JP6413587B2 - Multi-tube separation membrane module and liquid processing method - Google Patents

Description

  The present invention relates to a liquid processing method for separating a part of components from a solution, and a multitubular separation membrane module used in this method.

  A multi-tubular separation membrane module is known as an apparatus for separating components in a solution. The separation membrane element used in this multi-tubular separation membrane module is a tubular separation membrane made of zeolite or the like having fine pores about the size of the molecules to be separated. As a method for separating a specific component from a solution, a method is known in which a specific component is vaporized and separated by bringing the fluid of the solution into contact with one (outer surface) of the separation membrane element and depressurizing the other (inner surface). It has been.

  In such a multitubular separation membrane module, in order to increase the separation efficiency, it is necessary to efficiently bring the solution to be separated into contact with the entire length of the separation membrane element.

  Patent Document 1 describes a multi-tubular separation membrane module in which a plurality of separation membrane elements are horizontally installed in a cylindrical casing whose horizontal direction is the cylinder axis direction.

  Patent Document 2 illustrates a method in which a tubular zeolite membrane composite is immersed in a liquid to be separated so that the tube axis direction is in the vertical direction, the zeolite membrane composite is decompressed with a vacuum pump, and water is permeated and vaporized. Has been.

JP 2013-39546 A JP 2013-13884 A

  Patent Document 1 does not describe that the liquid to be processed is continuously supplied into the casing and the liquid to be processed is processed in a batch manner.

  As in Patent Document 2, when the zeolite membrane composite is immersed in the liquid to be processed and the liquid to be processed is processed, the liquid to be processed can be processed batchwise. However, in Patent Document 2, since the zeolite membrane composite is installed so that the tube axis direction is the vertical direction, when the liquid level of the liquid to be treated is lowered, the upper portion of the zeolite membrane composite is in the air. It is exposed and the separation operation cannot continue any further.

  An object of the present invention is to provide a multitubular separation membrane module that can efficiently process a liquid to be treated in a batch manner, and a liquid processing method using the multitubular separation membrane module.

  The multi-tubular separation membrane module of the present invention has a tank body having an opening on the upper surface, and a plurality of tubular separation membranes arranged and arranged in a substantially horizontal direction at the lower part of the tank body, To do.

  The multi-tubular separation membrane module of one aspect of the present invention is a multi-tubular separation membrane module including a separation membrane unit provided in the tank body, and the separation membrane unit can be attached to and detached from the opening. A lid plate mounted; the tubular separation membrane supported by the lid plate; a suction port provided in the lid plate; and communication means for communicating the suction port and the inside of the tubular separation membrane. It is characterized by.

  In one aspect of the present invention, the tank body may be provided with a plurality of the separation membrane units. Further, a support block is suspended from one end of the lower surface of the lid plate, a support plate is suspended from the other end of the lower surface of the lid plate, and one end side of the tubular separation membrane is fixed to the support block. ing. As the communication means, a passage is provided in the support block. Further, the other end side of the tubular separation membrane is sealed and supported by the support plate. In this case, it is preferable that the tubular separation membrane is inserted into and supported by an opening provided in the support plate.

  In the present invention, an agitation bar having one end supported by the support block and the other end supported by the support plate may be provided. In this case, a first magnet is provided at one end of the stirring rod, the first magnet faces the inner surface of the side wall of the tank body, and the first magnet is disposed on the outer surface of the side wall of the tank body. It is preferable that a second magnet is disposed so as to face the magnet, and the second magnet can be rotated by a motor.

  The liquid processing method of the present invention uses such a multitubular separation membrane module of the present invention.

  The liquid processing method includes a step of supplying a liquid to be processed into the tank, a step of depressurizing the inside of the tubular separation membrane to permeate the liquid to be processed, and a liquid level of the liquid to be processed in the tank. And a step of discharging the liquid in the tank after being lowered to a predetermined level.

  In the multi-tubular separation membrane module of the present invention, since a plurality of tubular separation membranes are installed substantially horizontally in the lower part of the tank body, when the liquid to be processed is accommodated in the tank body and processed in a batch manner, the tank Even if the liquid level of the liquid to be treated in the body is considerably lowered, the tubular separation membrane is immersed in the liquid, and the separation treatment of the liquid to be treated can be continued. For this reason, according to this invention, the batch type process of a to-be-processed liquid can be performed efficiently.

  In one embodiment of the present invention, since the separation membrane unit is detachable from the tank body, the separation membrane unit and the tank body can be carefully cleaned by removing the separation membrane unit from the tank body.

  In one embodiment of the present invention, since a plurality of separation membrane units are attached to the tank body, the separation membrane units can be easily attached and detached even when the number of tubular separation membranes is large.

  In one embodiment of the present invention, since the separation membrane unit is provided with the stirring rod, the liquid in the tank can be easily stirred. Further, the stirring mechanism can be taken into and out of the tank integrally with the separation membrane unit.

  By configuring the stirring rod to be rotationally driven by the magnet coupling mechanism, it is not necessary to provide a shaft seal device for the stirring rod in the tank body.

1 is a perspective view of a multitubular separation membrane module according to an embodiment. FIG. 2 is an exploded view of the multitubular separation membrane module of FIG. 1. It is a side view of the multi-tubular separation membrane module of FIG. It is the IV-IV sectional view taken on the line of FIG. It is the VV sectional view taken on the line of FIG. FIG. 6 is a cross-sectional view taken along line VI-VI in FIG. 5. It is an enlarged vertical sectional view of the VII part of FIG. It is a longitudinal cross-sectional view which shows the structure of the front end side of a tubular separation membrane. It is a perspective view of the multi-tubular separation membrane module which concerns on another embodiment. It is a side view of the tank body of FIG.

  Hereinafter, embodiments will be described with reference to the drawings. 1 to 8 show a multi-tubular separation membrane module according to the first embodiment.

  As shown in FIGS. 1 and 2, a multi-tubular separation membrane module 1 according to this embodiment includes a rectangular parallelepiped tank body 2 having an open top surface, and a separation membrane unit 3 detachably attached to the tank body 2. And a motor unit 4.

  In the motor unit 4, a motor 4a and a magnet plate 4b that is rotationally driven by the motor 4a are installed.

  The separation membrane unit 3 includes a cover plate 5 covering the upper surface of the tank body 2, grips 6 provided on the upper surfaces of both ends in the longitudinal direction of the cover plate 5, and upward from one end side of the cover plate 5 in the longitudinal direction. It is bridged between the protruding nozzle 7, the support plate 8 and the support block 10 provided so as to hang downward from the lower surface of the cover plate 5, and the lower portions of the support plate 8 and the support block 10. It has a tubular separation membrane 20 and a stirring rod 30 provided. Although not shown, a decompression device such as a vacuum pump is connected to the nozzle 7 via a pressure-resistant hose and a cold trap.

  The support block 10 is located on one end side in the longitudinal direction of the lid plate 5, and the support plate 8 is located on the other end side in the longitudinal direction of the lid plate 5.

  The support block 10 has a thick plate shape extending in the short width direction of the tank body 2, and includes a main block 11 and a top block 12 overlapping the upper surface of the main block 11 as shown in FIGS. The top block 12 is fixed to the lower surface of the lid plate 5 with bolts (not shown). The top block 12 is fixed to the main block 11 with bolts (not shown).

  A shallow concave groove 13 is provided on the upper surface of the main block 11. The concave groove 13 extends in the width direction of the tank body 2 so as not to reach the peripheral edge on the upper surface of the main block 11.

  A plurality of (four in this embodiment) vertical holes 14 are formed from the bottom surface of the concave groove 13 to the vicinity of the bottom of the main block 11. From the lower part of the vertical hole 14, a horizontal hole 15 is bored toward the center in the longitudinal direction of the tank body 2.

  The horizontal holes 15 are provided in a plurality (two in each vertical hole 14 in this embodiment) with different vertical positions. The horizontal hole 15 penetrates to the plate surface of the main block 11 on the center side in the longitudinal direction of the tank body 2.

  A female screw 15 a is engraved on the inner peripheral surface of the horizontal hole 15 on the plate surface side. The proximal end side of the tubular separation membrane 20 is screwed to the female screw 15a.

  By fixing the top block 12 to the upper surface of the main block 11, the inside of the groove 13 becomes a chamber communicating with each vertical hole 14. The lower end of the nozzle hole 7a is opened in this chamber. The upper end of the nozzle hole 7 a opens at the tip of the nozzle 7.

  In the embodiment shown in FIG. 1, the lid plate and the support block are integrated. However, the lid plate and the support block may not be integrated, and the lid plate and the support block may be separately detachable from the tank body.

  As shown in FIGS. 7 and 8, the tubular separation membrane 20 includes a tubular porous support 21, a zeolite membrane 22 formed on the outer peripheral surface of the porous support plate 21, and a base end of the porous support 21. It has a boss piece 23 provided coaxially and an end piece 24 provided coaxially at the tip of the porous support 21.

  The boss piece 23 has a cylindrical shape, and the inside of the tubular separation membrane 20 communicates with the lateral hole 15. The end piece 24 seals the tip of the tubular separation membrane 20. The boss piece 23 and the end piece 24 are connected to a porous support 21 with a zeolite membrane by heat shrink films 25 and 26. The end piece 24 has a hollow portion 24a recessed from the porous support 21 side in order to reduce weight.

  In the middle of the boss piece 23 in the longitudinal direction, a hexagonal flange 23a for tool engagement is provided. A male screw 23b that is screwed into the female screw 15a of the lateral hole 15 is formed on the outer peripheral surface on the main block 11 side of the flange 23a.

  An O-ring 27 is installed on the side surface of the flange 23a on the main block 11 side.

  When the boss piece 23 of the tubular separation membrane 20 is tightened into the horizontal hole 15, the O-ring 27 is sandwiched between the flange 23 a and the main block 11, thereby sealing the inside of the tank body 2 and the horizontal hole 15. Is done.

  The end piece 24 of the tubular separation membrane 20 is inserted into and supported by the insertion hole 8a of the support plate 8.

  As the material of the tubular porous support 21, an inorganic porous support of a ceramic sintered body containing silica, α-alumina, γ-alumina, mullite, zirconia, titania, yttria, silicon nitride, silicon carbide and the like. Can be mentioned.

  The zeolite membrane 22 is preferably formed by crystallizing zeolite on the surface of the porous support 21.

  The main zeolite constituting the zeolite membrane usually contains a zeolite having an oxygen 6-10 membered ring structure, and preferably contains a zeolite having an oxygen 6-8 membered ring structure.

  The zeolite membrane may be a single membrane of the zeolite, or the zeolite powder is dispersed in a binder such as a polymer to form a membrane, and the zeolite is fixed in a film form on various supports. A zeolite membrane composite may be used. The zeolite membrane may partially contain an amorphous component or the like.

  However, the present invention may use a tubular separation membrane having a separation membrane other than the zeolite membrane.

  The stirring rod 30 has a quadrangular prism shape except for both end sides. The tip of the stirring bar 30 is rotatably supported by the support plate 8. The base end side of the stirring rod 30 is a shaft rod 31 that is rotatably supported by the support block 10. A magnet plate 32 is fixed to the tip of the shaft 31. The magnet plate 32 faces the side wall of the tank body 2 and faces the magnet plate 4b of the motor unit 4 across the side wall to constitute a magnet coupling mechanism.

  In order to process a liquid using the multi-tubular separation membrane module 1 configured in this way, as shown in FIG. 2, the liquid to be treated is accommodated in the tank body 2, and the separation membrane unit 3 is placed in the tank body. Attach to 2. In this case, the grip 6 is gripped by a hand or a working robot, and the tubular separation membrane 20 is gently lowered so as to be immersed in the liquid to be treated, and the cover plate 5 is brought into contact with the upper edge of the tank body 2. In addition, you may provide packing and a shock absorbing material in the upper edge of the tank body 2, or the peripheral part lower surface of the cover board 5. FIG.

  Next, the decompression device (not shown) connected to the nozzle 7 is operated to decompress the inside of the tubular separation membrane 20. Further, the stirring bar is rotated by the motor unit 4 as necessary. As a result, a specific component (for example, water) in the liquid to be treated permeates the separation membrane, is vaporized in the tubular separation membrane 20, and is discharged through the horizontal hole 15, the vertical hole 14, and the nozzle 7, and the separation operation is performed. Is called.

  If the liquid level in the tank body 2 is lowered to a specified level above the uppermost surface of the tubular separation membrane 20, the decompression is stopped, the separation membrane unit 3 is pulled up from the tank body 2, and the inside of the tank body 2 is Remove the concentrate. The tank body 2 may be provided with a drainage port, the liquid may be discharged from the drainage port, the liquid may be pumped out using a liquid feed pipe, and the tank body 2 is tilted to cause the liquid to flow out. May be.

  Thereafter, a new liquid to be treated is accommodated in the tank body 2, and the separation process is performed according to the above procedure.

  In this multi-tubular separation membrane module 1, the tubular separation membrane 20 is horizontally installed at the lower part in the tank body 2, so that even when the liquid in the tank body 2 is highly concentrated, the tubular separation membrane 20 Is not exposed to the gas phase and can be efficiently concentrated in a batch manner.

  In this multitubular separation membrane module 1, since the stirring rod 30 is provided, the separation efficiency can be improved. The stirring rod 30 is rotationally driven by the motor unit 4 via a magnet coupling mechanism. For this reason, the shaft bar 31 of the stirring rod 30 does not penetrate the side wall of the tank body 2 and does not require a liquid seal bearing. Therefore, the liquid to be treated is not contaminated by grease or the like.

  In this multitubular separation membrane module 1, the separation membrane unit 3 can be easily taken out from the tank body 2, and the separation membrane unit 3 and the tank body 2 can be easily cleaned.

  The subject to be separated or concentrated is not particularly limited as long as it is a liquid mixture composed of a plurality of components that can be separated or concentrated by a separation membrane, and may be any mixture. The liquid to be treated may be fruit juice or a mixture of an organic compound such as ethanol and water, for example, a brewing liquid.

  In the embodiment described above, one separation membrane unit 3 is installed in the tank body 2, but a plurality of separation membrane units may be installed. Moreover, the separation membrane unit 3 may be configured not to have a stirring bar.

  An example of such a multitubular separation membrane module 1A is shown in FIGS. In this multitubular separation membrane module 1A, three separation membrane units 3A are installed in the tank body 2A. The separation membrane unit 3A is not provided with the stirring rod 30, is different in the arrangement and number of the tubular separation membranes 20, and has a through-hole 8b in the upper part of the support plate 8, except for the separation membrane unit 3A. 3 has the same structure.

  The upper surface of the tank body 2A is covered with the lid plate 5 and the lid plate 40 of the three separation membrane units 3A. In the tank body 2 </ b> A, a circulation space 41 is formed below the lid plate 40. A drainage pipe 42 with a valve 43 is connected to the bottom of the space 41. The tank body 2 </ b> A is installed on the gantry 44.

  In the space 41, a rotary blade or a submerged pump for circulating the liquid in the tank body 2A may be provided. A heater or a heat exchanger may be provided in the tank body 2A.

  This multi-tubular separation membrane module 1A can also efficiently process the liquid to be processed. In this multitubular separation membrane module 1A, since a large number of tubular separation membranes 20 are provided, a large amount of liquid to be treated can be processed. In this multi-tubular separation membrane module 1A, since a plurality of separation membrane units 3A are provided, the weight of each separation membrane unit 3A is small and easy to attach and detach.

  The above embodiment is an example of the present invention, and the present invention may be other than the above.

  Examples The present invention will be described more specifically with reference to examples. However, the present invention is not limited to the description of the following examples unless it exceeds the gist.

(Example)
The multi-tubular separation membrane module shown in FIG. 1 was used to dehydrate the koji juice as the liquid to be treated. A glass trap was connected to the nozzle (permeate vapor outlet) of the multi-tubular separation membrane module via a vacuum tube, and a vacuum pump was disposed at the subsequent stage to form a vacuum line.

Eight tubular separation membranes having a diameter of 12 mm and a length of 40 cm (zeolite separation membrane, effective membrane area: 0.1023 m ² , MSM-1, manufactured by Mitsubishi Chemical Corporation) were attached to the separation membrane unit. A separation membrane unit equipped with the above tubular separation membrane is put into a PET tank containing 4 L of persimmon juice (100% concentrated reduced persimmon juice, trade name: Welch 100, manufactured by Calpis Co., Ltd.) using a stirring rod. The liquid to be treated was stirred.

  Dehydration was performed at temperatures of 10, 15, and 30 ° C. In the case of 10 and 15 ° C., the temperature was controlled by bringing the cooling coil into contact with the surface of the koji juice in the tank. In the case of 30 ° C., the koji juice separately heated to 30 ° C. was put into the tank, and a rubber heater was placed under the tank to control the temperature. Further, the permeation side pressure varied depending on the test temperature, but was 0.3 to 0.9 kPaA.

  The treated permeate was colorless and transparent. Table 1 shows the results of measuring the weight of this permeate and converting it to permeate flux. The reason why the permeation flux at 30 ° C. suddenly increases as compared to 10,15 ° C. is that the water pressure increases rapidly above 15 ° C. It was confirmed that the permeation flux was proportional to the driving force when organized by driving force (water pressure on the supply side-pressure on the permeation side).

DESCRIPTION OF SYMBOLS 1,1A Multitubular separation membrane module 2,2A Tank body 3,3A Separation membrane unit 4 Motor unit 8 Support plate 10 Support block 20 Tubular separation membrane 30 Stirring rod

Claims (7)

A tank body having an opening on the upper surface;
A plurality of tubular separation membranes arranged in a substantially horizontal direction at the bottom of the tank;
Have a, a multi-tubular separation membrane module with a separation membrane unit provided cistern body,
The separation membrane unit is
A lid plate removably attached to the opening;
The tubular separation membrane supported by the lid plate;
A suction port provided in the lid plate;
Communicating means for communicating between the suction port and the inside of the tubular separation membrane;
Multitubular separation membrane module, characterized in that the have a. The multitubular separation membrane module according to claim 1 , wherein the tank body is provided with a plurality of the separation membrane units. In claim 1 or 2 ,
One end side of the tubular separation membrane is fixed to a support block,
The other end of the tubular separation membrane is sealed and supported by a support plate;
A multi-tubular separation membrane module, wherein a passage is provided in the support block for sucking the inside of the tubular separation membrane. 4. The multi-tubular separation membrane module according to claim 3 , wherein the tubular separation membrane is inserted into and supported by an opening provided in the support plate. In Claim 3 or 4 , a stirring rod having one end supported by the support block and the other end supported by the support plate is provided.
A first magnet is provided at one end of the stirring bar, the first magnet faces the inner surface of the side wall of the tank body,
A multi-tubular separation membrane characterized in that a second magnet is arranged on the outer surface of the side wall of the tank body so as to face the first magnet, and the second magnet can be rotated by a motor. module. A liquid processing method using the multi-tubular separation membrane module according to any one of claims 1 to 5 . In claim 6 ,
Supplying a liquid to be treated into the tank;
Depressurizing the inside of the tubular separation membrane to permeate the liquid to be treated;
A step of discharging the liquid in the tank after the liquid level of the liquid to be treated in the tank is lowered to a predetermined level;
The liquid processing method characterized by having.

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