JP2013049029A - Catalyst separation apparatus - Google Patents

Abstract

PROBLEM TO BE SOLVED: To eliminate a useless space inside a reactor and to separate and discharge liquid and a catalyst remaining after completion of reaction.SOLUTION: A raw material gas 28 is supplied from a delivery port of a gas distributor 30 into the reactor 21 of a generally cylindrical shape. A reacting liquid 24, the raw material gas and the catalyst 25 are made to flow vertically and react with each other inside the reactor. A catalyst separation apparatus 22 is provided with a partition plate 35 having an opening of a cylindrical wall 36 in the center on the lower side of the gas distributor 30. A riser tube 39 is inserted to the inside of the cylindrical wall 36 and an ascending flow is generated by the gas. A small hole 43 is arranged on the outer periphery side of the partition plate 35, and a down tube 44 is inserted therethrough and is placed alonside a recessed curved surface of the lower end part of the reactor. The upper end of the down tube 44 is protruded upward of the partition plate and is surrounded by a roof section 45. Catalyst separation filters 47 and discharge pipes 48 are arranged below the partition plate. The partition plate, the down tube and the riser tube form a circulation passage for slurry, the slurry discharged from a lower end outlet of the down tube is raised in a stagnation space, and product liquid is separated by the catalyst separation filters.

Description

  The present invention relates to a catalyst separation device for separating a catalyst from a reactive liquid.

Conventionally, in a catalytic reaction apparatus that uses a catalyst to react liquid and gas in a reactor to produce liquid or gas as a product, for example, the catalyst is separated from the product liquid remaining in the reactor after the reaction is completed. There is known a catalyst separation apparatus that is adapted to be removed.
An example of such a catalyst separation device is described in Patent Document 1. This catalyst separation apparatus will be described with reference to FIG.
In the catalyst separation apparatus 1 shown in FIG. 5, the reaction liquid 3 is accumulated up to the vicinity of the upper part in a substantially cylindrical and capsule-shaped reactor 2 having a high pressure resistance, and a liquid surface is formed. For example, finely divided catalyst 4 is dispersed to form a slurry. A supply pipe 7 for supplying the raw material gas 6 is inserted into the substantially hemispherical lower end portion of the reactor 2, and the supply pipe 7 is connected to a gas distributor 8 for the raw material gas 6.

A plurality of nozzles are formed downward in the gas distributor 8 at predetermined intervals, and the raw material gas 6 is discharged as bubbles. Formed in the upper part of the gas distributor 6 is a bubbling flow consisting of bubbles of the raw material gas 6 and further a slurry bed 9 which flows in a gas-liquid solid three phase to which a liquid and a particulate catalyst are added.
In the reactor 2, a plurality of catalyst separation filters 10 for separating the catalyst 4 from the product solution after the reaction are arranged near the liquid surface of the reaction solution 3 as a filter, and the catalyst separation filter 10 passes through the discharge pipe 11. The product liquid from which the catalyst 4 has been separated is discharged to the outside. In the slurry bed 9, cooling pipes 12 for circulating cooling water are arranged in the lower part of the catalyst separation filter 10 as vertical pipe groups.

Then, the raw material gas 6 is discharged as bubbles from the gas distributor 8 and raised, thereby causing the slurry containing the reaction liquid 3 to flow upward. Then, the slurry is appropriately cooled by the cooling pipe 12 to promote the reaction of the reaction liquid 3, the raw material gas 6, and the catalyst 4 to generate a product liquid.
In the slurry bed 9, an upward flow of the slurry containing the reaction liquid 3 and the catalyst 4 is generated in the central region in the reactor 2 by the upward flow of the bubbles of the raw material gas 6 discharged from the gas reactor 8, and the liquid It is reversed to the outside near the surface and becomes a downward flow in the outside region. Furthermore, it is converted again into an upward flow in the central region by the bubble flow of the gas distributor 8.

  The product liquid and the catalyst 4 are separated by the catalyst separation filter 10 provided near the liquid surface in the reactor 2, the catalyst 4 is captured by the catalyst separation filter 10, and the product liquid is discharged together with a part of the unreacted liquid 3. It is taken out from the tube 11 to the outside. Also, the product gas after the reaction is caused to flow upward from the liquid surface together with a part of the unreacted raw material gas 6, and is discharged from the upper end of the reactor 2 to the outside through the gas discharge pipe.

Special table 2007-516065 gazette

By the way, since the catalyst separation apparatus 1 described above has the vertical cylindrical reactor 2, the bottom end has a concave curved surface structure such as an end plate for pressure resistance, and on the other hand, it is disposed immediately above. The gas distributor 8 usually has a structure in which a plurality of nozzles are arranged in the horizontal direction at the same level, so that the bubbles of the raw material gas float above and contribute to the reaction. As a result, the lower region derived from the concave curved shape on the lower side of the gas distributor 8 becomes a useless space as a volume for reaction.
Further, since the catalyst separation filter 10 as a filter for separating the catalyst and the product liquid is provided in the upper part of the slurry bed 9 where the reaction liquid 3, the raw material gas 6 and the catalyst 4 react, the installation of the catalyst separation filter 10 is performed. In the region, the raw material gas 6 remains. Therefore, the reaction by the raw material gas 6 continues, and the dense cake layer that is generated and adhered to the catalyst separation filter 10 contains the unreacted reaction solution 3 and the catalyst 4, so that the reaction is more efficient than the slurry bed 9. Will wake up. For example, in the case of an exothermic reaction, the cake layer and the catalyst separation filter 10 described above are heated to a high temperature and clogged due to catalyst sintering, filter burn-in, and the like. Further, the catalyst separation filter 10 may adversely affect the flow of the entire reactor 2 due to the flow resistance of the filter.

In addition, the catalyst separation filter 10 that is a filter is originally installed for the purpose of extracting the product liquid, but the raw material gas accompanies the product liquid due to the presence of the raw material gas, and the catalyst separation filter 10 is related to the magnitude of the filtration resistance. As a result, the source gas preferentially flows out of the discharge pipe 11. As a result, it is necessary to install a gas-liquid separation device in the wake region, which is the upper part in the reactor 2, and there is a disadvantage that the device configuration becomes complicated.
Moreover, in the reactor 2, the product liquid and the catalyst 4 remain after the reaction of the reaction liquid 3, the raw material gas 6, and the catalyst 4 is stopped, and these product liquid and the catalyst 4 are discharged to the outside of the reactor 2. In this case, the product liquid up to the installation height of the catalyst separation filter 10 and the catalyst 4 can be extracted, but the product liquid remaining below and the catalyst 4 remaining liquid can be discharged using the catalyst separation filter 10. There was a problem that the catalyst could not be separated and was discharged without being separated.

  The present invention has been made in view of such circumstances, eliminates a useless space in the reactor, and can efficiently separate and discharge the liquid and catalyst remaining in the reactor after the reaction is completed. An object is to provide a catalyst separation device.

The catalyst separation apparatus according to the present invention supplies a raw material gas to a substantially cylindrical reactor, and reacts the liquid, the raw material gas and the catalyst using the catalyst in the reactor to obtain a product liquid. In the reactor, a gas distributor for supplying the raw material gas is provided, a partition plate having an opening for flowing the product liquid and the catalyst is provided below the gas distributor, and a catalyst separation filter and a discharge are provided below the partition plate. A tube is provided.
According to the present invention, a gas-liquid solid-phase three-phase slurry of liquid, raw material gas, and catalyst is generated by discharging the raw material gas bubbles from the gas distributor in the reactor to form a bubble flow upward. The raw material gas is separated by a downward flow toward the partition plate, and when the product liquid and the catalyst pass through the opening of the partition plate and flow down along the lower end of the reactor, The product liquid and the catalyst are separated in advance by gravity sedimentation and then separated from the catalyst by the catalyst separation filter when rising at a low speed toward the catalyst separation filter arranged upside down at the bottom and arranged below the partition plate. The liquid is discharged to the outside through the discharge pipe.

Moreover, it is preferable that the opening of a partition plate has the 1st opening which raises a catalyst and a production | generation liquid, and the 2nd opening which drops a catalyst and a production | generation liquid.
On the partition plate and the lower side thereof, a circulating flow of the product liquid and the catalyst is generated by the partition plate, the first opening, the second opening, and the bottom surface of the lower end of the reactor.

In addition, the partition plate is formed to be inclined downward from the outer peripheral side provided with the second opening toward the central part provided with the first opening, and at the bottom center of the reactor in the first opening. It is preferable to provide a riser pipe for supplying the gas rising from the tank.
By causing the gas rising to the riser pipe to flow, an upward flow can be generated from the bottom of the reactor toward the upper side of the partition plate, and the product liquid and the catalyst flowing into the lower side of the partition plate can be circulated.

In addition, a substantially cylindrical wall extending downward along the riser pipe is formed in the first opening of the partition plate, and a catalyst separation filter is disposed on the outer peripheral side of the cylindrical wall and above the lower end of the cylindrical wall. A discharge pipe is preferably provided.
By providing a catalyst separation filter above the lower end of the cylindrical wall, the flow of the product liquid and catalyst flowing into the lower side of the annular space between the cylindrical wall and the riser pipe can be converted into an upward flow through the riser pipe. A circulating flow can be formed, and the product liquid flowing downward from the partition plate creates a stagnation in the flow of the product liquid containing the catalyst in the middle of the circulation path toward the riser pipe. An upward flow can be obtained.

In addition, a tube is disposed in the second opening in the outer peripheral side region of the partition plate so that the product liquid and the catalyst flow from the upper side of the partition plate toward the center of the bottom of the reactor. You may protrude above a board.
The product liquid and catalyst can be separated from the gas and part of the catalyst by rising from the partition plate to the top inlet of the tube, and the product liquid and catalyst can be reacted by flowing down from the top inlet through the tube along the bottom of the reactor. It can be guided toward the riser pipe provided near the bottom center of the vessel. At this time, the flow from the outlet at the lower end of the tube to the riser tube becomes smooth along the bottom surface of the reactor, and a low-speed upward flow from that region toward the catalyst separation filter can be obtained.

Moreover, the upper end inlet of the tube may be covered with the roof part.
As a result, it is possible to prevent the liquid, catalyst and source gas flowing up and down in the reactor from flowing directly into the upper end inlet of the tube after the reaction.

Also, a gas nozzle for supplying gas to the riser pipe is provided, and an upward flow is formed in the riser pipe by the gas flow of the gas nozzle, and a flow of the product liquid and the catalyst is formed from above to below in the gap between the cylindrical wall and the riser pipe. You may do it.
As a result, an upward flow is formed in the riser pipe by the gas flow of the gas nozzle, and the upward flow is formed by inverting the product liquid and the catalyst descending from the upper side of the partition plate in the gap between the cylindrical wall and the riser pipe with the riser pipe. it can.

According to the catalyst separation device of the present invention, the reaction liquid, the raw material gas, and the catalyst are allowed to react upstream and downstream by bubbles supplied upward from the gas distributor, and the lower side of the partition plate is generated from the opening. When the liquid and the catalyst flow, the product liquid and the catalyst are separated by the catalyst separation filter provided on the lower side of the partition plate, and the catalyst is captured and the product liquid can be discharged by the discharge pipe. For this reason, it can be used effectively by providing a catalyst separation filter below the gas distributor in the reactor, which has conventionally been wasted space, and if no catalyst separation filter is provided on the upper side, it can be produced. It does not adversely affect the flow such as obstructing the reverse flow of liquid and gas.
Further, since the raw material gas does not easily flow into the lower side of the partition plate, it is possible to prevent the adverse effect of the gas accompanying the product liquid flowing into the lower side of the partition plate. Moreover, by providing a filter consisting of a catalyst separation filter on the lower side of the reactor, the product liquid and the catalyst can be filtered and separated to the bottom of the reactor equipped with the catalyst separation filter in a state where the reaction is stopped. The amount of the product liquid remaining in the catalyst remaining in the reactor can be reduced.

  Moreover, since the opening of the partition plate has a first opening for raising the catalyst and the product liquid and a second opening for lowering the catalyst and the product liquid, the catalyst is moved downward from the second opening of the partition plate. The product liquid is allowed to flow down and flow into the first opening through the riser tube at the center of the bottom of the reactor, so that the upward flow of the product liquid and catalyst can be formed downward from the second opening of the partition plate. The product liquid containing the catalyst to be separated can be separated into the product liquid and the catalyst by the catalyst separation filter.

The partition plate is formed by inclining downward from the outer peripheral side provided with the second opening toward the central part provided with the first opening, and rising from the center of the bottom of the reactor to the first opening. Since the riser pipe is supplied, the flow of gas rising to the riser pipe can generate a flow from the bottom of the reactor to the upper side of the partition plate, and it flows into the lower side of the partition plate. A circulation path can be formed by generating an upward flow of liquid and catalyst.
In addition, since the partition plate is inclined downward toward the central portion, the downward flow in the outer region is reversed again to the upward flow in the central region by the bubble flow of the gas distributor with respect to the upper slurry flow. The pressure loss at the time of performing can be suppressed, and a smooth circulation amount can be formed.

  In addition, a substantially cylindrical wall extending downward along the riser pipe is formed in the first opening of the partition plate, and the catalyst separation filter and the discharge are disposed on the outer peripheral side of the cylindrical wall and above the lower end of the cylindrical wall. Since the pipe is arranged, most of the product liquid and catalyst flowing in from the second opening slowly descends slowly along the bottom of the reactor and flows to the inlet of the riser pipe. Is obtained from the catalyst, so that the rising liquid is separated from the catalyst.

    In addition, a tube is disposed in the second opening in the outer peripheral side region of the partition plate so that the product liquid and the catalyst flow from the upper side of the partition plate toward the center of the bottom of the reactor. Since the product liquid and the catalyst that descends to the partition plate flow up to the tube and then flow up to the upper end inlet of the tube, the raw material gas can be separated and a part of the catalyst can be separated. Further, gas entrainment can be prevented from the product liquid descending to the lower side of the partition plate through the tube, catalyst entrainment can be suppressed, and the catalyst load on the catalyst separation filter is reduced.

  In addition, because the upper end inlet of the tube is covered with a roof, the product solution, catalyst, and gas generated by the reaction of the reaction solution, catalyst, and raw material gas above the gas distributor descend and flow directly into the tube. It is possible to prevent the gas from entraining the product liquid descending below the partition plate.

  Also, a gas nozzle for supplying gas to the riser pipe is provided, and an upward flow is formed in the riser pipe by the gas flow of the gas nozzle, and a flow of the product liquid and the catalyst is formed from above to below in the gap between the cylindrical wall and the riser pipe. Therefore, an upward flow can be formed in the riser pipe by the gas flow of the gas nozzle, and the product liquid and the catalyst descending from above in the gap between the cylindrical wall and the riser pipe can be reversed by the riser pipe to form the upward flow. Thus, a flow path can be formed that guides the flow of the product liquid and the catalyst descending from the second opening of the partition plate to the catalyst separation filter.

It is a schematic block diagram of the reactor containing the catalyst separation apparatus by embodiment of this invention. It is the elements on larger scale which show the structure of the catalyst separation apparatus of the reactor shown in FIG. It is the figure of the AA line of the gas distributor in the reactor shown in FIG. 2, and the BB sectional drawing. It is CC main part sectional drawing which shows the catalyst separation filter of a catalyst separation apparatus. It is a schematic explanatory drawing which shows the catalyst separation structure in the conventional reactor.

Hereinafter, a catalyst separation apparatus according to an embodiment of the present invention will be described with reference to the accompanying drawings.
The catalyst reaction device 20 shown in FIGS. 1 and 2 is provided with a catalyst separation device 22 below the reactor 21. The reactor 21 provided in the catalyst reaction apparatus 20 is substantially cylindrical, and has a substantially capsule shape in which upper and lower end portions are respectively formed with a substantially hemispherical upper end portion 21a and a lower end portion 21b. Therefore, this reactor 21 can withstand the reaction of the reaction liquid and gas under high temperature and high pressure.
The reactor 21 is filled with a reaction solution 24 which is a reaction solution, and a liquid surface 24a is formed in the vicinity of the upper end 21a. Further, for example, a fine catalyst 25 is dispersed and mixed in the reaction solution 24 as a catalyst. Note that a slurry is formed by the reaction solution 24 and the catalyst 25, and bubbles due to a raw material gas 28 described later are mixed into the slurry and reacted.

A cooling pipe 27 is disposed in a substantially cylindrical portion of the reactor 21 that stores the reaction liquid 24. In the cooling pipe 27, a supply side pipe 27 a and a discharge side pipe 27 b extend substantially parallel to the horizontal direction on the upper side in the reactor 21. A substantially U-shaped cooling pipe 27c having both ends connected to the supply side conduit 27a and the discharge side conduit 27b extends downward in a substantially U shape, and the substantially U-shaped cooling pipe 27c is supplied to the supply side conduit 27a and the discharge side conduit 27b. A plurality of lines are arranged at predetermined intervals in the extending direction of the side pipe line 27a and the discharge side pipe line 27b.
Therefore, the temperature of the reaction liquid 24 in the reactor 21 can be lowered and adjusted to a temperature suitable for the reaction by flowing the cooling liquid in the cooling pipe 27 and circulating it.

  In the reactor 21, a gas distributor 30 for supplying the raw material gas 28 upward is provided below the cooling pipe 27. The gas distributor 30 is provided with, for example, a multi-annular pipe (in FIG. 1 and FIG. 3, for example, a double annular pipe) substantially coaxially with the reactor 21, for example, an outer first annular pipe 31 and an inner side. The second annular tube 32 is disposed. The gas distributor 30 is provided with a communication pipe 33 connected to the first and second annular pipes 31 and 32 from the outside of the reactor 21 to supply the raw material gas 28.

The first annular pipe 31 has nozzles 31a formed at predetermined intervals on the lower surface thereof, and the second annular pipe 32 has nozzles 32a formed at predetermined intervals on the lower surface thereof. The plurality of nozzles 31a and 32a are preferably arranged on the same horizontal plane.
Therefore, the gas distributor 30 is supplied with the raw material gas 28 from an external tank (not shown) through the communication pipe 33 to the first and second annular pipes 31 and 32 and discharged from each nozzle 31a and 32a as bubbles. The bubbling device that rises to the top is configured. An upward flow is also generated in the reaction solution 24 and the catalyst 25 along with the upward flow of bubbles of the raw material gas 28.
As a result, the bubbles of the raw material gas 28, the reaction liquid 24, and the catalyst 25 form an upward flow in the central region in the reactor 21, and when they rise to the vicinity of the liquid surface 24a, they are reversed outside and fall downward. A flow is formed, and the bubbles of the raw material gas 28 react with the reaction liquid 24 and the catalyst 25. And there are many unreacted raw material components in the upward flow, and there are many reaction product components in the downward flow after reversing. This part constitutes the catalytic reaction apparatus 20.

Next, the catalyst separation device 22 will be described.
In the reactor 21 shown in FIGS. 1 and 2, a substantially mortar-shaped partition plate 35 is disposed below the gas distributor 30, and the outer peripheral edge thereof is in contact with the inner peripheral surface of the reactor 21. For example, a substantially cylindrical tubular wall 36 is formed at the center of the partition plate 35, and the tubular wall 36 is formed so as to descend in a substantially vertical direction toward the lower end portion 21 b. The opening 37 formed in step 1 is defined as the first opening.
In FIG. 2, for example, a riser pipe 39 is provided on the inner side of the cylindrical wall 36 so as to be substantially coaxially penetrated in the vertical direction, the upper end reaches the vicinity of the gas distributor 30, and the lower end is the cylindrical wall 36. Although it protrudes further downward, it may be retracted or at the same height.

A nozzle 40 for supplying a raw material gas 28 (or riser gas) extending through the lower end 21 b of the reactor 21 is inserted into the riser tube 39, and a small amount of the raw material gas 28 is discharged from the nozzle 40. Thus, an upward flow is formed in the riser pipe 39. The reason why the raw material gas 28 is supplied as bubbles from the nozzle 40 is to cause an upward flow in the riser pipe 39.
On the other hand, a ring-shaped space 41 having a relatively small and small area is formed between the riser tube 39 and the cylindrical wall 36. In this ring-shaped space 41, a downward flow is mainly formed by a slurry containing the product liquid 28 and the catalyst 25, and this slurry is reversed from the downward flow to the upward flow through the riser pipe 39.

  Small holes 43 are formed in the vicinity of the outer peripheral edge of the mortar-shaped partition plate 35 as a second opening in the circumferential direction at predetermined intervals, and slurry that descends above the partition plate 35 is placed in the small holes 43. Further, a down tube 44 for lowering is inserted. The upper end inlet of the down tube 44 protrudes above the small hole 43, and the lower part of the down tube 44 is bent below the partition plate 35 along the substantially hemispherical concave curved surface of the lower end 21 b of the reactor 21, so that the cylindrical wall A bottom exit is located near 36.

In addition, a roof portion 45 having a substantially L-shaped cross section is formed so as to surround the upper end inlet of each down tube 44, and a minute opening is formed as a vent hole 45a on the top surface of the roof portion 45. In addition, a small opening is formed in the partition plate 35 as a vent hole 46 in another region near the outer peripheral edge. These vent holes 45a and 46 are configured to allow the bubbles of the raw material gas 28 contained in the slurry and the product gas generated by the reaction to escape above the partition plate 35.
In the reactor 21, the slurry containing the bubbles of the raw material gas 28 and the product gas descending downward flows into the roof portion 45 through the gap between the partition plate 35 and the roof portion 45, and becomes an upward flow. Bubbles are separated and escape upward from the vent hole 45a of the roof portion 45, and slurry containing almost no bubbles flows from the upper end inlet of the down tube 44.

In FIG. 2, the catalyst 25 is separated from the slurry containing the product liquid 29 in a region where the central cylindrical wall 36 and the small holes 43 and the vent holes 46 in the vicinity of the outer peripheral end are removed from the lower side of the partition plate 35. Then, a catalyst separation filter 47 to be captured is provided as a filter. Further, the catalyst separation filter 47 is connected to a discharge pipe 48 for discharging the product liquid 29 obtained by removing the catalyst 25 from the slurry and the remaining unreacted raw material components to the outside.
As shown in FIG. 4, the catalyst separation filter 47 is arranged in a ring shape so as not to contact each other, for example, around the cylindrical wall 36, and further arranged in a ring shape so as not to be in contact with each other outside. . Therefore, these catalyst separation filters 47 are arranged in a double manner around the cylindrical wall 36, and are positioned above the lower end of the cylindrical wall 36 (see FIG. 2). As a result, the slurry discharged from the down tube 44 is filtered by the catalyst separation filter 47 through a low-speed liquid rising flow that can be separated by gravity, so that the high concentration catalyst slurry is adsorbed on the filter surface of the catalyst separation filter 47. To prevent it.
The discharge pipes 48 connected to the double catalyst separation filters 47 are arranged so as to protrude outward in the radial direction of the partition plate 35 to the outside of the reactor 21. Through the discharge pipe 48, the product liquid 29 and a slight amount of unreacted raw material components are discharged to the outside.

The upward flow of the slurry generated in the riser pipe 39 is generated by the upward flow of gas from the nozzle 40, but most of the slurry is generated in the down tube 44 so that the unreacted raw material gas 28 in the slurry at this time is minimized. The opening area of the ring-shaped space 41 and the diameter and quantity of the piping of the down tube 44 are set so that the slurry descends from the ring-shaped space 41 of the cylindrical wall 36 to the minimum. And
At this time, the flow rate flowing through the down tube 44 is greater than the downward flow in the ring-shaped space 41, and the flow rate of the slurry flowing through the down tube 44 and the flow rate of the slurry rising up the riser tube 39 are substantially equal.

The catalyst separation device 22 according to the present embodiment has the above-described configuration, and the catalyst separation method will be described with reference to FIGS. 1 and 2.
First, in the reactor 21, in the catalytic reaction device 20, the raw material gas 28 is supplied from the gas distributor 30 in a state where the slurry containing the reaction liquid 24 in which the catalyst 25 is dispersed in the reactor 21 is filled up to the liquid level 24 a. Are bubbled into the reaction solution 24 as bubbles. Then, the slurry containing bubbles becomes an upward flow in the central region due to the upward flow of the bubbles, reverses outward near the liquid surface 24 a to become a downward flow, and moves toward the partition plate 35. Then, the downward flow becomes a circulating flow that again becomes an upward flow in the central region due to the upward flow caused by the bubbles in the gas distributor 30.
The circulating flow is an upward flow in the central region between the liquid level 24a and the gas distributor 30, and the slurry contains many bubbles of the reaction solution 24, the catalyst 25, and the raw material gas 28 before the reaction. Then, the reaction liquid 24, the catalyst 25, and the raw material gas 28 react to generate a generated liquid 29 and a generated gas. In the downward flow in the outer region, the generated liquid 29, the catalyst 25, and the raw material gas 28 that are contained in a large amount in the slurry. And product gas.

In the catalyst separation device 22 on the lower side of the partition plate 35, a part of the slurry containing bubbles that have descended to the vicinity of the gas distributor 30 due to the downward flow in the reactor 21 is part of the roof 45 and the partition plate 35. By flowing into the roof portion 45 from the gap and once becoming an upward flow toward the upper end inlet of the down tube 44, the bubbles of the raw material gas 28 and the generated gas are separated from the slurry and escape upward from the vent hole 45a. . Thereby, almost no bubbles remain in the slurry. A part of the catalyst 25 is also separated from the product liquid 29 by gravity separation.
The remaining slurry flows into the down tube 44 from the upper end inlet of the down tube 44 and gently flows at a low speed along the substantially hemispherical concave curved surface of the lower end portion 21b of the reactor 21 toward the center of the bottom surface of the lower end portion 21b. It flows out from the exit.

  On the other hand, in the central region of the partition plate 35, a small amount of slurry is generated in the annular space 41 between the cylindrical wall 36 and the riser pipe 39 at a low speed at which the slurry falls downward from the opening 37. At this time, bubbles are separated from the descending slurry and rise. Further, bubbles of the raw material gas 28 (or riser gas) are supplied from the nozzle 40 to the riser pipe 39 loosely inserted into the cylindrical wall 36 via the ring-shaped space 41, and an upward flow is caused to the slurry in the riser pipe 39. It is generated. Therefore, a low-speed downward flow of the slurry is generated in the ring-shaped space 41, and is reversed at the lower end thereof and flows into the riser pipe 39 to generate a low-speed upward flow.

The slurry discharged at a low speed from the lower end outlet of the down tube 44 contains almost no bubbles, and flows up to the riser pipe 39 to become an upward flow, whereby the partition plate 35, the down tube 44, and the riser pipe. A circulation flow through 39 is formed. Moreover, between the lower end outlet of the down tube 44 and the riser pipe 39, the flow rate of the slurry is low and a smooth flow along the bottom surface occurs.
As a result, before reaching the riser pipe 39, a part of the slurry flows into a stagnation space 49 in the upper part of the smooth bottom surface flow region, and becomes an ascending flow with a low flow velocity. At this time, the product liquid 29 and the catalyst 25 in the slurry are separated by gravity sedimentation, and the product liquid 29 having a reduced concentration of the catalyst 25 flows into the catalyst separation filter 47.

In the catalyst separation filter 47, a part of the product liquid 29 and the catalyst 25 is separated in advance, so that a cake is hardly formed, and the filtration resistance is lowered. Then, the catalyst 25 is trapped by being filtered by the catalyst separation filter 47, and the product liquid 29 separated from the catalyst 25 remains a little unreacted reaction liquid 24 (and a slightly mixed raw material gas 28 and product gas). At the same time, it is discharged from the discharge pipe 48 to the outside.
By repeating such an action, the slurry containing the product liquid 29 produced by the reaction in the catalyst reaction device 20 is separated and removed when the raw material gas 28 flows into the upper end inlet of the down tube 44 of the catalyst separation device 22. Is done. Further, when the slurry of the product liquid 29 and the catalyst 25 flows out from the lower end outlet of the down tube 44, the catalyst 25 is separated by gravity when rising at a low speed in the stagnation space 49 formed in the upper part of the smooth bottom surface flow region. As a result, the amount of the catalyst 25 to be adsorbed and removed on the surface of the catalyst separation filter 47 can be reduced as much as possible. Therefore, the burden on the catalyst separation filter 47 is reduced and the frequency of backwashing is reduced or backwashing itself is performed. Can be eliminated.
Further, since the catalyst separation filter 47 and the discharge pipe 48 are provided in the vicinity of the lower end portion 21b below the gas distributor 30 and the partition plate 35 in the reactor 21, the reactor 21 is compared with the conventional catalyst separation device of this type. The product liquid 29 can be filtered and separated to near the bottom of the reactor, and the product liquid 29 in the slurry remaining in the lower part of the reactor 21 can be reduced.

  It should be noted that it is preferable to operate so that the flow velocity of the upward flow of the product liquid 29 from the stagnation space 49 to the catalyst separation filter 47 is smaller than the sedimentation speed of the catalyst 25 below the partition plate 35.

As described above, according to the catalyst separation device 22 according to the present embodiment, the gas distributor 30 is installed above the partition plate 35 and the catalyst separation filter 47 is arranged below the partition plate 35. Thus, the reaction process by the vertical flow of the reaction solution 24, the catalyst 25, and the raw material gas 28 can be sufficiently performed, and the catalyst is separated into a space below the gas distributor 30 that has been a wasteful space in the past. A filter 47 and a discharge pipe 48 can be installed and used effectively.
Moreover, by installing the catalyst separation filter 47 in the space below the gas distributor 30 of the reactor 21, it is provided near the bottom of the reactor 21 when the reaction in the reactor 21 is terminated or stopped. Since the product liquid 29 and the catalyst 25 can be separated by filtration up to the height of the catalyst separation filter 47 and the discharge pipe 48, the product liquid 29 and the catalyst 25 remaining in the reactor 21 can be reduced.

In addition, in the catalyst separation device 22, since the bubbles of the raw material gas 28 hardly flow below the partition plate 35, the catalyst resulting from the exothermic reaction due to the high-efficiency reaction described above, which is a harmful effect accompanying the gas in the product liquid 29. It is possible to prevent clogging due to sintering or filter-tightening, and there is no need to install a gas-liquid separator due to gas outflow.
Further, according to the catalyst separation device 22, a circulation flow is formed by the partition plate 35, the down tube 44, and the riser tube 39, and an upward flow occurs between the upper end inlet of the down tube 44 and the roof portion 45. A part of the raw material gas 28 and the catalyst 25 can be separated, and in the region where the catalyst separation filter 47 is arranged, the product liquid 29 and the catalyst 25 are separated by gravity by moving up the sludge stagnation space 49 at a low speed. It can settle and separate.
Therefore, in the catalyst separation filter 47, since the product liquid 29 and the catalyst 25 are partially separated in advance, the catalyst 25 contained in the product liquid 29 is reduced, the filtration resistance is low, and it is difficult to form a cake. The catalyst 25 can be separated and discharged from the liquid 29. Therefore, the catalyst adsorption load on the catalyst separation filter 47 can be reduced, the frequency of backwashing of the reactor 21 including the catalyst separation filter 47 can be reduced, or backwashing can be eliminated.

Further, in the catalytic reaction device 20 in the reactor 21, the slurry is introduced into the down tube 44 of the catalyst separation device 22 at the end of the downward flow that is the end of the reaction path consisting of the upward flow and the downward flow after inversion. Therefore, since the raw material gas and the product gas are separated from the product liquid 29 by the downward flow and the residual gas in the product liquid 29 is small, the separation of the catalyst 25 from the subsequent slurry is easy and the product liquid 29 is easily separated. . In particular, in this embodiment, since the upper part of the reactor 21 is not provided with a filter such as a catalyst separation filter, the slurry flows smoothly in the vertical direction, and the reaction and subsequent gas separation can be performed smoothly.
In the present embodiment, the catalyst reaction apparatus 20 is configured not to be provided with a catalyst separation filter on the upper side of the reactor 21, so that the upward flow of the slurry composed of the reaction liquid 24, the catalyst 25, and the raw material gas 28 and the downward flow due to inversion are reversed. The overall flow is better than the conventional catalytic reactor.

In addition, this invention is not limited to the above-mentioned embodiment, In the range which does not change the summary of this invention, the structure of embodiment mentioned above can be changed suitably.
For example, in the above-described embodiment, the small tube 43 is provided in the vicinity of the outer peripheral edge of the partition plate 35 and the down tube 44 is fitted, but the down tube 44 is not necessarily provided, and the inside of the reactor 21 is lowered. The slurry may rise from the center side of the partition plate 35 along the mortar-shaped inclined surface and flow from the small hole 43 to the lower side of the partition plate 35.

In the above-described embodiment, the opening 37 is provided in the center of the partition plate 35, and the ring-shaped space 41 and the coaxial riser pipe 39 are provided inside the opening 37. However, the opening 37 is configured only by the riser pipe 39. Thus, the ring-shaped space 41 may not be provided. Further, the upper end of the riser tube 39 may be located below the partition plate 35.
In the above-described embodiment, since the catalyst separation filter is not provided on the upper side of the reactor 21, the upward flow of the slurry composed of the reaction liquid 24, the catalyst 25, and the raw material gas 28 and the downward flow due to inversion are good. However, a catalyst separation filter may be provided in the upper part of the reactor 21. In this case, backwashing is necessary.

20 Catalytic reactor 21 Reactor 21b Lower end 22 Catalyst separator 24 Reaction liquid 25 Catalyst 28 Raw material gas 29 Product liquid 30 Gas distributor 31a, 32a Nozzle 35 Partition plate 37 Opening 39 Riser tube 41 Ring-shaped space 43 Small hole 44 Down Tube 45 Roof 45a, 46 Vent hole 47 Catalyst separation filter 48 Drain pipe 49 Stagnation space

Claims (7)

In a catalyst separation apparatus that supplies a raw material gas to a vertical substantially cylindrical reactor and reacts the reaction liquid, the raw material gas, and the catalyst with the catalyst in the reactor to obtain a product liquid,
A gas distributor for supplying a raw material gas is provided in the reactor, a partition plate having an opening through which the product liquid and the catalyst are circulated is provided on the lower side of the gas distributor, and a catalyst separation filter is provided on the lower side of the partition plate. A catalyst separation device characterized in that a discharge pipe is provided.   2. The catalyst separation device according to claim 1, wherein the opening of the partition plate includes a first opening for raising the catalyst and the product liquid and a second opening for lowering the catalyst and the product liquid.     The partition plate is formed to be inclined downward from the outer peripheral side provided with the second opening toward the central part provided with the first opening, and from the center of the bottom of the reactor to the first opening. 3. The catalyst separation device according to claim 1, further comprising a riser pipe for supplying the rising gas.     A substantially cylindrical wall extending downward along the riser pipe is formed in the first opening of the partition plate, and the catalyst separation filter is on the outer peripheral side of the cylindrical wall and above the lower end of the cylindrical wall. The catalyst separation device according to claim 3, wherein a discharge pipe is provided.     In the outer peripheral side region of the partition plate, a tube is disposed in the second opening so that the product liquid and the catalyst flow from the upper side of the partition plate toward the center of the bottom of the reactor, and an upper end of the tube is disposed. The catalyst separation device according to claim 3 or 4, wherein the inlet projects upward from the partition plate.   The catalyst separation device according to claim 5, wherein an upper end inlet of the tube is covered with a roof portion.   A gas nozzle for supplying gas to the riser pipe is provided, and an upward flow is formed in the riser pipe by the gas flow of the gas nozzle, and the flow of the generated liquid and the catalyst flows from above to below in the gap between the cylindrical wall and the riser pipe. The catalyst separation device according to any one of claims 4 to 6, wherein the catalyst separation device is formed.

Images