JP4566087B2 - Concentrator and method of operating the same - Google Patents

Description

The present invention relates to a concentrating device for concentrating a solution, a crystallizing device for growing crystals from the concentrated solution, and a concentrating crystallization system in which the concentrating device and the crystallizing device are combined.

Non-Patent Document 1 proposes a batch type concentration apparatus shown in FIG. 6 as a concentration apparatus for concentrating a solution in which a solute is dissolved in a solvent to produce solute crystals. The batch type concentrator 100 includes a heating container 101, a gas-liquid separation container 102, a supply pipe 103 for supplying a solution and its vapor from the heating container 101 to the gas-liquid separation container 102, and a heating container from the gas-liquid separation container 102. A return pipe 104 for returning the solution (concentrated liquid) to 101 and a discharge pipe 105 for taking out the concentrated liquid from the gas-liquid separation container 102 are provided. According to the concentrating device 100, the solution is heated in the heating container 101 by the heater 106 disposed inside the heating container 101. The heated solution and its vapor are supplied to the gas-liquid separation container 102 through the supply pipe 103. In the gas-liquid separation container 102, droplets are collected by a gas-liquid separator (demister blanket) 107 provided on the upper part of the gas-liquid separation container 102. The collected liquid droplets are collected in the gas-liquid separation container 102 together with the solution supplied from the heating container 101, and are returned to the heating container 101 again via the return pipe 104. However, since the concentration apparatus 100 is a batch type concentration apparatus, the solution to be concentrated is exposed to a high temperature state for a long time (for example, 10 hours) and is subjected to thermal stress. Therefore, it is not suitable for the concentration of materials whose physical properties are likely to change when heated.
Nuclear Industry Vol.38, NO.8 (1992)

As a crystallization apparatus for precipitating crystals from a solution concentrated by a concentration apparatus, a crystallization apparatus shown in FIG. The crystallizer 110 includes a crystallization vessel 111, a stirring blade 112 for stirring the concentrated solution stored in the crystallization vessel 111, and a crystal slurry containing crystals grown in the crystallization vessel 111. A return pipe 113 and a pump 114 are provided that are extracted from the bottom of 111 and returned to the crystallization vessel 111 again. In the crystallizer 110 having such a configuration, the stirring blade 112 constantly rotates and agitates the solution in order to increase the crystal growth efficiency by effectively cooling the concentrated solution during crystal growth. Therefore, when the pump 114 is driven in a state where the amount of the solution present in the crystallization vessel 111 is small, bubbles mixed in the solution by the stirring of the stirring blade 112 enter the pump 114, and the pump 114 runs idle and is damaged. Therefore, the crystallization process cannot be started until the solution is sufficiently stored in the crystallization vessel 111.
JP 2005-33951 A

Accordingly, the present invention has a high concentration rate, thermal stress on the solution is small, and an object thereof is to provide a continuous solution concentrator and an operating method of a continuous capable concentrated.

  In order to achieve such an object, the concentrating device according to the present invention includes at least one heating pipe (27) arranged in the vertical direction, and a solution (from the lower end opening (29) to the heating pipe (27) ( 2) a supply unit (3) for supplying the liquid, a droplet separation chamber (43) that surrounds the upper portion of the heating tube (27) and is located on the upper end opening (28) of the heating tube (27), and an upper end of the heating tube A container (37) forming a concentrate recovery chamber (39) surrounding the opening, a concentrate return pipe (46) connecting the concentrate recovery chamber (39) and the lower end opening (29) of the heating pipe (27), A droplet separator (45) is disposed in the droplet separation chamber (43), and separates the droplets contained in the vapor and supplies the droplets to the concentrate recovery chamber (39).

The concentration apparatus according to the present invention also includes a heating chamber (30) that surrounds the periphery of the heating tube (27) and accommodates a heating medium that heats the solution in the heating tube (27).

The concentration apparatus according to the present invention further includes a density measuring unit (50) for measuring the density of the concentrated solution, and extracting the concentrated solution from the concentrated liquid recovery chamber (39) or the concentrated liquid return pipe (46). And a first control unit (51) for controlling the extraction unit (48) based on the density measured by the density measurement unit (50) and extracting the concentrated solution.

The concentration apparatus according to the present invention further includes a flow rate measurement unit (50) for measuring the flow rate of the solution flowing through the concentrate return pipe (46), a solution supply unit (3) for supplying the solution to the heating pipe (27), A second control unit (51) is provided that adjusts the amount of solution supplied from the solution supply unit (3) to the heating tube (27) based on the flow rate measured by the flow rate measurement unit (50).

Concentrator according to the present invention further, the upper end position of the heat pipe (27) is arranged above the upper end position of the concentrate return pipe (46), concentrate collection chamber (39), the concentrate return pipe ( 46), It is comprised so that a solution may circulate naturally through a heating tube (27).

The operation method of the concentrating device according to the present invention was concentrated from the sampling unit by controlling the sampling unit based on the density measured by the density measuring unit by the first control unit using the concentrating device of the present invention. Extracting the solution, adjusting the amount supplied from the solution supply unit to the heating tube based on the flow rate measured by the flow rate measurement unit by the second control unit, and continuously extracting a constant density solution from the extraction unit. Features.

  The concentrated crystallization system of the present invention is a combination of the above concentration apparatus and crystallization apparatus.

  According to the concentrating device and the system including the concentrating device according to the present invention, it is possible to control the concentration of the solution at an arbitrary constant magnification. Moreover, the solution supplied continuously or almost continuously from the solution supply unit can be continuously concentrated and discharged. Therefore, the solution supplied to the concentrating device at a certain time is not exposed to the heated state for a long time. Therefore, the concentration apparatus of the present invention is suitable for concentration of materials whose physical properties are easily changed by receiving heat because the thermal stress applied to the solution is small. Furthermore, since the main part of the concentrating device is composed of two containers arranged one above the other, the occupation area is small and the overall size can be reduced.

  The best mode for carrying out the present invention will be described below with reference to the accompanying drawings. In the following description, “upper”, “lower” and their derivatives are used to describe the state and positional relationship of the components shown in the drawings, but their use makes it easier to understand the invention. And should not be used to define the technical scope of the invention. Moreover, the same code | symbol is used for the same or similar part represented by several drawing.

[1] Concentrated crystallization system: FIG. 1 shows a schematic configuration of a concentrated crystallization system according to the present invention (hereinafter simply referred to as “system”). In the illustrated system 1, a solution 2 to be processed by the system 1 is stored in a solution storage container (solution supply unit) 3. The solution storage container 3 is connected to the continuous concentration apparatus 4 according to the present invention via a solution supply means 5. The solution supply means 5 includes a solution supply pipe 6 that connects the solution storage container 3 and the concentrating device 4, and a solution supply valve 7 attached to the solution supply pipe 6, and is based on opening and closing of the solution supply valve 7. Then, the solution is supplied from the solution storage container 3 to the concentration device 4 through the solution supply pipe 6.

  The concentrating device 4 includes a heating unit 8 having a lower structure and a recovery unit 9 having an upper structure connected to the heating unit 8. The heating unit 8 heats the solution supplied from the solution storage container 3 by the heating unit 8. The recovery unit 9 recovers the heated solution and separates and recovers the droplets from the vapor. The solution (concentrated liquid) collected by the collection unit 9 is returned to the heating unit 8. In this way, the solution is concentrated by repeating the process of heating and gas-liquid separation. On the other hand, the vapor from which the droplets have been removed by the recovery unit 9 is condensed by the condenser 10, and the condensate is recovered by a recovery device (not shown).

  The solution 2 concentrated by the concentrator 4 (hereinafter, this concentrated solution is referred to as “concentrate 11”) is sent to the crystallizer 13 via the concentrate transport means (concentrate transport pipe 12). The crystallization apparatus 13 includes a crystallization container 14, and the concentrated liquid 11 sent from the concentration apparatus 4 via the concentrated liquid transporting means 12 is supplied to the crystallization container 14. The crystallizer 13 is provided with a poor solvent storage container 15 for storing a poor solvent (for example, methanol) that promotes crystallization of a solute, and transport of the poor solvent from the product solvent storage container 15 to the crystallization container 14. The poor solvent 17 is supplied through the means (the poor solvent transport pipe 16) and mixed with the concentrate 11. The ratio of the concentrated liquid 11 and the poor solvent 17 supplied to the crystallization container 14 is managed to be constant.

  The crystallizer 13 has a circulation means 18 for taking out a part of the concentrated liquid 11 from the crystallizer 14 and returning it to the crystallizer 14 again. The circulation means 18 starts from the bottom of the crystallization vessel 14, passes through the ceiling portion of the crystallization vessel 14 and returns to the crystallization vessel 14, and the crystallization vessel 14 passes through the return tube 19. A circulation pump 20 is provided which takes out the concentrate 11 from the bottom and sends it back into the crystallization vessel 14 again. The return pipe 19 is provided with a cooling unit or cooler (first cooler) 21 so that the concentrated liquid transported through the return pipe 19 is cooled by the cooler 21. The bottom of the crystallization vessel 14 is connected to a solid-liquid separator 22. Therefore, the concentrated liquid in the crystallization vessel 14 is cooled by the cooler 21 while being circulated through the return pipe 19 to be crystallized into a crystal slurry. Then, the crystal slurry is taken out from the crystallization vessel 14 and supplied to the solid-liquid separator 22 where only the grown crystals are taken out.

[2] Concentrator: The concentrator 4 will be described with reference to FIG. The heating unit 8, which is the lower structure of the concentrating device 4, has a lower container 23. The lower container 23 is formed of a cylindrical body, has a cylindrical wall portion 24 arranged in the vertical direction, and an upper end portion and a lower end portion of the cylindrical wall portion 24 are closed by an upper wall 25 and a lower wall 26, respectively. Has been. The plurality of heating tubes 27 through which the heated fluid solution 2 passes in the heating unit 8 are arranged in the vertical direction inside the cylindrical wall portion 24, and the upper end portion (upper end opening 28) and the lower end of each heating tube 27. A portion (lower end opening 29) projects through the upper wall 25 and the lower wall 26. As shown in FIG. 3, in the embodiment, nine heating tubes 27 are arranged at regular intervals in the horizontal direction, but the number and arrangement of the heating tubes 27 are not limited to the example. . Returning to FIG. 2, the heating medium chamber (heating chamber) 30 that is surrounded by the cylindrical wall portion 24, the upper wall 25, and the lower wall 26 and that is in contact with the outer peripheral surface of the heating tube 27 is the cylindrical wall portion 24. Are connected to the heating medium supply unit 33 and the heating medium recovery unit 34 via the heating medium inlet 31 and the heating medium outlet 32 provided in the heating medium, respectively. The heating medium is supplied from the heating medium supply unit 33 to the heating medium chamber 30. Thereafter, the heating medium is discharged from the heating medium chamber 30 to the heating medium recovery unit 34 and recovered.

  The bottom of the cylindrical wall portion 24 is covered with a bottom lid 35, and a lower end opening 29 of each heating pipe 27 is connected to a distribution chamber (supply portion) 36 formed between the bottom lid 35 and the lower wall 26. Yes. The distribution chamber 36 is connected to the solution storage container 3 via the solution supply pipe 6. Based on the control of the solution supply valve 7, the solution 2 is supplied from the solution storage container 3 to each heating pipe 27 via the distribution chamber 36. To be supplied.

  The collection unit 9 that is the upper structure of the concentrating device 4 has an upper container 37. The upper container 37 is formed of a cylindrical body having a larger diameter than the cylindrical body of the lower container 23 and has a cylindrical wall portion 38 disposed in the vertical direction. The cylindrical wall portion 38 of the upper container 37 is disposed coaxially with the cylindrical wall portion 24 of the lower container 23. Further, the lower part of the cylindrical wall part 38 in the upper container 37 is externally spaced from the upper part of the cylindrical wall part 24 in the lower container 23, and a recovery chamber 39 consisting of an annular space on the upper outer periphery of the lower container 23. Is formed. The upper container 37 and the lower container 23 are connected to an annular flange 40 fixed to the lower end of the upper container 37 on an annular flange 40 fixed to the outer periphery of the lower container 23. The bottom of the recovery chamber 39 is closed. The upper part of the upper container 37 is opened to form a steam outlet 42, which is connected to the condenser 10 (see FIG. 1).

  A droplet separation chamber 43 is formed inside the upper container 37, and gas-liquid separation means is disposed in the droplet separation chamber 43. In the embodiment, the gas-liquid separating means is opposed to the upper end opening 28 of the heating tube 27 with a predetermined distance upward, and disperses the steam discharged from the heating tube 27 radially outward, and the dispersion plate 44 A droplet separator (demister blanket) 45 that contacts and separates and collects the droplets contained in the vapor in contact with the vapor dispersed by the plate 44 is disposed.

  The collection chamber 39 is connected to the distribution chamber 36 of the lower container 23 via the concentrated liquid return pipe 46, and the concentrated liquid (solution) 11 collected in the collection chamber 39 is connected to the lower container 23 via the concentrated liquid return pipe 46. Returned to the distribution chamber 36. As shown in the figure, the concentrated liquid return pipe 46 extends in the horizontal direction from the recovery chamber 39, and the lower end of the inner surface of the horizontal portion is positioned at a predetermined height H 1 from the bottom of the recovery chamber 39.

  The collection chamber 39 is connected to the crystallization container 14 via the concentrated liquid transport pipe 12. The concentrated liquid transport pipe 12 is provided with a concentration adjusting valve (extraction portion) 48, and the concentration of the concentrated liquid 11 is adjusted by adjusting the opening and closing of the concentration adjusting valve 48 as will be described in detail later. Further, the concentrate transport pipe 12 is connected to the droplet separation chamber 43 of the upper container 37 through a pressure equalizing pipe 49. Further, as shown in the figure, the concentrate transport pipe 12 is connected to the recovery chamber 39 from the horizontal direction, and the lower end of the inner surface thereof is located at a predetermined height H2 from the bottom of the recovery chamber 39, and this height H2 Is larger than the height H1 of the concentrate return pipe 46.

  In order to control the concentration rate in the concentrating device 4 and the supply amount of the solution to the concentrating device 4, a mass flow meter (density measuring unit) 50 capable of measuring the flow rate and the mass density is provided in the concentrated liquid return pipe 46. The output unit of the mass flow meter 50 is connected to the input unit of the control unit (concentration rate and supply amount control unit) 51, and the density of the concentrate 11 and the return flow rate measured by the mass flow meter 50 are transferred to the control unit 51. It is supposed to be output. The output unit of the control unit 51 is connected to a concentration adjustment valve 48 provided in the concentrate transport pipe 12, and the concentration adjustment valve 48 is controlled to open and close based on the output from the control unit 51. Further, the output unit of the control unit 51 is connected to the solution supply valve 7 provided in the solution supply pipe 6 and the flow meter 52, and the control unit 51 refers to the solution supply amount measured by the flow meter 52. The solution supply valve 7 is controlled. The concentrated liquid return tube 46 is also provided with an observation window or sight glass 53 for monitoring the residual amount (hole up amount) of the solution 2 or the concentrated liquid 11 present in the concentrating device 4, and the concentrated liquid is passed through the sight glass 53. The liquid level of the concentrated liquid 11 in the return pipe 46 is made visible.

  According to the concentration device 4 having such a configuration, the solution 2 supplied from the solution storage container 3 via the solution supply pipe 6 based on the control of the solution supply valve 7 is supplied to the lower container 23 in the heating unit 8. It enters the distribution chamber 36 where it is distributed to a plurality of heating tubes 27. On the other hand, a heating medium heated from the heating medium supply unit 33 is supplied to the heating medium chamber 30 of the lower container 23, and the solution 2 in the heating tube 27 is heated by this heating medium. The heating medium may be either gas or liquid.

  The heated solution 2 is in a gas-liquid mixed phase in which gas and liquid are mixed in the heating tube 27, and the solution (concentrated liquid) 11 flowing out from the upper end opening 28 of the heating tube 27 into the droplet separation chamber 43 is the lower part. It moves outward on the upper wall 25 of the container 23 and flows into the collection chamber 39. On the other hand, the vapor of the solution 2 rises from the upper end opening 28 of the heating tube 27 to the droplet separation chamber 43 and is dispersed by the dispersion plate 44, and then the droplet (concentrated solution) is separated by the droplet separator 45. And recovered. The droplets collected by the droplet separator 45 fall to the bottom of the upper container 37 and are collected in the collection chamber 39. The concentrated liquid 11 stored in the recovery chamber 39 passes through the concentrated liquid return pipe 46 based on the density difference between the concentrated liquid 11 in the concentrated liquid return pipe 46 and the gas-liquid mixed phase solution 2 in the heating pipe 27. And move naturally to the distribution chamber 36. That is, the solution 2 (concentrated liquid 11) naturally circulates along a circulation path (concentrated liquid circulation system) connecting the distribution chamber 36 to the heating pipe 27, the recovery chamber 39, and the concentrated liquid return pipe 46. The principle of this natural circulation will be described later.

  In this way, the density of the concentrate 11 gradually increases in the process of circulating the concentrate 11. The density of the concentrate 11 is measured by a mass flow meter 50 provided in the concentrate return pipe 46 and output to the control unit 51. The control unit 51 determines whether or not the measured density has reached a density (predetermined value) corresponding to the target concentration rate. If the measured density is equal to or higher than the predetermined value, the concentration adjusting valve 48 is opened to collect the recovery chamber 39. The concentrated liquid 11 is discharged to the crystallizer 13. Conversely, when the measured density is less than the predetermined value, the control unit 51 closes the concentration adjustment valve 48 and interrupts the extraction of the concentrate 11. As described above, in the concentration device 4, the extraction amount is adjusted according to the concentration of the concentrated solution 11, thereby appropriately managing the density (concentration rate) of the concentrated solution 11 supplied to the crystallizer 13.

  The density (concentration rate) control is closely related to the management of the solution supply amount from the solution storage container 3 to the concentration device 4. Therefore, the control unit 51 supplies the solution 2 to the concentration device 4 through the solution supply pipe 6 while referring to the flow rate of the concentrated liquid transported through the concentrated liquid return pipe 46 based on the output of the mass flow meter 50. At this time, the control unit 51 cascade-controls the solution supply valve 7 while confirming the supply amount based on the output of the flow meter 52 provided in the solution supply pipe 6, thereby the concentrate flowing through the concentrate return pipe 46. 11, that is, the hold-up amount of the concentrator 4 is kept constant. In addition, the concentration apparatus 4 of the embodiment includes the sight glass 53 in the concentrated liquid return pipe 46, and if the liquid level confirmed through the sight glass 53 is constant, the hold-up amount is maintained constant. When the hold-up amount increases or decreases, the liquid level rises or falls, so it can be visually confirmed whether or not the hold-up amount is maintained constant via the sight glass 53.

  The principle of natural circulation will be described with reference to FIG. In the figure, symbol L1 indicates the lower end height of the heating tube 27, symbol L2 indicates the upper end height of the heating tube 27, and symbol L2 'indicates the minimum height at which the concentrate flows from the recovery chamber into the return tube. The symbol h1 indicates the distance from L1 to L2, and the symbol h1 'indicates the distance from L1 to L2'. The symbol ρ indicates the specific gravity of the solution 2 in the gas-liquid mixed phase in the heating tube 27, and the symbol ρ ′ (> ρ) indicates the specific gravity of the concentrated liquid 11. In the concentrating device 4, the heights h <b> 1 and h <b> 1 ′ are determined so that the relationship of ρ · h <ρ′h ′ is established. As a result, the solution 2 in the gas-liquid mixed phase in the heating pipe 27 forms an upward flow, the concentrated liquid 11 in the concentrated liquid return pipe 46 forms a downward flow, and the heating pipe 27 and the concentrated liquid as a whole. A circulation flow that circulates through the return pipe 46 is formed. Note that the upper end opening of the heating tube is above the upper end position of the concentrate return tube.

  Thus, according to the concentration apparatus 4 according to the present invention, the solution supplied continuously or almost continuously from the solution storage container 3 can be continuously concentrated to the target magnification and discharged. In addition, since the degree of concentration can be controlled, there is no need for additional concentration to compensate for insufficient concentration. Therefore, the solution supplied to the concentrating device 4 at a certain time is not exposed to the heated state for a long time. Therefore, the concentration apparatus of the present invention is suitable for concentration of materials whose physical properties are easily changed by receiving heat because the thermal stress applied to the solution is small. Moreover, the heating unit 8 and the recovery unit 9 are arranged one above the other, and the main part of the concentrating device 4 is composed of one container in which the lower container 23 of the heating unit 8 and the upper container 37 of the recovery unit 9 are combined. . Further, the area occupied by the concentrator is small, and as a whole, the concentrator can be reduced in size as compared with the conventional concentrator.

  In the above description, the annular concentrated liquid recovery chamber 39 is formed outside the lower container 23. However, the heating tube 27 is sufficiently protruded from the lower container upper wall 25 and is adjacent to the lower container upper wall 25 and heated. The surrounding space surrounding the tube protrusion can also be used as a concentrate recovery chamber.

[3] Crystallizer: The crystallizer 13 will be described with reference to FIG. As shown in the figure, the crystallizer 13 has a crystallizer 14 for mixing and stirring the concentrate 11 and the poor solvent 17 respectively supplied from the concentrator 4 and the poor solvent storage container 15 to produce a crystal slurry. . The crystallization vessel 14 has a substantially cylindrical peripheral wall 55 centered on the vertical axis, a substantially spherical ceiling portion 56 projecting upward, and a substantially spherical bottom portion 57 projecting downward. A large-capacity upper concentrated liquid storage chamber (first concentrated liquid storage chamber) 58 is formed on the bottom 57. Further, the bottom 57 has a central portion bulging downward, and a lower concentrated liquid storage chamber (second concentrated liquid storage chamber) 59 having a smaller diameter and a smaller volume than the upper concentrated liquid storage chamber 58 is formed. Hereinafter, the whole of the upper concentrated liquid storage chamber 58 and the lower concentrated liquid storage chamber 59 is referred to as a “concentrated liquid storage chamber 60” as necessary.

  In order to cool the concentrate 11 stored in the crystallization vessel 14, one end of a slurry transport pipe 61 is connected to the center of the bottom of the lower concentrate storage chamber 59. The slurry transport pipe 61 includes the slurry circulation pump 20 and the cooler 21, and extends through the ceiling portion 56 of the crystallization container 14 into the concentrated liquid storage chamber 60. An end of the slurry transport pipe 61 located in the concentrate storage chamber 60 is directed in the circumferential horizontal direction to form an injection nozzle 63, and the upper concentrate storage chamber 58 is formed by the slurry injected from the injection nozzle 63. In addition, a rotary stirring flow is formed in the lower concentrated liquid storage chamber 59.

  The concentrated liquid transport pipe 12 and the poor solvent transport pipe 16 pass through the ceiling portion 56 and are connected to the concentrated liquid storage chamber 60. Similarly, a seed crystal supply pipe 65 from the seed crystal storage container 64 connects the ceiling portion 56 to the concentrated liquid storage chamber 60.

  According to the crystallization apparatus 13 configured in this way, the concentrate, the poor solvent, and the seed crystal are supplied to the crystallization container 14 from the concentration apparatus 4, the poor solvent storage container 15, and the seed crystal storage container 64, respectively. Then, at the start of the crystallization process, the supplied concentrated liquid or the like accumulates in the lower concentrated liquid storage chamber 59. When a predetermined amount (a predetermined depth) of concentrated liquid or the like is accumulated in the lower concentrated liquid storage chamber 59, the slurry circulation pump 20 starts to drive, and the concentrated liquid extracted from the lower concentrated liquid storage chamber 59 is transferred to the slurry transport pipe 61. The concentrated liquid or the like moving through the slurry transport pipe 61 is cooled by the cooler 21. At this time, the concentrated liquid or the like stored in the lower concentrated liquid storage chamber 59 moves in the circumferential direction by extracting the concentrated liquid or the like from the bottom of the lower concentrated liquid storage chamber 59 based on the driving of the slurry circulation pump 20. The center of the liquid level drops. However, since the cross-sectional area of the lower concentrated liquid storage chamber 59 is extremely smaller than the cross-sectional area of the upper concentrated liquid storage chamber 58, the liquid level required for circulation can be secured with a small amount of concentrated liquid. Moreover, there is no stirring blade in the conventional crystallizer. Therefore, air is not involved in the concentrated liquid or the like extracted from the crystallization vessel 14, and the idling of the slurry circulation pump 20 caused by the entrained air can be avoided.

  The concentrated liquid or the like extracted from the lower concentrated liquid storage chamber 59 in this way is supplied to the cooler 21 via the slurry transport pipe 61 and cooled here to precipitate crystals, and then the injection nozzle 63. To the concentrate storage chamber 60. At this time, the crystal slurry sprayed from the spray nozzle 63 forms a stirring flow in the lower concentrated liquid storage chamber 59, whereby the mixed liquid, the poor solvent, and the seed crystal are mixed and stirred. Usually, a predetermined time (for example, 1 hour) is required for crystallization. Therefore, when about 1 hour has passed after the supply of the concentrated liquid or the like is completed, the crystallization is completed, the valve 67 of the slurry discharge pipe 66 branched from the slurry transport pipe 61 is opened, and the solid-liquid separator 22 is supplied.

  As described above, according to the crystallizer 13 according to the present invention, the cooling and crystal growth process can be started from the time when a predetermined amount of concentrate or the like is accumulated in the lower concentrate storage chamber 59. In comparison, the time required to start crystallization can be shortened. Further, immediately after the start of crystallization, only the cooler 21 provided in the slurry transport pipe 61 may be driven to cool the slurry.

1 is a diagram showing a schematic configuration of a concentrated crystallization system according to the present invention. The longitudinal cross-sectional view of the concentration apparatus which concerns on this invention. FIG. 3 is a transverse cross-sectional view of the concentrator shown in FIG. 2 taken along line III-III. 1 is a longitudinal sectional view of a crystallization apparatus according to the present invention. The figure explaining the principle by which a circulating flow is formed in a concentration apparatus. The perspective view of the conventional concentration apparatus. Sectional drawing of the conventional crystallizer.

Explanation of symbols

1: system, 2: solution, 3: solution storage container (solution supply unit), 4: concentrator, 5: solution supply means, 6: solution supply pipe, 7: solution supply valve, 8: heating unit, 9: recovery Parts: 10: condenser, 11: concentrate, 12: concentrate transport means (concentrate transport pipe), 13: crystallizer, 14: crystallizer, 15: poor solvent storage container, 16: poor solvent transport means (Poor solvent transport pipe), 17: Poor solvent, 18: Circulation means, 19: Return pipe, 20: Circulation pump, 21: Cooler, 22: Solid-liquid separator, 23: Lower container, 24: Cylindrical wall 25: upper wall, 26: lower wall, 27: heating pipe, 28: upper end opening, 29: lower end opening, 30: heating medium chamber (heating chamber), 31: heating medium inlet, 32: heating medium outlet, 33: Heating medium supply unit, 34: heating medium recovery unit, 35: bottom lid, 36: distribution chamber (supply unit), 37: upper container 38: cylindrical wall part, 39: recovery chamber, 40: annular flange, 41: annular flange, 42: steam outlet, 43: droplet separation chamber, 44: dispersion plate, 45: droplet separator, 46: concentrate Return pipe, 48: Concentration adjustment valve (extraction part), 49: Pressure equalizing pipe, 50: Mass flow meter, 51: Control part, 52: Flow meter, 53: Cytoglass, 55: Peripheral wall, 56: Ceiling part, 57: Bottom: 58: Upper concentrate storage chamber, 59: Lower concentrate storage chamber, 60: Concentrate storage chamber, 61: Slurry transport pipe, 63: Injection nozzle, 64: Seed crystal storage container, 65: Seed crystal supply pipe.

Claims (2)

At least one heating tube arranged in a vertical direction;
A solution supply section for supplying a solution to the heating tube from its lower end opening;
Surrounds the upper part of the heating tube, a container forming a concentrate collection chamber surrounding the upper end opening of the heating tube and the droplet separation chamber located on the upper end opening of the heating tube,
A droplet separator that is disposed in the droplet separation chamber, separates the droplets contained in the vapor, and drops the droplets to the concentrate recovery chamber ;
A concentrated liquid return tube for connecting the concentrated liquid recovery chamber and the solution supply unit, and returning the concentrated solution recovered in the concentrated liquid recovery chamber to the solution supply unit;
A heating chamber surrounding a heating tube and containing a heating medium for heating the solution in the heating tube;
An extractor for extracting the concentrated solution from the concentrate recovery chamber or the concentrate return pipe;
A density measuring unit for measuring the density of the concentrated solution;
A first control unit for controlling the extraction unit based on the density measured by the density measurement unit to extract the concentrated solution;
A flow rate measuring unit for measuring the flow rate of the solution flowing through the concentrate return pipe,
A solution supply unit for supplying a solution to the heating tube;
A second control unit that adjusts the amount of the solution supplied from the solution supply unit to the heating tube based on the flow rate measured by the flow rate measurement unit;
The upper end position of the heating pipe is disposed above the upper end position of the concentrate return pipe, and the solution is configured so that the solution naturally circulates in the concentrate recovery chamber, the concentrate return pipe, and the heating pipe. To concentrate. At least one heating tube arranged in a vertical direction;
A solution supply unit for supplying a solution to the heating tube from its lower end opening;
A container that surrounds the upper portion of the heating tube and forms a liquid droplet separation chamber located on the upper end opening of the heating tube and a concentrated liquid recovery chamber surrounding the upper end opening of the heating tube;
A droplet separator that is disposed in the droplet separation chamber, separates the droplets contained in the vapor, and drops the droplets to the concentrate recovery chamber;
A concentrated liquid return pipe for connecting the concentrated liquid recovery chamber and the solution supply unit, and returning the concentrated solution recovered in the concentrated liquid recovery chamber to the solution supply unit;
A heating chamber that surrounds the heating tube and contains a heating medium that heats the solution in the heating tube;
An extractor for extracting the concentrated solution from the concentrate recovery chamber or the concentrate return tube;
A density measuring unit for measuring the density of the concentrated solution;
A first control unit for controlling the extraction unit based on the density measured by the density measurement unit and extracting the concentrated solution;
A flow rate measuring unit for measuring the flow rate of the solution flowing through the concentrate return pipe,
A solution supply unit for supplying a solution to the heating tube;
A second control unit that adjusts the amount of the solution supplied from the solution supply unit to the heating tube based on the flow rate measured by the flow rate measurement unit;
  Using the concentrator configured so that the upper end position of the heating pipe is located above the upper end position of the concentrate return pipe, and the solution is naturally circulated through the concentrate recovery chamber, the concentrate return pipe, and the heating pipe. ,
  The first control unit controls the extraction unit based on the density measured by the density measurement unit to extract the concentrated solution from the extraction unit,
  The second control unit adjusts the amount supplied from the solution supply unit to the heating tube based on the flow rate measured by the flow rate measurement unit,
  A method for operating a concentrator, wherein a solution having a constant density is continuously extracted from the extraction portion.

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