected to the bottom of the vessel body, a pump body is installed on the reflux pipe, and the end of the reflux pipe away from the vessel body is connected to the liquid inlet pipe.

[0012] Preferably, the partition assembly includes a partition plate slidably disposed between the reaction tube and the storage hopper, a movable plate connected to the bottom of the partition plate, a connecting plate disposed on the storage hopper, a second elastic element disposed between the connecting plate and the movable plate, the partition assembly further includes a rack plate connected to the movable plate, the rack plate meshing with an incomplete gear, a first support plate disposed on the reaction tube, and the rack plate slidably connected to the first support plate.

[0013] Preferably, a stirring rod is rotatably mounted on the vessel body, and the stirring rod is provided with uniformly distributed stirring blades, which are movably mounted inside the reaction tube.

[0014] Preferably, a second support plate is fixed on the vessel body, a transmission rod is rotatably mounted on the second support plate, a synchronous pulley is mounted on both the transmission rod and the stirring rod, a belt is mounted between the two synchronous pulleys, a driven bevel gear is mounted on the transmission rod, a rotating rod is rotatably mounted on the vessel body, a driving bevel gear is mounted on the rotating rod and meshes with the driven bevel gear, and a second gear is mounted on the end of the rotating rod away from the driving bevel gear and meshes with an incomplete gear.

[0015] The present invention provides a method for preparing tetrahydrofuran using the above-mentioned apparatus, comprising the following steps:

[0016] (1) Add catalyst to the storage hopper and reaction tube, and the height of the catalyst in the reaction tube shall not exceed the feed tank;

[0017] (2) Introduce preheated 1,4-butanediol into the inlet pipe at the bottom of the reactor body, and control the amount of catalyst in the reaction tube to be 2-3% of the mass of 1,4-butanediol in the reactor body, so that 1,4-butanediol and catalyst can be fully contacted in the reaction tube.

[0018] (3) During the reaction between the material and the catalyst, the drive component intermittently drives the isolation component and the cleaning component to automatically replace the failed catalyst.

[0019] (4) Control the reaction temperature inside the reactor to 100-150℃ so that the water and tetrahydrofuran obtained from the reaction are discharged from the top of the reactor in gaseous form through the gas outlet pipe.

[0020] (5) Water and tetrahydrofuran in gaseous form are fed to a distillation column. The temperature of the rectification section of the distillation column is controlled at 60-64℃ and the temperature of the stripping section is controlled at 90-95℃. Water and tetrahydrofuran are separated. Water is discharged from the wastewater outlet of the distillation column bottom and sent to the environmental protection treatment unit for treatment and reuse in the production system. The obtained tetrahydrofuran is discharged from the outlet at the top of the distillation column to the subsequent refining unit for treatment to obtain tetrahydrofuran.

[0021] Beneficial effects: Compared with the prior art, the significant advantages of the present invention are:

[0022] 1. The device for preparing tetrahydrofuran uses a drive component to drive a cleaning component and a partition component to work together to replace the dead catalyst in the reaction tube and replenish the new catalyst. No shutdown is required during the material replacement process, which reduces the workload of the staff, greatly improves production efficiency and reduces production costs.

[0023] 2. The apparatus for preparing tetrahydrofuran uses a sliding rod on a rotating tube to abut against a protrusion on a fixed rod during rotation. This causes the sliding rod to intermittently abut against the sleeve, thereby effectively discharging the spent catalyst in the placement tank outside the sleeve into the waste chamber. This prevents the placement tank from containing residual spent catalyst, which could affect the reaction rate of the catalyst in the subsequent reaction tube.

[0024] 3. The apparatus for preparing tetrahydrofuran uses a cleaning component and a partition component working together to replace the dead catalyst in the reaction tube and replenish the new catalyst. After the incomplete gear meshes with the second gear, the second gear drives the driving bevel gear on the rotating rod to mesh with the driven bevel gear on the transmission rod. This causes the stirring rod to rotate with the transmission rod under the action of the synchronous pulley and belt. The stirring rod drives the stirring blades to stir the catalyst in the reaction tube. This disturbs the catalyst in the reaction tube and allows it to fall naturally into the new placement tank under the action of gravity, avoiding the catalyst from being unable to fall due to local caking or sticking to the reaction tube. Attached Figure Description

[0025] Figure 1 This is a schematic diagram of the structure of the present invention;

[0026] Figure 2 For the present invention Figure 1 Enlarged view of part A in the middle;

[0027] Figure 3 This is a cross-sectional structural diagram of the present invention;

[0028] Figure 4 For the present invention Figure 2 Enlarged view of part B in the middle;

[0029] Figure 5 This is a schematic cross-sectional view of the working tube of the present invention;

[0030] Figure 6 This is a schematic diagram of the structure of the driving component of the present invention;

[0031] Figure 7 For the present invention Figure 6 Enlarged view of part C in the middle.

[0032] In the diagram: 1. Kettle body; 101. Gas outlet pipe; 102. Liquid inlet pipe; 103. Discharge port; 2. Fixing plate; 3. Reaction tube; 301. Feeding trough; 4. Storage hopper; 401. Connecting plate; 5. Working tube; 501. Top opening; 502. Side opening; 5021. Filter screen; 503. Bottom opening; 5031. Enclosure plate; 6. Drive motor; 601. Drive shaft; 602. Incomplete gear; 7. Rotating tube; 701. First gear; 702. Sleeve; 7021. Baffle; 8. Fixed... Fixed rod; 801, protrusion; 9, slide rod; 901, connecting plate; 902, first elastic element; 903, rubber ball; 10, return pipe; 1001, pump body; 11, partition plate; 111, moving plate; 112, second elastic element; 113, rack plate; 12, first support plate; 13, stirring rod; 131, stirring blade; 14, second support plate; 15, transmission rod; 151, driven bevel gear; 16, synchronous pulley; 17, rotating rod; 171, driving bevel gear; 172, second gear. Detailed Implementation

[0033] The technical solution of the present invention will be further described in detail below with reference to the accompanying drawings. It should be noted that the raw materials used in the preparation of tetrahydrofuran in the present invention are all well-known and commonly used in the field, and can all be purchased from the market.

[0034] Reference Figure 1 , Figure 3 , Figure 4 , Figure 5 and Figure 6 The apparatus for preparing tetrahydrofuran of the present invention includes a vessel body 1. A gas outlet pipe 101 and a liquid inlet pipe 102 are respectively provided at the top and bottom of the vessel body 1. A fixing plate 2 is provided inside the vessel body 1. A reaction tube 3 and a storage hopper 4 are provided at the bottom of the fixing plate 2. The storage hopper 4 is sleeved on the outside of the reaction tube 3. A feeding groove 301 is opened on the reaction tube 3. A partition component for blocking the feeding groove 301 is provided on the storage hopper 4. A working pipe 5 is connected to the bottom of the reaction tube 3. The liquid inlet pipe 102 is connected to the working pipe 5. A cleaning component for cleaning the depleted catalyst is provided inside the working pipe 5. A driving component for driving the cleaning component is provided on the vessel body 1, and the driving component is connected to the partition component.

[0035] Specifically, preheated 1,4-butanediol is introduced through the inlet pipe 102 at the bottom of the reactor body 1. The amount of catalyst in the reaction tube 3 is controlled to be 2-3% of the mass of 1,4-butanediol in the reactor, so that 1,4-butanediol and catalyst can fully contact each other in the reaction tube 3. The water and tetrahydrofuran produced by the reaction are discharged in gaseous form from the top of the reactor through the outlet pipe 101. During this process, the cleaning component and the isolation component are driven by the drive component to work together. The cleaning component removes the failed catalyst in the working tube 5, and the catalyst in the storage hopper 4 enters the reaction tube 3 through the replenishment tank 301 to replenish it. This realizes the replacement of the failed catalyst in the reaction tube 3 and the replenishment of new catalyst. There is no need to stop the machine during the material replacement process, which reduces the workload of the staff, greatly improves the production efficiency and reduces the production cost.

[0036] Reference Figure 1 , Figure 2 and Figure 7 The drive assembly includes a drive motor 6 fixed on the vessel body 1. The output end of the drive motor 6 is connected to a drive shaft 601. The end of the drive shaft 601 away from the drive motor 6 passes through the vessel body 1 and is rotatably mounted on the working tube 5. An incomplete gear 602 is connected to the drive shaft 601. Specifically, by controlling the operation of the drive motor 6, the output end of the drive motor 6 drives the incomplete gear 602 to rotate through the drive shaft 601.

[0037] Reference Figure 1 , Figure 3 , Figure 5 and Figure 7 The cleaning assembly includes a rotating tube 7 rotatably mounted on the working tube 5. The rotating tube 7 is provided with a first gear 701 that meshes with the incomplete gear 602. A sleeve 702 is fixedly connected to the outside of the rotating tube 7. The sleeve 702 is coaxially mounted with the working tube 5. The sleeve 702 is provided with evenly distributed baffles 7021. A placement groove is formed between two adjacent baffles 7021 and the inner wall of the working tube 5.

[0038] Furthermore, the working tube 5 is provided with an upper opening 501, a side opening 502 and a lower opening 503. The working tube 5 is connected to the reaction tube 3 through the upper opening 501. The side opening 502 is connected to the interior of the vessel body 1. A filter screen 5021 is provided in the side opening 502. A surrounding plate 5031 that cooperates with the lower opening 503 is provided in the vessel body 1. A waste chamber is formed between the surrounding plate 5031 and the inner wall of the vessel body 1. A discharge port 103 that communicates with the waste chamber is provided on the vessel body 1.

[0039] Specifically, the material entering the working tube 5 from the inlet pipe 102 first reacts with the catalyst in the placement tank connected to the reaction tube 3. The catalyst in the placement tank will be deactivated first. When the drive shaft 601 drives the incomplete gear 602 to rotate, the incomplete gear 602 meshes with the first gear 701. The first gear 701 drives the rotating tube 7 to rotate, and the rotating tube 7 drives the sleeve 702 to rotate in the working tube 5. This causes the deactivated catalyst in the placement tank connected to the reaction tube 3 to rotate with the sleeve 702. During the rotation, it passes through the side opening 502. At this time, the liquid reactant contained in the deactivated catalyst will pass through the filter screen 5021 and enter the vessel body 1. As the rotating tube 7 continues to rotate, the deactivated catalyst moves with the sleeve 702 to the lower opening 503. The catalyst enters the waste chamber under its own weight and can be cleaned out of the vessel body 1 through the discharge port 103.

[0040] Reference Figure 3 and Figure 5 A fixing rod 8 is fixedly connected to the inner wall of the vessel body 1. The fixing rod 8 is set inside the rotating tube 7 and is coaxial with the rotating tube 7. A protrusion 801 is set on the outer side of the fixing rod 8. A sliding rod 9 is slidably connected to the rotating tube 7. The sliding rod 9 and the protrusion 801 are movably abutted against each other. A connecting plate 901 is set on the sliding rod 9. A first elastic element 902 is sleeved on the sliding rod 9. The two ends of the first elastic element 902 are respectively connected to the rotating tube 7 and the connecting plate 901. A rubber ball 903 is connected to the end of the sliding rod 9 away from the protrusion 801. The rubber ball 903 is movably abutted against the sleeve 702.

[0041] Specifically, during the rotation of the rotating tube 7, the sliding rod 9 sliding on it abuts against the protrusion 801 on the fixed rod 8, causing the sliding rod 9 to drive the rubber ball 903 to intermittently abut against the sleeve 702, causing the sleeve 702 to vibrate. This facilitates the separation of the degraded catalyst from the placement tank, preventing it from sticking inside the placement tank. This allows the degraded catalyst in the placement tank outside the sleeve 702 to be effectively discharged into the waste chamber, preventing the placement tank from containing residual degraded catalyst, which would affect the amount of catalyst added by the subsequent reaction tube 3 entering the placement tank and reduce the reaction rate of the catalyst in the reactor 1.

[0042] Reference Figure 1 and Figure 5 The bottom of the vessel body 1 is connected to a reflux pipe 10, and a pump body 1001 is installed on the reflux pipe 10. The end of the reflux pipe 10 away from the vessel body 1 is connected to the liquid inlet pipe 102. Specifically, the material solution that enters the vessel body 1 through the filter screen 5021 on the working pipe 5 can be returned to the liquid inlet pipe 102 through the reflux pipe 10 under the action of the pump body 1001, and then re-enter the vessel body 1 through the liquid inlet pipe 102 to react with the catalyst, so as to reasonably recover and reuse the material.

[0043] Reference Figure 1 , Figure 3 , Figure 4 , Figure 6 and Figure 7 The partition assembly includes a partition plate 11 slidably disposed between the reaction tube 3 and the storage hopper 4. A movable plate 111 is connected to the bottom of the partition plate 11. A connecting plate 401 is disposed on the storage hopper 4. A second elastic element 112 is disposed between the connecting plate 401 and the movable plate 111. The partition assembly also includes a rack plate 113 connected to the movable plate 111. The rack plate 113 is meshed with an incomplete gear 602. A first support plate 12 is disposed on the reaction tube 3. The rack plate 113 is slidably connected to the first support plate 12.

[0044] Specifically, when the drive shaft 601 drives the incomplete gear 602 to rotate, it will mesh with the rack plate 113, causing the rack plate 113 to move up and down on the first support plate 12. The movement of the rack plate 113 causes the moving plate 111 and the partition plate 11 to move down, so that the partition plate 11 no longer blocks the feeding trough 301. At this time, the catalyst in the storage hopper 4 will enter the reaction tube 3 from the feeding trough 301. Subsequently, when the incomplete gear 602 no longer meshes with the rack plate 113, the moving plate 111 is reset under the elastic force of the second elastic element 112, so that the partition plate 11 blocks the feeding trough 301 again, avoiding the presence of too much catalyst in the reaction tube 3, which would affect the upward flow speed of the generated gas and thus affect the production efficiency of the product.

[0045] Reference Figure 1 , Figure 2 , Figure 3 and Figure 7 A stirring rod 13 is rotatably mounted on the vessel body 1, and stirring blades 131 are evenly distributed on the stirring rod 13. The stirring blades 131 are movably mounted inside the reaction tube 3.

[0046] Furthermore, a second support plate 14 is fixedly provided on the vessel body 1, and a transmission rod 15 is rotatably provided on the second support plate 14. Both the transmission rod 15 and the stirring rod 13 are provided with synchronous pulleys 16, and a belt is provided between the two synchronous pulleys 16. A driven bevel gear 151 is provided on the transmission rod 15, and a rotating rod 17 is rotatably provided on the vessel body 1. A driving bevel gear 171 is provided on the rotating rod 17 and meshes with the driven bevel gear 151. A second gear 172 is provided at the end of the rotating rod 17 away from the driving bevel gear 171 and meshes with the incomplete gear 602.

[0047] Specifically, through the coordinated operation of the cleaning and isolation components, the replacement of the failed catalyst in the reaction tube 3 and the replenishment of the new catalyst are achieved. Then, the incomplete gear 602 meshes with the second gear 172, causing the second gear 172 to drive the active bevel gear 171 on the rotating rod 17 to mesh with the driven bevel gear 151 on the transmission rod 15. This causes the stirring rod 13 to rotate with the transmission rod 15 under the action of the synchronous pulley 16 and the belt. The stirring rod 13 drives the stirring blades 131 to stir the catalyst in the reaction tube 3. This can disturb the catalyst in the reaction tube 3, break up the locally hardened and adhered catalyst, and allow it to fall naturally into the new placement tank under the action of gravity, thus preventing the catalyst in the reaction tube 3 from being unable to fall due to local hardening or adhesion to the reaction tube 3.

[0048] Working principle: Preheated 1,4-butanediol is introduced through the inlet pipe 102 at the bottom of the reactor body 1. The amount of catalyst in the reaction tube 3 is controlled to be 2-3% of the mass of 1,4-butanediol in the reactor, so that the 1,4-butanediol and the catalyst are in full contact in the reaction tube 3. The material entering the working tube 5 from the inlet pipe 102 reacts first with the catalyst in the placement tank connected to the reaction tube 3. The catalyst in the placement tank will be deactivated first. The water and tetrahydrofuran obtained from the reaction are discharged in gaseous form from the top of the reactor through the vent pipe 101. During this process, the drive motor 6 is controlled to run, so that the output end of the drive motor 6 drives the incomplete gear 602 to rotate through the drive shaft 601. When the incomplete gear 602 rotates, it meshes with the rack plate 113, causing the rack plate 113 to move up and down on the first support plate 12. The movement of the rack plate 113 drives the moving plate 111 and the partition plate 11 to move down, so that the partition plate 11 no longer blocks the feeding trough 301. At this time, the catalyst in the storage hopper 4 will enter the reaction tube 3 from the feeding trough 301. Subsequently, when the incomplete gear 602 no longer meshes with the rack plate 113, the moving plate 111 resets under the elastic force of the second elastic element 112, causing the partition plate 11 to block the feeding trough 301 again, preventing the presence of too much catalyst in the reaction tube 3, which would affect the upward flow rate of the generated gas and thus affect production efficiency. When gear 602 meshes with the first gear 701, the first gear 701 drives the rotating tube 7 to rotate, and the rotating tube 7 drives the sleeve 702 to rotate inside the working tube 5. This causes the spent catalyst in the placement tank connected to the reaction tube 3 to rotate with the sleeve 702. During rotation, the catalyst passes through the side opening 502, and the liquid reactants contained in the spent catalyst pass through the filter screen 5021 and enter the reactor body 1. As the rotating tube 7 continues to rotate, the spent catalyst moves with the sleeve 702 to the lower opening 503. Under its own weight, the catalyst enters the waste chamber and can be removed from the reactor body 1 through the discharge port 103. This achieves the cleaning of the spent catalyst in the reaction tube 3. After the catalyst replacement and replenishment, the incomplete gear 602 meshes with the second gear 172, causing the second gear 172 to drive the driving bevel gear 171 on the rotating rod 17 to mesh with the driven bevel gear 151 on the transmission rod 15. This causes the stirring rod 13 to rotate with the transmission rod 15 under the action of the synchronous pulley 16 and the belt. The stirring rod 13 drives the stirring blades 131 to stir the catalyst in the reaction tube 3. This can disturb the catalyst in the reaction tube 3, break up the locally hardened and adhered catalyst, and allow it to fall naturally into the new placement tank under the action of gravity, thus preventing the catalyst in the reaction tube 3 from being unable to fall due to local hardening or adhesion to the reaction tube 3.

[0049] The method for preparing tetrahydrofuran using the above-described apparatus according to the present invention includes the following steps:

[0050] S1: Add strong acid ion exchange resin particle catalyst to the storage hopper 4 and the reaction tube 3, and the height of the catalyst in the reaction tube 3 shall not exceed the feeding tank 301.

[0051] S2: 1,4-Butanediol that has been preheated is introduced into the inlet pipe 102 at the bottom of the vessel 1. The amount of catalyst in the reaction tube 3 is controlled to be 2-3% of the mass of 1,4-butanediol in the vessel, so that 1,4-butanediol and catalyst are in full contact in the reaction tube 3.

[0052] S3: During the reaction between the material and the catalyst, the drive component intermittently drives the isolation component and the cleaning component to automatically replace the failed catalyst.

[0053] S4: Control the reaction temperature inside the reactor 1 to 100-150℃, so that the water and tetrahydrofuran obtained from the reaction are discharged from the top of the reactor in gaseous form through the gas outlet pipe 101.

[0054] S5: Gaseous water and tetrahydrofuran are fed to a distillation column. The temperature of the rectification section of the distillation column is controlled at 60-64℃, and the temperature of the stripping section is controlled at 90-95℃. The water and tetrahydrofuran are separated. The water is discharged from the wastewater outlet of the distillation column bottom and sent to the environmental protection treatment unit for treatment and reuse in the production system. The resulting tetrahydrofuran is discharged from the outlet at the top of the distillation column and sent to the subsequent refining unit for further treatment to obtain tetrahydrofuran.

Claims

1. An apparatus for producing tetrahydrofuran comprising a kettle body (1), characterized in that: The top and bottom of the kettle body (1) are respectively provided with an air outlet pipe (101) and a liquid inlet pipe (102), the kettle body (1) is provided with a fixed plate (2), the bottom of the fixed plate (2) is provided with a reaction tube (3) and a storage hopper (4), the storage hopper (4) is sleeved outside the reaction tube (3), the reaction tube (3) is provided with a feeding slot (301), the storage hopper (4) is provided with a partition assembly for blocking the feeding slot (301), the bottom of the reaction tube (3) is communicated with a working pipe (5), the liquid inlet pipe (102) and the working pipe (5) are communicated with each other, the working pipe (5) is provided with a cleaning assembly for cleaning the invalid catalyst, the kettle body (1) is provided with a driving assembly for driving the cleaning assembly, and the driving assembly is connected with the partition assembly; The driving assembly comprises a driving motor (6) fixed on the kettle body (1), the output end of the driving motor (6) is connected with a driving shaft (601), one end of the driving shaft (601) away from the driving motor (6) penetrates through the kettle body (1) and is rotationally arranged on the working pipe (5), and the driving shaft (601) is connected with an incomplete gear (602); The cleaning assembly comprises a rotating pipe (7) rotationally arranged on the working pipe (5), the rotating pipe (7) is provided with a first gear (701) meshedly connected with the incomplete gear (602), the outer side of the rotating pipe (7) is fixedly connected with a sleeve pipe (702), the sleeve pipe (702) is coaxially arranged with the working pipe (5), the sleeve pipe (702) is provided with uniformly distributed baffles (7021), and adjacent two baffles (7021) and the inner wall of the working pipe (5) form a placing groove therebetween; The working pipe (5) is provided with an upper opening (501), a side opening (502) and a lower opening (503), the working pipe (5) is communicated with the reaction tube (3) through the upper opening (501), the side opening (502) is communicated with the inside of the kettle body (1), the side opening (502) is provided with a filter screen (5021), the kettle body (1) is provided with a surrounding plate (5031) matched with the lower opening (503), the surrounding plate (5031) and the inner wall of the kettle body (1) form a waste chamber therebetween, and the kettle body (1) is provided with a discharge port (103) communicated with the waste chamber; The inner wall of the kettle body (1) is fixedly connected with a fixed rod (8), the fixed rod (8) is arranged in the rotating pipe (7) and coaxially arranged with the rotating pipe (7), the outer side of the fixed rod (8) is provided with a protruding block (801), the rotating pipe (7) is slidably connected with a sliding rod (9), the sliding rod (9) is movably abutted with the protruding block (801), the sliding rod (9) is provided with a connecting plate (901), the sliding rod (9) is sleeved with a first elastic element (902), the two ends of the first elastic element (902) are connected with the rotating pipe (7) and the connecting plate (901) respectively, one end of the sliding rod (9) away from the protruding block (801) is connected with a rubber ball (903), and the rubber ball (903) is movably abutted with the sleeve pipe (702).

2. The apparatus for producing tetrahydrofuran according to claim 1, characterized by: The bottom of the kettle body (1) is connected with a reflux pipe (10), the reflux pipe (10) is provided with a pump body (1001), and the end, away from the kettle body (1), of the reflux pipe (10) is connected with a liquid inlet pipe (102).

3. The apparatus for producing tetrahydrofuran according to claim 1, wherein: The partition assembly comprises a partition plate (11) slidingly arranged between the reaction tube (3) and the storage hopper (4), the bottom of the partition plate (11) is connected with a moving plate (111), the storage hopper (4) is provided with a connecting plate (401), the second elastic element (112) is arranged between the connecting plate (401) and the moving plate (111), the partition assembly further comprises a rack plate (113) connected with the moving plate (111), the rack plate (113) is in meshing connection with the incomplete gear (602), and the reaction tube (3) is provided with a first supporting plate (12), the rack plate (113) is slidingly connected on the first supporting plate (12).

4. The apparatus for producing tetrahydrofuran according to claim 2, wherein: The kettle body (1) is further provided with a stirring rod (13) rotatably arranged thereon, the stirring rod (13) is provided with stirring blades (131) uniformly distributed thereon, and the stirring blades (131) are movably arranged in the reaction tube (3).

5. The apparatus for producing tetrahydrofuran according to claim 4, wherein: The kettle body (1) is further provided with a second supporting plate (14) fixedly arranged thereon, the second supporting plate (14) is rotatably provided with a transmission rod (15), the transmission rod (15) and the stirring rod (13) are both provided with synchronous wheels (16), a belt is arranged between the two synchronous wheels (16), the transmission rod (15) is provided with a driven bevel gear (151), the kettle body (1) is rotatably provided with a rotating rod (17), the rotating rod (17) is provided with a driving bevel gear (171) in meshing connection with the driven bevel gear (151), and the end, away from the driving bevel gear (171), of the rotating rod (17) is provided with a second gear (172) in meshing connection with the incomplete gear (602).

6. A process for the production of tetrahydrofuran using the apparatus of claim 1, characterized in that: The method comprises the following steps: (1) adding catalysts into the storage hopper (4) and the reaction tube (3), and the height of the catalysts in the reaction tube (3) does not exceed the height of the feeding groove (301); (2) inputting preheated 1,4-butanediol from the liquid inlet pipe (102) at the bottom of the kettle body (1), controlling the catalyst dosage in the reaction tube (3) to be 2-3% of the mass of the 1,4-butanediol in the kettle, and making the 1,4-butanediol and the catalyst fully contact in the reaction tube (3); (3) during the reaction of the material and the catalyst, the driving assembly intermittently drives the partition assembly to cooperate with the material cleaning assembly to automatically replace the invalid catalysts; (4) controlling the reaction temperature in the kettle body (1) to be 100-150°C, making the water and the tetrahydrofuran obtained by the reaction be discharged from the gas outlet pipe (101) at the top of the reaction kettle in a gaseous form; (5) transporting the water and the tetrahydrofuran in a gaseous form to a rectifying tower, controlling the temperature of the rectifying section of the rectifying tower to be 60-64°C and the temperature of the distillation section to be 90-95°C, separating the water and the tetrahydrofuran, discharging the water from the wastewater outlet of the tower kettle of the rectifying tower to be sent into an environmental protection treatment unit, treating the water after treatment, and recycling the water into a production system, and discharging the obtained tetrahydrofuran from the outlet at the top of the rectifying tower to a subsequent refining unit for treatment to obtain tetrahydrofuran.

Citation Information

Patent Citations

  • Device for preparing tetrahydrofuran and method thereof

    CN111318236A