Device for recovering palladium metal in palladium-carbon catalyst of PTA (pure terephthalic acid) device

Abstract

The invention discloses a device for recovering palladium metal in a palladium-carbon catalyst of a PTA (pure terephthalic acid) device, which belongs to the technical field of chemical production and comprises a hydrogenation reactor, the bottom of the hydrogenation reactor is connected with a refining crystallizer through a pipeline, the pipeline is connected with a desalting water pipeline, and the upper part of the hydrogenation reactor is connected with a recovery tank through a pipeline. The recycling tank is connected with a conveying pump through a pipeline, the conveying pump is connected with a plate-and-frame filter press through a pipeline, the bottom of the plate-and-frame filter press is connected with a spiral discharger through a pipeline, the spiral discharger is connected with a drying oven through a pipeline, a stirring device is arranged in the recycling tank, a driving device is arranged on the upper portion of the recycling tank, and the stirring device is connected with the driving device. A flocculant device and a carbon powder device are further arranged on the upper portion of the recycling tank, the driving device is connected with the flocculant device and the carbon powder device, under the condition that stirring is conducted at the same time, a flocculant and carbon powder alternately enter the recycling tank, the alternating time and the discharging amount during alternating are accurately controlled, the flocculation effect is good, and by-products are few.

Description

Technical Field

[0001] The invention relates to the technical field of chemical production, in particular to a device for recovering palladium metal in a palladium-carbon catalyst of a PTA device. Background Art

[0002] PTA, or terephthalic acid, is an organic compound and the largest dicarboxylic acid in production. It is solid at room temperature. It does not melt when heated, but sublimates above 300°C. If heated in a sealed container, it can melt at 427°C. Terephthalic acid is the raw material for producing polyester, especially polyethylene terephthalate (PET).

[0003] In the latest process technology of the PTA unit, the catalyst used in the refined hydrogenation reactor is a palladium-carbon catalyst, with palladium metal as the active component and carbon as the carrier. A total of 67.5 tons of catalyst is used, of which palladium metal accounts for 0.5%. After the hydrogenation reactor is produced, palladium-carbon catalyst remains inside it, and the palladium metal in the palladium-carbon catalyst has a high economic value. When the hydrogenation reactor is backwashed, if the residual palladium-carbon catalyst is directly washed away, the palladium-carbon catalyst will be wasted. Therefore, it is necessary to recover the palladium metal in the palladium-carbon catalyst backwashed out of the hydrogenation reactor. Recovering the palladium metal in the palladium-gold catalyst can reduce the cost of the catalyst in production and provide High resource utilization rate. In the palladium metal recovery process, carbon powder and flocculant need to be put into a recovery tank with a palladium-carbon catalyst solution. The carbon powder and flocculant are mixed with the solution during stirring. The flocculant adsorbs the suspended particles in the solution to make floccules, and the carbon powder mixed therein becomes a reducing agent for subsequent heating. In order to ensure that the flocculant first interacts with the palladium-carbon catalyst solution to reduce by-products and ensure mixing efficiency, the prior art continuously adds flocculants and carbon powder by an alternating method of first adding the flocculant and then adding the carbon powder. However, the prior art cannot control the time and amount of alternating feeding of the flocculant and the carbon powder, which still results in poor flocculation effect and increased by-products. Summary of the invention

[0004] In order to solve the technical problems mentioned in the above background technology, the present invention provides a palladium metal recovery device in a palladium-carbon catalyst of a PTA device, and the technical solution adopted is as follows:

[0005] The invention comprises a hydrogenation reactor, wherein the bottom of the hydrogenation reactor is connected with a refining crystallizer through a pipeline, and the pipeline is connected with a desalted water pipeline, the upper part of the hydrogenation reactor is connected with a recovery tank through a pipeline, the recovery tank is connected with a delivery pump through a pipeline, the delivery pump is connected with a plate and frame filter press through a pipeline, a filtrate pipeline is arranged at the bottom of the plate and frame filter press, the bottom of the plate and frame filter press is connected with a spiral feeder through a pipeline, the spiral feeder is connected with an oven through a pipeline, a stirring device is arranged in the recovery tank, a driving device is arranged on the upper part of the recovery tank, the stirring device is connected with the driving device, a flocculant device and a carbon powder device are also arranged on the upper part of the recovery tank, and the driving device is respectively connected with the flocculant device and the carbon powder device.

[0006] Furthermore, the stirring device includes a stirring rod, on which stirring blades are arranged, and the stirring rod is connected to the driving device.

[0007] Furthermore, the driving device includes a driving member and a lifting member. The driving member includes a motor. A worm is connected to the output shaft of the motor. A first bearing is provided on the worm. The first bearing is fixed on the recovery tank. The worm is connected to the stirring rod, and the worm is connected to the driving member.

[0008] Furthermore, a support plate is provided on the motor, and the support plate is fixed on the recovery tank.

[0009] Furthermore, the lifting member includes a fixed plate, a second bearing is provided on the fixed plate, a worm gear is provided on one side of the fixed plate, the worm gear is meshed with the worm, the axial end of the worm gear passes through the fixed plate and is connected to the second bearing, the axial end of the worm gear is connected to a crank, a first connecting rod is hinged on the crank, a second connecting rod is hinged on the first connecting rod, a rotating shaft is provided on the second connecting rod, one end of the rotating shaft is fixed to the fixed plate, a third connecting rod is hinged on the second connecting rod, a first lifting rod is hinged on the third connecting rod, a first cross beam is provided on the first cross beam, a first rack is provided on the first cross beam, a fourth connecting rod is also hinged on the second connecting rod, a second lifting rod is hinged on the fourth connecting rod, a second cross beam is provided on the second lifting rod, a second rack is provided on the second cross beam, a fixed platform is provided on the fixed plate, a first limiting groove and a second limiting groove are provided on the fixed platform, the first lifting rod passes through the first limiting groove, and the second lifting rod passes through the second limiting groove.

[0010] Furthermore, the flocculant device includes a flocculant tank, a flocculant discharge pipe is arranged at the bottom of the flocculant tank, the flocculant discharge pipe is connected to the recovery tank, a first flap valve is arranged on the flocculant discharge pipe, a first gear is arranged on the valve shaft of the first flap valve, and the first gear is meshed with the first rack.

[0011] Furthermore, the carbon powder device includes a carbon powder canister, a carbon powder discharge pipe is arranged at the bottom of the carbon powder canister, the carbon powder discharge pipe is connected to the recovery tank, a second flap valve is arranged on the carbon powder discharge pipe, a second gear is arranged on the valve shaft of the second flap valve, and the second gear is meshed with the second rack.

[0012] The invention has the following advantages: the material generated in the hydrogenation reactor enters the refining crystallizer through the pipeline, the palladium-carbon catalyst remains in the hydrogenation reactor, the desalted water enters the hydrogenation reactor through the pipeline, the palladium-carbon catalyst in the hydrogenation reactor is backwashed, the backwashed palladium-carbon catalyst solution enters the recovery tank through the pipeline, the driving device drives the stirring device to rotate, and at the same time drives the flocculant device to open, the flocculant in the flocculant device enters the recovery tank, the flocculant device discharges a part of the flocculant and then closes, the driving device drives the carbon powder device to open, the carbon powder in the carbon powder device enters the recovery tank, the carbon powder device discharges a part of the carbon powder and then The flocculant device is closed, and the flocculant device continues to be opened, and at the same time, the stirring device is coordinated to stir, so that the palladium-carbon catalyst solution in the recovery tank produces floccules. After the stirring is completed, the flocculant solution in the recovery tank is sent to the plate and frame filter press through the delivery pump, so that the floccules are partially pressed into cakes, and the filtrate is discharged through the pipeline at the same time. The cake is sent to the oven through a spiral feeder for heating. Under the action of the reducing agent carbon powder in the cake, the carbon in the palladium-carbon catalyst is removed to obtain palladium metal. Under the condition of simultaneous stirring, the flocculant and the carbon powder are alternately fed into the recovery tank, the alternation time and the amount of material discharged during the alternation are accurately controlled, the flocculation effect is good, and the by-products are less. BRIEF DESCRIPTION OF THE DRAWINGS

[0013] Figure 1 It is a schematic diagram of the process of the present invention;

[0014] Figure 2 It is a three-dimensional diagram of the reflux tank of the present invention;

[0015] Figure 3 For the present invention Figure 2 Some screenshots of;

[0016] Figure 4 The driving device of the present invention is three-dimensional Figure 1 ;

[0017] Figure 5 The driving device of the present invention is three-dimensional Figure 2 .

[0018] Figures: 1 hydrogenation reactor, 2 refining crystallizer, 3 recovery tank, 4 delivery pump, 5 plate and frame filter press, 6 screw feeder, 7 oven, 8 stirring rod, 9 stirring blade, 10 motor, 11 worm, 12 first bearing, 13 support plate, 14 fixed plate, 15 second bearing, 16 worm gear, 17 crank, 18 first connecting rod, 19 second connecting rod, 20 rotating shaft, 21 third connecting rod, 22 first lifting rod, 23 first rack, 24 fourth connecting rod, 25 second lifting rod, 26 second rack, 27 fixed platform, 28 first limiting groove, 29 second limiting groove, 30 flocculant tank, 31 flocculant discharge pipe, 32 first flap valve, 33 first gear, 34 carbon powder tank, 35 carbon powder discharge pipe, 36 second flap valve, 37 second gear, 38 first beam, 39 second beam. DETAILED DESCRIPTION

[0019] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0020] Please refer to Figure 1-5 The present invention provides a palladium metal recovery device in a palladium-carbon catalyst of a PTA device, comprising a hydrogenation reactor 1, wherein the bottom of the hydrogenation reactor 1 is connected to a refining crystallizer 2 through a pipeline, and a desalted water pipeline is connected to the pipeline, and the material produced in the hydrogenation reactor 1 is sent to the refining crystallizer 2 through the pipeline for crystallization, and palladium-carbon catalyst remains in the hydrogenation reactor 2, and the desalted water is charged into the hydrogenation reactor 1 through the pipeline to backwash the palladium-carbon catalyst remaining in the hydrogenation reactor 1, and a recovery tank 3 is connected to the upper part of the hydrogenation reactor 1 through a pipeline, and the palladium-carbon catalyst solution obtained by backwashing enters the recovery tank 3 through the pipeline to be recovered, and the recovery tank 3 is connected to a delivery pump 4 through the pipeline, and the delivery pump 4 is connected to a plate-frame filter press 5 through the pipeline, and the flocculant solution produced in the recovery tank 3 passes through the pipeline through the delivery pump 4. Entering into the plate and frame filter press 5, a filtrate pipeline is arranged at the bottom of the plate and frame filter press 5, the flocculant solution is pressed into cake material in the plate and frame filter press 5, and the filtrate is discharged through the pipeline. A spiral feeder 6 is connected to the bottom of the plate and frame filter press 5 through a pipeline, and the spiral feeder 6 is connected to an oven 7 through a pipeline. The cake material is fed into the oven 7 through the spiral feeder 6. Under the heating condition of the oven 7, the carbon powder in the cake material is used as a reducing agent to remove the carbon in the cake material to obtain palladium metal. A stirring device is arranged in the recovery tank 3, and a driving device is arranged on the upper part of the recovery tank 3. The driving device drives the stirring device to rotate, and the stirring device is connected to the driving device. A flocculant device and a carbon powder device are also arranged on the upper part of the recovery tank 3, and the driving device is respectively connected to the flocculant device and the carbon powder device, and the driving device drives the switches of the flocculant device and the carbon powder device respectively.

[0021] The stirring device includes a stirring rod 8, on which a stirring blade 9 is arranged. The stirring rod 8 is connected to a driving device, which drives the stirring rod 8 to rotate, and the stirring rod 8 drives the stirring blade 9 to rotate. The driving device includes a driving member and a lifting member, and the driving member drives the lifting member to lift and lower. The driving member includes a motor 10, and a worm 11 is connected to the output shaft of the motor 10. A first bearing 12 is arranged on the worm 11, and the first bearing 12 is fixed on the recovery tank 3. The motor 10 drives the worm 11 to rotate on the first bearing 12, and the worm 11 is connected to the stirring rod 8, and the worm 11 drives the stirring rod 8 to rotate. The worm 11 is connected to the driving member, and a support plate 13 is arranged on the motor 10, and the support plate 13 is fixed on the recovery tank 3, and the motor 10 is fixed on the recovery tank 3 by the support plate 13.

[0022] The lifting member includes a fixed plate 14, which is fixed on the recovery tank 3. A second bearing 15 is provided on the fixed plate 14. A worm gear 16 is provided on one side of the fixed plate 14. The worm gear 16 is meshed with the worm 11. The shaft end of the worm gear 16 passes through the fixed plate 14 and is connected to the second bearing 15. The worm 11 drives the worm gear 16 to rotate on the second bearing 15. A crank 17 is connected to the shaft end of the worm gear 16. The worm gear 16 drives the crank 17 to rotate. A first connecting rod 18 is hinged on the crank 17. The crank 17 drives the first connecting rod 18 to rotate. The first connecting rod 18 is hinged with a second connecting rod 19, and a rotating shaft 20 is arranged on the second connecting rod 19. One end of the rotating shaft 20 is fixed on the fixed plate 14. The first connecting rod 18 drives the second connecting rod 19 to rotate on the rotating shaft 20 and causes the two ends of the second connecting rod 19 to tilt up and down. The second connecting rod 19 is hinged with a third connecting rod 21, and the second connecting rod 19 drives the third connecting rod 21 to rotate at a certain angle and causes the third connecting rod 21 to move up and down. The third connecting rod 21 is hinged with a first lifting rod 22, and the up and down movement of the third connecting rod 21 drives The first lifting rod 22 moves up and down, and a first crossbeam 38 is arranged on the first lifting rod 22, and a first rack 23 is arranged on the first crossbeam 38. The first lifting rod 22 drives the first crossbeam 38 and the first rack 23 to move up and down. A fourth connecting rod 24 is also hinged on the second connecting rod 19, and the second connecting rod 19 drives the fourth connecting rod 24 to rotate relatively and make the fourth connecting rod 24 move up and down. A second lifting rod 25 is hinged on the fourth connecting rod 24, and a second crossbeam 39 is arranged on the second lifting rod 25. A second rack 23 is arranged on the second crossbeam 39. The fourth connecting rod 24 drives the second lifting rod 25, the second cross beam 39 and the second rack 26 to rise and fall. A fixed platform 27 is provided on the fixed plate 14. The fixed platform 27 is provided with a first limiting groove 28 and a second limiting groove 29. The first lifting rod 22 passes through the first limiting groove 28. The first lifting rod 22 is lifted and lowered in the first limiting groove 28 and limited by the first limiting groove 28. The second lifting rod 25 passes through the second limiting groove 29. The second lifting rod 25 is lifted and lowered in the second limiting groove 29 and limited by the second limiting groove 29.

[0023] The flocculant device includes a flocculant tank 30, which is filled with flocculant. A flocculant discharge pipe 31 is arranged at the bottom of the flocculant tank 30, and the flocculant discharge pipe 31 is connected to the recovery tank 3. The flocculant in the flocculant tank 30 enters the recovery tank 3 through the flocculant discharge pipe 31. A first flap valve 32 is arranged on the flocculant discharge pipe 31 to control the switch of the flocculant discharge pipe 31. A first gear 33 is arranged on the valve shaft of the first flap valve 32, and the first gear 33 is meshed with the first rack 23. The lifting and lowering of the first rack 23 drives the first gear 33 to rotate, and the first gear 33 drives the valve shaft of the first flap valve 32 to rotate, so that the flap in the first flap valve 32 rotates.

[0024] The toner device includes a toner canister 34, which contains toner. A toner discharge pipe 35 is provided at the bottom of the toner canister 34, which is connected to the recovery tank 3. The toner in the toner canister 34 is discharged into the recovery tank 3 through the toner discharge pipe 35. A second flap valve 36 is provided on the toner discharge pipe 35 to control the switch of the toner discharge pipe 35. A second gear 37 is provided on the valve shaft of the second flap valve 36. The second gear 37 is meshed with the second rack 26. The lifting and lowering of the second rack 26 drives the second gear 37 to rotate. The second gear 37 drives the valve shaft of the second flap valve 36 to rotate, so that the flap in the second flap valve 36 rotates.

[0025] The working principle of the present invention is as follows: the material produced in the hydrogenation reactor 1 enters the refining crystallizer 2 through a pipeline, the palladium-carbon catalyst remains in the hydrogenation reactor 1, the desalted water enters the hydrogenation reactor 1 through a pipeline, the palladium-carbon catalyst in the hydrogenation reactor 1 is backwashed, the backwashed palladium-carbon catalyst solution enters the recovery tank 3 through a pipeline, the motor 10 drives the worm 11 to rotate, the worm 11 drives the stirring rod 8 to rotate, the stirring rod 8 drives the stirring blade 9 to rotate, the palladium-carbon catalyst solution in the recovery tank 3 is stirred, the worm 11 drives the worm gear 16 to rotate, the worm gear 16 drives the crank 17 to rotate, and the crank 17 drives the first connecting rod 18 to rotate The first connecting rod 18 drives the second connecting rod 19 to rotate on the rotating shaft 20 and causes the two ends of the second connecting rod 19 to tilt up and down. The second connecting rod 19 drives the third connecting rod 21 to rotate at a certain angle relative to each other and causes the third connecting rod 21 to move up and down. The up and down movement of the third connecting rod 21 drives the first lifting rod 22 to move up and down. The first lifting rod 22 drives the first cross beam 38 and the first rack 23 to move up and down. The second connecting rod 19 drives the fourth connecting rod 24 to rotate relatively and causes the fourth connecting rod 24 to move up and down. The fourth connecting rod 24 drives the second lifting rod 25, the second cross beam 39 and the second rack 26 to move up and down. When the third connecting rod 21 descends, the fourth connecting rod 24 rises. Therefore, when the third connecting rod 21 descends, the first rack 23 descends, the first rack 23 drives the first gear 33 to rotate forward, and the first gear 33 drives the valve shaft of the first flap valve 32 to rotate, so that the flap in the first flap valve 32 rotates, the flocculant discharge pipe 31 opens, and the flocculant in the flocculant tank 30 falls into the recovery tank 3 through the flocculant discharge pipe 31. When the third connecting rod 21 rises, the fourth connecting rod 24 descends. At this time, the first flap valve 32 is closed, and the flocculant stops being discharged. As the fourth connecting rod 24 descends, the second rack 26 also descends, the second rack 26 drives the second gear 37 to rotate, and the second gear 37 drives the second flap valve 3 The valve shaft of 6 rotates, so that the flap in the second flap valve 36 rotates, the carbon powder discharge pipe 35 opens, and the carbon powder in the carbon powder tank 34 enters the recovery tank 3 through the carbon powder discharge pipe 35, so that the flocculant and the carbon powder alternately and continuously enter the recovery tank 3, and the palladium-carbon catalyst solution in the recovery tank 3 produces floccules by stirring. After stirring, the flocculent solution in the recovery tank 3 is sent to the plate and frame filter press 5 through the delivery pump 4, so that the flocculent part is pressed into a cake material, and the filtrate is discharged through the pipeline. The cake material is sent to the oven 7 through the spiral feeder 6 for heating. Under the action of the reducing agent carbon powder in the cake material, the carbon in the palladium-carbon catalyst is removed to obtain palladium metal.

[0026] The present invention is simple to operate, convenient to use, and suitable for comprehensive promotion and application. Although the embodiments of the present invention have been shown and described, it is understood by those skilled in the art that various changes, modifications, substitutions and variations may be made to these embodiments without departing from the principles and spirit of the present invention, and the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A palladium metal recovery device in a palladium-carbon catalyst of a PTA device, comprising a hydrogenation reactor (1), wherein the bottom of the hydrogenation reactor (1) is connected to a refining crystallizer (2) through a pipeline and a desalted water pipeline is connected to the pipeline, the upper part of the hydrogenation reactor (1) is connected to a recovery tank (3) through a pipeline, the recovery tank (3) is connected to a delivery pump (4) through a pipeline, the delivery pump (4) is connected to a plate-frame filter press (5) through a pipeline, a filtrate pipeline is arranged at the bottom of the plate-frame filter press (5), a spiral feeder (6) is connected to the bottom of the plate-frame filter press (5) through a pipeline, and the spiral feeder (6) is connected to an oven (7) through a pipeline, characterized in that: A stirring device is arranged in the recovery tank (3), a driving device is arranged on the upper part of the recovery tank (3), the stirring device is connected to the driving device, a flocculant device and a carbon powder device are also arranged on the upper part of the recovery tank (3), and the driving device is connected to the flocculant device and the carbon powder device respectively.

2. A palladium metal recovery device in a PTA device palladium-carbon catalyst according to claim 1, characterized in that: The stirring device comprises a stirring rod (8), on which a stirring blade (9) is arranged, and the stirring rod (8) is connected to a driving device.

3. A palladium metal recovery device in a PTA device palladium-carbon catalyst according to claim 2, characterized in that: The driving device comprises a driving member and a lifting member, the driving member comprises a motor (10), a worm (11) is connected to the output shaft of the motor (10), a first bearing (12) is arranged on the worm (11), the first bearing (12) is fixed on the recovery tank (3), the worm (11) is connected to the stirring rod (8), and the worm (11) is connected to the driving member.

4. A palladium metal recovery device in a PTA device palladium-carbon catalyst according to claim 3, characterized in that: A support plate (13) is provided on the motor (10), and the support plate (13) is fixed on the recovery tank (3).

5. A palladium metal recovery device in a palladium-carbon catalyst of a PTA device according to claim 3, characterized in that: The lifting member comprises a fixed plate (14), a second bearing (15) is arranged on the fixed plate (14), a worm wheel (16) is arranged on one side of the fixed plate (14), the worm wheel (16) is meshed with the worm (11), the shaft end of the worm wheel (16) passes through the fixed plate (14) and is connected to the second bearing (15), the shaft end of the worm wheel (16) is connected to a crank (17), a first connecting rod (18) is hinged on the crank (17), and the first connecting rod A second connecting rod (19) is hingedly connected to the support plate (18), a rotating shaft (20) is arranged on the second connecting rod (19), one end of the rotating shaft (20) is fixed to the fixed plate (14), a third connecting rod (21) is hingedly connected to the second connecting rod (19), a first lifting rod (22) is hingedly connected to the third connecting rod (21), a first crossbeam (38) is arranged on the first lifting rod (22), and a first rack (23) is arranged on the first crossbeam (38); The second connecting rod (19) is also hinged with a fourth connecting rod (24), the fourth connecting rod (24) is hinged with a second lifting rod (25), the second lifting rod (25) is provided with a second crossbeam (39), and the second crossbeam (39) is provided with a second rack (26); A fixing platform (27) is arranged on the fixing plate (14), a first limiting groove (28) and a second limiting groove (29) are arranged on the fixing platform (27), the first lifting rod (22) passes through the first limiting groove (28), and the second lifting rod (25) passes through the second limiting groove (29).

6. A palladium metal recovery device in a palladium-carbon catalyst of a PTA device according to claim 5, characterized in that: The flocculant device comprises a flocculant tank (30), a flocculant discharge pipe (31) is arranged at the bottom of the flocculant tank (30), the flocculant discharge pipe (31) is connected to the recovery tank (3), a first flap valve (32) is arranged on the flocculant discharge pipe (31), a first gear (33) is arranged on the valve shaft of the first flap valve (32), and the first gear (33) is meshed with the first rack (23).

7. A palladium metal recovery device in a palladium-carbon catalyst of a PTA device according to claim 5, characterized in that: The carbon powder device comprises a carbon powder tank (34), a carbon powder discharge pipe (35) is arranged at the bottom of the carbon powder tank (34), the carbon powder discharge pipe (35) is connected to the recovery tank (3), a second flap valve (36) is arranged on the carbon powder discharge pipe (35), a second gear (37) is arranged on the valve shaft of the second flap valve (36), and the second gear (37) is meshed with the second rack (26).

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