JPS6351903A - Extractor - Google Patents

Abstract

PURPOSE:To uniformize diameters of droplets and liquid flux diameters by connecting an adjusting tank for adjusting the liquid face level of light liquid in an extraction tank with a light liquid chamber. CONSTITUTION:A board 4b formed with a porous plate is installed horizontally at the upper section of the inside of an extraction tank 4, on the upper face of which a heavy liquid chamber 4B is formed, while on the lower side of which a light liquid chamber 4A is formed. An introduction port 4c for the heavy liquid provided in the heavy liquid chamber 4B, while a discharge port 4d for the heavy liquid is provided at the bottom of the light liquid chamber 4A. Further, a liquid level adjusting tank 5 is communicated with through said light oil chamber 4A and a piping 6, and the height of the end of an overflow tube 5a is so set as to keep the liquid level of an extractant A [the level of (a) in the sketch], which is to be a light liquid in the extraction tank 4, slightly higher than that of the drawing board 4b. As a result, the diameters of droplets dropping out of a drop port of the drawing board 4b and the flux diameter are uniformized, and the range of heavy liquid flow forming stabilized single droplets are widened.

Description

DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a liquid-liquid extraction device, and particularly to a gravity flow type extraction device.

[Prior art] A heavy liquid is dripped or flowed down from the top of an extraction tank, and as it falls through the light liquid filled in the extraction tank, it comes into liquid contact with the light liquid, and the target component (extract) is extracted. 8alJ in light liquid,
Liquid-liquid extraction devices for separating and collecting this to obtain the target product are used in various fields such as the petrochemical industry, the pharmaceutical industry, and the atomic crab industry.

FIG. 3 is a sectional view showing a schematic configuration of a conventional gravity flow type extraction device. Reference numeral 1 designates an extraction tank, in which a drawing board 2 having a flow outlet 2a is installed horizontally in the upper part thereof, and a heavy liquid chamber 1a and a light liquid chamber 1b are vertically divided.

A heavy liquid inlet 3a is provided at the top of the extraction tank 1, and a heavy liquid outlet 3b is provided at the bottom. Further, a light liquid extraction port 3d and an inlet port 3C are provided at the top and bottom of the light liquid chamber 1b, respectively. The heavy liquid introduced into the heavy liquid chamber la from the inlet 3a falls through the light liquid chamber 1b as droplets or a thin flux from the outlet 2a of the drawing plate 2, and during this period it comes into contact with the light liquid and becomes liquid. extraction is performed.

In addition, instead of the flat drawing board 2, there are also known ones in which a nozzle 2b is provided at the outlet 2a as shown in FIG. 4, and in which a spray device 2C is provided in the upper part of the extraction tank 1 as shown in FIG. ing. The spray device 2c shown in FIG. 5 has a drawing board on its lower side and a heavy liquid chamber 1a inside.

[Problems to be Solved by the Invention] In the gravity flow type extraction device as described above, droplets or a thin flux are formed from the flow opening 2a of the drawing plate 2 and fall through the light liquid, but when the heavy liquid It is not easy to form droplets or liquid flux with a constant particle size or bundle size depending on the flow rate of the light liquid, the liquid surface position of the light liquid, etc. If the particle size of the droplets varies in the extraction or back-extraction operation, a problem arises in that the extraction rate and back-extraction rate cannot be accurately controlled.

[Means for Solving the Problems] The present invention provides a drawing board in which a heavy liquid flow port is opened on the lower surface side to form a heavy liquid chamber above the drawing board, and a light liquid chamber below the drawing board. Adjustment for adjusting the liquid level of the light liquid in the extraction tank in an extraction device in which the heavy liquid formed and supplied to the heavy liquid chamber drips or flows down into the light liquid chamber from the flow-out port of the drawing plate. The tank is connected to a light liquid chamber.

[Function] In the extraction device of the present invention, it is possible to adjust the liquid level so that the liquid level of the light liquid is a predetermined height above the upper surface of the screen, and the liquid level can be adjusted in this way. By doing so, the diameter and flux diameter of droplets flowing down from the flow opening of the drawing board can be made uniform. Additionally, the range of heavy liquid flow rates at which stable single droplets are formed is widened.

[Example] Examples will be described below with reference to the drawings.

FIG. 1 is a longitudinal sectional view showing the configuration of an extraction device according to an embodiment of the present invention. Reference numeral 4 designates an extraction tank, inside of which a drawing board 4b made of a perforated plate is installed horizontally, a heavy liquid chamber 4B is formed on the upper surface thereof, and a light liquid chamber 4A is formed below it. The heavy liquid chamber 4B is provided with a heavy liquid inlet 4C, and the light liquid chamber is provided with a heavy liquid outlet 4d at the bottom. In order to return the heavy liquid from these outlet ports 4d to the inlet port 4C, a pipe 4e in which a pump 4f is interposed connects the inlet port 4C and the outlet port 4d.

Reference numeral 5 denotes a liquid level adjustment tank, which is communicated with the light liquid chamber 4A of the extraction tank 4 via piping 6. This liquid level adjustment tank 5 is provided with an overflow pipe 5a that is movable in the vertical direction and is inserted into the inside from the bottom surface thereof, and an extraction port 5b provided on the side wall of the liquid level adjustment tank 5 and this overflow The bottom of the pipe 5a is connected to the bottom of the pipe 5a by a circulation pipe 5d having a pump 5C.

In the extraction apparatus configured as described above, the operation will be described when a back extractant is used as the heavy liquid B and an oil agent is used as the light liquid A.

The back extractant introduced into the heavy liquid chamber 4B from the inlet 4C is
The reverse extractant B falls as droplets B' from the opening 4a of the drawing board 4b into the light liquid chamber 4A, and during this time it comes into contact with the oil agent and performs extraction. The liquid is returned to the heavy liquid chamber 4B from the port 4d via the pipe 4e. In the liquid level adjustment tank 5, the oil is continuously circulated from the extraction port 5b through the pipe 5d and into the overflow pipe 5d, but the liquid level of the light liquid extractant A in the extraction tank 4 is The height of the tip of the overflow pipe 5a is set so that the level is slightly above the drawing board 4b (the level indicated by the symbol "A").

The reverse extractant B in the heavy liquid chamber 4B reaches the opening 4a to replace the light liquid oil that has entered the bottom of the heavy liquid chamber 4B, and becomes droplets B'.

In this case, the reverse extraction agent as a heavy liquid will stay in the openings 4a up to the level indicated by the symbol "mouth", and each opening 4
The retention amount of the back-extracting agent in a is equalized, so that the back-extracting agent B is dripped with a uniform particle size. In addition, heavy liquid chamber 4B
The liquid level of extractant A, which is a light liquid in the interior (above “A”)
By adjusting up and down the reverse extractant liquid level (the above-mentioned "port") in each opening 4a can be adjusted, and the back extractant can be adjusted to obtain droplets with the optimum particle size for extraction. be.

FIG. 2 is a sectional view showing an extraction device comprising an extraction device 4a8 equipped with a tubular or holofiber type solid membrane and a crystallization means 9 according to an embodiment of the present invention.

First, the configuration of the extraction tank 8 will be explained.

In FIG. 2, reference numeral 10 denotes a cylindrical device casing of the extraction means 1, and a partition plate 1 is provided in two stages on the upper part of the casing.
2.14 defines a back extraction side introduction chamber 16 and a extraction material introduction chamber 18 on the lower surface side of the base 16. Furthermore, the lower part of the device casing 10 is also provided with two partition plates 20.
22 defines a raffinate discharge chamber 24 and a back extractant discharge chamber 26 below the raffinate discharge chamber 24 . In addition, the partition plates 14 and 20
A first chamber is provided between the two and serves as an oil chamber 28 through which oil flows. A vibrator-shaped solid membrane 3 is provided so as to communicate the extraction material introduction chamber 18 and the raffinate discharge chamber 24.
0 is provided, and its interior is a second chamber. Further, the lower part of the reverse extraction side introduction chamber 16 is communicated with the upper part of the oil chamber 28 through a drip pipe 32. Further, the lower part of the oil chamber 28 is communicated with the back extractant discharge chamber 26 through a communication pipe 34.

36 and 38 are an inlet and an outlet for the oil, respectively, and are connected by a pipe 42 having a pump 40.

44 and 46 are an inlet and an outlet for the extraction material, respectively, and 48 and 50 are an inlet and an outlet for the back-extracting agent, respectively.

Next, the structure of the crystallization means 9 will be explained.

Reference numeral 52 denotes a casing, the bottom of which is provided with a back extraction side inlet 54, and the upper part of which is provided with a back extraction sub-discharge port 56. The back-extraction side inlet 54 is connected to the back-extraction sub-discharge port 50 of the extraction tank 8 by a liquid supply means (in this embodiment, a pipe 60 having a pump 58). Further, the back extraction sub-discharge port 56 of the crystallization means is connected to the back extraction side inlet 48 of the extraction tank 8 by a liquid supply means (piping 62 in this embodiment).

Note that a discharge port 64 for extracting a portion of the back-extracting agent is provided at a mid-height portion of the casing 52 of the crystallization means 9, and this discharge port 64 is connected to a pipe 68 having a pump 66. The back extractant can be returned to the bottom of the casing 60 by the casing 60. Note that a pipe 70 for replenishing a back extractant such as H2304 is connected to the middle of the pipe 60 (downstream of the pump 58).

In the figure, 72 is a seed crystal placed in the casing 60.

In the extraction tank 8, the oil is introduced into the oil chamber 28, which is a first chamber, through the inlet 36, flows upward therein, reaches the extraction port 38, and is extracted out of the device casing 10. The oil extracted from the outlet 38 is returned to the inlet 36 through the pipe 42 and continuously circulated.

The extracted material is introduced into the extracted material introduction chamber 18 from the extracted material supply port 44 and then into the second chamber inside the solid membrane 30. Then, it flows downward therein and enters the raffinate discharge chamber 24. While passing through the pipe-shaped solid membrane 30, the extracted material comes into contact with the oil in the oil chamber 28 via the pipe wall surface of the solid membrane 30. As a result, extraction is performed, and the target substance (extract) in the extracted material flows into the oil solution.

The extracted material (raffinate) is stored in the raffinate discharge chamber 2.
4 and then discharged to the outside of the device casing 10 from the raffinate outlet 46.

The back extraction agent is introduced into the back extraction side introduction chamber 16 from the supply port 48 and then supplied into the extraction chamber 28 from the dripping pipe 32. In this embodiment, the back-extracting agent has a higher specific gravity than the oil agent and has a property that it does not dissolve in the oil agent, so when it is sent into the oil agent from the lower end of the dripping tube 32,
The liquid drops in the form of droplets or liquid columns (droplets in the illustrated example) through the extraction agent in the extraction chamber 28, and comes into direct contact with the oil agent for back extraction. Due to this direct contact, the extract in the oil agent is efficiently transferred to the back extractant.

The back-extracting agent that has undergone this back-extraction is introduced into the back-extracting agent discharge chamber 26 through the connecting pipe 34, and then is introduced into the back-extracting sub-discharge port 5.
0 to the crystallization means 9 through a pipe 60 having a pump 58. Note that, as described above, since the specific gravity of the back-extracting agent is greater than that of the oil agent, the extracting agent in the extraction chamber 28 does not enter the back-extracting agent discharge chamber 26.

The back extractant supplied into the casing 52 of the crystallization means 2 via the pipe 60 through the inlet 54 rises inside the casing 52 and brings the seed crystals 72 into a fluid state. Then, the contained substance to be extracted (extract) touches the seed crystal 72 and crystallizes.

On the other hand, the back-extracting agent from which the substance to be extracted has been crystallized and removed is extracted from the extraction port 56 and circulated through the piping 62 to the back-extracting agent supply port 48 of the extraction tank 8 .

The oil chamber 28 is connected to the overflow pipe 76 of the liquid level adjustment tank 74 via a flexible hose 78. The liquid level adjustment 4174 is constructed such that an overflow pipe 76 is inserted into the inside from the bottom surface and is erected, and this overflow pipe 76 is slidable in the vertical direction. Also, overflow pipe 7
The lower part of the overflow pipe 76 is branched into a T-shape, and the flexible hose 78 is connected to one of the branched overflow pipes 76. An oil extraction lower 4a is opened in the lower part of the adjustment tank 74, and a pipe 80, an extractant tank 82, and a pipe 84 communicate with the lower end of the other branched overflow pipe 76. and a pump 86 are installed. Therefore, in this extraction device as well, by adjusting the vertical position of the overflow pipe 76, the liquid level of the oil in the extraction tank 8 can be adjusted to be slightly above the partition plate 12.

In the above explanation, the extraction material and the oil agent are brought into contact with each other through a solid membrane, and the oil agent and the back-extracting agent are brought into direct contact with each other. By replacing them, the back extractant is introduced through the supply port 44 and the extraction material is introduced through the supply port 48, so that the back extraction agent and the oil agent are brought into contact through the solid film, and the extraction material and the extraction agent are brought into direct contact. You may also let them do so.

That is, in this example, either the extractant or the back-extracting agent is brought into contact with the oil agent through the solid membrane, and the other is brought into direct contact with the oil agent. Whether or not to contact the oil agent through the solid membrane is determined by the liquid quality of the three liquids, the extractant, the oil agent, and the back-extracting agent. If the extractor and the back-extractant that are more likely to form an emulsion with the oil agent are brought into contact with the oil agent through a solid film, emulsion formation can be prevented.

Furthermore, contacting with -+IQ without a solid membrane has the advantage that the extraction rate is faster and there is no possibility of crystals adhering to the solid membrane. Therefore, the extraction rate can be increased by bringing the side with a lower extraction rate into direct contact with the oil agent. Furthermore, by appropriately changing the flow rate of the liquid that is brought into direct contact with this oil agent, it is possible to control the extraction rate. Therefore, it is possible to adapt very easily to changes in water quality and amount of extracted material, etc.

Although FIG. 2 shows an apparatus equipped with - pipe-shaped solid membranes 30, the number of solid membranes may be two or more. Furthermore, a plurality of drip tubes 32 can be provided. By installing a plurality of solid membranes or dropping tubes, the processing capacity can be improved.

In this embodiment, examples of the solid membrane include semipermeable membranes made of polytetrafluoroethylene, cellulose acetate, polysulfone, polyvinyl chloride, polypropylene, polyamide, and the like.

In addition, in the embodiments shown in FIG. 1.2 above, the liquid droplets are dropped by the drawing plate 2.14, but
A nozzle may be provided at the drip opening of this drawing board 2.14. Further, the present invention can also be applied to an extraction device equipped with a spray device 2c as shown in FIG. Furthermore, the present invention
Instead of dropping droplets, a trickle flux may be allowed to flow down.

In the above embodiment, the level of the light liquid is adjusted by moving the overflow pipe up and down, but in the present invention, the liquid level in the extraction tank is adjusted by moving the liquid level adjustment tank 5.74 itself up and down. When operating the device of the present invention, the liquid level of the light liquid may be adjusted only at the beginning of operation, and during continuous operation, the liquid level may be adjusted. It is not enough to do that.

[Effects of the Invention] As described above, according to the present invention, the liquid level of the light liquid in the extraction tank can be adjusted to a desired level.
The droplet diameter of the heavy liquid dropped into the light liquid becomes constant, and the extraction rate and back extraction rate can be easily controlled. Furthermore, the range of heavy liquid amounts at which a single droplet is stably formed is expanded. Furthermore, according to the present invention, there is also the effect that it becomes difficult to form an emulsion in the extraction tank.

[Brief explanation of drawings]

FIGS. 1 and 2 are cross-sectional views showing the configuration of an extraction device according to an embodiment of the present invention, and FIGS. 3, 4, and 5 are cross-sectional views schematically showing 13 components of a conventional extraction device. . 4.8...Extraction tank, 5...Liquid level adjustment tank,
16... Reverse extractant introduction chamber, 18... Extractant introduction chamber, 26... Reverse extractant discharge chamber, 28... Extractant chamber,
30...Solid membrane, 74...Liquid level adjustment tank. Agent Patent Attorney Tsuyoshi Shigeno Figure 1

Claims (2)

[Claims] (1) A drawing board with a heavy liquid outlet opening on the lower side is provided inside, a heavy liquid chamber is formed above the drawing board, and a light liquid chamber is formed below, and the heavy liquid chamber an extraction tank having a heavy liquid inlet opening at the bottom and a heavy liquid outlet opening at the bottom of the light liquid chamber; and a light liquid level adjustment tank connected to the light liquid chamber. An extraction device featuring: (2) The extraction device according to claim 1, wherein the extraction tank defines a chamber through which the extraction material or a back-extracting agent passes through a solid membrane.