JP2013078737A - Liquid extraction device and fluid removing method - Google Patents

Abstract

PROBLEM TO BE SOLVED: To suppress energy consumption when replacing a liquid component of a mixture with a supercritical fluid.SOLUTION: A liquid extraction device 20 includes an accommodation part 450 and a filtering extraction part 452. The accommodation part 450 accommodates a mixture and a supercritical fluid. The mixture includes a solid component and a liquid component. The filtering extraction part 452 extracts some of the liquid component from the mixture, by filtering the mixture in the accommodation part 450. The liquid extraction device 20 further includes a pressurizing part. The pressurizing part pressurizes the filtering extraction part 452 so that a pressure is applied to the mixture when the filtering extraction part 452 filters the mixture.

Description

  The present invention relates to a liquid take-out apparatus and a fluid removal method, and more particularly to a liquid take-out apparatus and a fluid removal method capable of suppressing energy consumption when a liquid component of a mixture is replaced with a supercritical fluid.

  Patent document 1 discloses the manufacturing method of a nanoparticle. This method includes a step of replacing the solvent of the dispersion with a supercritical fluid, and a step of vaporizing the supercritical fluid. In this dispersion, particles are dispersed in a solvent. This supercritical fluid is a gas at normal temperature and pressure. According to the method disclosed in Patent Document 1, industrially useful dried nanoparticles can be produced. Further, according to the method disclosed in Patent Document 1, the following effects can also be obtained. The first effect is that the nanoparticles can be cleaned better than before. The second effect is that the nanoparticles can be dried better than before. The third effect is that the nanoparticles during drying can be prevented from being exposed to the outside.

JP 2009-160518 A

  However, the method disclosed in Patent Document 1 has a problem that a large amount of energy is consumed in the replacement with the supercritical fluid. The present invention has been made to solve such problems. An object of the present invention is to provide a liquid take-out apparatus and a fluid removal method capable of suppressing energy consumption when a liquid component of a mixture is replaced with a supercritical fluid.

  The liquid take-out device of the present invention will be described with reference to the drawings. It should be noted that the reference numerals in the figure are used in this column in order to help understanding of the contents of the invention, and are not intended to limit the contents to the illustrated range.

  In order to solve the above-described problems, according to one aspect of the present invention, the liquid take-out device 20 takes out a part of the liquid component from the mixture. The mixture includes a solid component and a liquid component. The liquid extraction device 20 includes a storage unit 450, a filtration extraction unit 452, and a pressurization unit 182. The accommodating part 450 accommodates a mixture and a supercritical fluid. The filtration extraction part 452 extracts a part of liquid component from a mixture by filtering the mixture in the accommodating part 450. FIG. The pressurizing unit 182 applies pressure to the mixture when the filter extraction unit 452 filters the mixture.

  Much energy is required to make a material a supercritical fluid. In order to replace a liquid component with a supercritical fluid, a supercritical fluid corresponding to the amount of the liquid component is required. The fact that a supercritical fluid corresponding to the amount of the liquid component is required means that a lot of energy corresponding to the amount of the liquid component is required. This is a cause of consuming a lot of energy. By removing a part of the liquid component from the mixture before the replacement with the supercritical fluid by the filter extraction unit 452, the amount of the liquid component replaced by the supercritical fluid can be reduced as compared with the case where the filtration is not performed. The amount of liquid component to be taken out is not particularly limited. For example, the amount may be an amount such that aggregation does not occur in the solid component in the mixture after the liquid component is removed. As the amount of liquid component replaced by the supercritical fluid decreases, the amount of energy consumed to produce the supercritical fluid also decreases. When the liquid extraction part 452 applies pressure to the mixture at the time of taking out the liquid component from the mixture, the following effects are produced as compared with the case where the filtration extraction part 452 does not apply pressure. The effect is that when the liquid component remaining in the mixture after filtration is replaced with a supercritical fluid, the energy required for the supercritical fluid to once become a supercritical fluid after it is no longer a supercritical fluid can be reduced. It is the effect. If the pressure in the storage unit 450 is lower than the pressure of the supercritical fluid, the pressure of the supercritical fluid decreases when the supercritical fluid is caused to flow into the storage unit 450. When the pressure drops, the supercritical fluid may become a gas. In order to make this gas a supercritical fluid again, it is necessary to apply pressure to at least the gas. The lower the pressure in the container 450, the greater the pressure required to make the gas a supercritical fluid again. If the filtration extraction part 452 applies a pressure to a mixture, the average pressure in the accommodating part 450 can be made high compared with the case where the filtration extraction part 452 does not apply a pressure. If the average pressure in the container 450 is high, the pressure that must be added to make the gas a supercritical fluid again becomes small. In some cases, the supercritical fluid that has entered the housing portion 450 may not become a gas. If the added pressure is small, the energy for adding the pressure is also small. Since consumption of energy for generating the supercritical fluid and energy for adding pressure can be suppressed, energy consumption when replacing the liquid component of the mixture with the supercritical fluid can be suppressed.

  Moreover, it is desirable that the above-described filter extraction unit 452 includes a filter medium 462 and a re-mixing prevention unit 466. The filter medium 462 filters the mixture in the container 450. The re-mixing prevention unit 466 prevents the filtrate from re-mixing into the mixture. The filtrate is a liquid component extracted from the mixture by the filter medium 462.

  By preventing the re-mixing of the filtrate into the mixture by the re-mixing prevention unit 466, the amount of the mixture after filtration can be reduced as compared with the case where the filtrate is easily mixed into the mixture. Thereby, energy consumption can be suppressed.

  Alternatively, it is desirable that the above-described re-mixing prevention unit 466 includes the discharge pipe 510 and the valves 512, 514, 516, and 518. The discharge pipe 510 discharges the filtrate out of the storage unit 450. The valves 512, 514, 516 and 518 are connected to the discharge pipe 510.

  When the discharge pipe 510 discharges the filtrate out of the housing portion 450, the possibility that the filtrate is mixed again into the mixture is reduced as compared with the case where the filtrate is not discharged. The possibility of the filtrate entering the supercritical fluid is also reduced. Since the supercritical fluid has solubility, the mixing of the filtrate into the supercritical fluid means that the amount of supercritical fluid required for replacing the liquid component is increased. Decreasing the possibility of increasing the amount of supercritical fluid means increasing the possibility of suppressing the loss of energy consumption. In addition, since the valves 512, 514, 516, and 518 are connected to the discharge pipe 510, the container portion is replaced when the liquid component in the mixture is replaced as compared with the case where the valves 512, 514, 516, and 518 are not connected. The state where the average pressure in 450 is high can be easily maintained. Thereby, since the state where the average pressure in the accommodating part 450 is high can be maintained easily, the pressure which must be added in order to make the gas which was a supercritical fluid into a supercritical fluid again can be made small. Since the pressure to be added can be reduced, the energy for adding the pressure can be reduced. As a result, energy consumption when replacing the liquid component of the mixture with a supercritical fluid can be suppressed.

  Alternatively, it is desirable that the above-described filter extraction unit 452 further includes a partition member 460. A filter medium 462 is attached to the partition member 460. The partition member 460 can move within the housing portion 450. The partition member 460 partitions the inside of the storage portion 450 into a space in which the mixture is stored and a space in which the mixture is prevented from entering. In this case, the pressurizing unit 182 applies pressure to the mixture via the filter extraction unit 452 by applying a force to the partition member 460.

  When the filtration extraction part 452 has the partition member 460, compared with the case where it is not so, after extracting a filtrate from a mixture, the volume of a mixture can be restrained. If the volume of the mixture can be reduced, the amount of supercritical fluid can be reduced during replacement. As a result, energy consumption when replacing the liquid component of the mixture with a supercritical fluid can be suppressed.

  Alternatively, it is desirable that the housing portion 450 described above has a cylindrical portion 480. In this case, the partition member 460 slides inside the accommodating portion 450 along the inner peripheral surface of the cylindrical portion 480.

  According to another aspect of the present invention, the fluid removal method includes a replacement step S332 and a vaporization step S340. The replacement step S332 is a step of replacing the liquid component of the mixture with a supercritical fluid. The mixture includes a solid component and a liquid component. The vaporization step S340 is a step of vaporizing the supercritical fluid. The fluid removal method further includes an extraction step S324. The extraction step S324 is a step of extracting a part of the liquid component from the mixture prior to the replacement step S332.

  By removing a part of the liquid component from the mixture in the extraction step S324 prior to the replacement step S332, the amount of the liquid component replaced by the supercritical fluid can be reduced as compared with the case where it is not. The amount of liquid component to be taken out is not particularly limited. For example, the amount may be an amount such that aggregation does not occur in the solid component in the mixture after the liquid component is removed. Since the amount of liquid component replaced by the supercritical fluid can be reduced, the amount of energy consumed to produce the supercritical fluid can be reduced.

  In addition, the above-described extraction step S324 is desirably a step of extracting a part of the liquid component from the mixture while applying pressure to the mixture in the apparatus 20. In this case, the replacement step S332 includes a step of replacing the liquid component with the supercritical fluid in the apparatus 20.

  When the liquid component is taken out of the mixture, if the pressure is applied to the mixture in the apparatus 20 and the liquid component is replaced with the supercritical fluid in the apparatus 20, the following effects are produced as compared with the case where the liquid component is not replaced. The effect is an effect that, in the replacement step S332, the energy necessary for the supercritical fluid to once become a supercritical state after being no longer a supercritical fluid can be reduced. If the pressure in the device 20 is lower than the pressure of the supercritical fluid, the pressure of the supercritical fluid decreases when the supercritical fluid is flowed into the device 20. When the pressure drops, the supercritical fluid may become a gas. In order to make this gas a supercritical fluid again, it is necessary to apply pressure to at least the gas. The lower the pressure in the device 20, the greater the pressure that must be added to make the gas a supercritical fluid again. When pressure is applied to the mixture in advance, the average pressure in the apparatus 20 can be increased compared to the case where pressure is not applied in advance. If the average pressure in the device 20 is high, the pressure that must be added in order to turn the gas that was a supercritical fluid back into a supercritical fluid will be small. In some cases, the supercritical fluid that has entered the housing portion 450 may not become a gas. If the added pressure is small, the energy for adding the pressure is also small. Since energy consumption for generating the supercritical fluid and energy consumption for adding pressure can be suppressed, the energy consumption when replacing the liquid component of the mixture including the solid component and the liquid component with the supercritical fluid is reduced. Can be suppressed.

  According to the present invention, there is an effect that energy consumption when the liquid component of the mixture is replaced with a supercritical fluid can be suppressed.

It is a figure which shows the structure of the fluid removal system concerning embodiment of this invention. It is a figure which shows the structure of the liquid extraction apparatus concerning embodiment of this invention. It is sectional drawing of the cylinder unit concerning embodiment of this invention. It is a figure which shows the structure of the raw material acceptance unit concerning embodiment of this invention. It is a figure which shows the structure of the purified water supply unit and washing | cleaning liquid supply unit concerning embodiment of this invention. It is a figure which shows the structure of the waste_water | drain primary acceptance unit concerning embodiment of this invention. It is a figure which shows the structure of the carbon dioxide supply apparatus concerning embodiment of this invention. It is a figure which shows the structure of the carbon dioxide reproduction | regeneration apparatus concerning embodiment of this invention. It is a figure which shows the structure of the washing | cleaning liquid reproduction | regeneration apparatus concerning embodiment of this invention. It is a figure which shows the structure of the product acceptance unit concerning embodiment of this invention. It is a figure which shows a structure with the waste_water | drain secondary receiving unit concerning embodiment of this invention. It is a figure which shows the procedure of the fluid removal method concerning embodiment of this invention.

  Hereinafter, the present invention will be described in detail with reference to the drawings. In the following description, the same parts are denoted by the same reference numerals. Their names and functions are also the same. Therefore, detailed description thereof will not be repeated.

<Description of configuration of fluid removal system>
The configuration of the fluid removal system according to the present embodiment will be described with reference to FIG. The fluid removal system according to the present embodiment includes a liquid take-out device 20, a raw material receiving unit 22, a purified water supply unit 24, a cleaning liquid supply unit 26, a waste water primary receiving unit 28, a carbon dioxide supply device 30, and a carbon dioxide supply. A carbon regenerator 32, a cleaning liquid regenerator 34, a chiller unit 36, a product receiving unit 38, and a drainage secondary receiving unit 40 are provided.

  The mixture in the present embodiment refers to a mixture of a solid component and a liquid component. An example of a solid component is a particle. An example of a liquid component is an aqueous solution. However, the solid component and the liquid component are not particularly limited. The liquid extraction device 20 in the present embodiment is a device that extracts a part of the liquid component from the mixture. In the case of this embodiment, a liquid component is taken out from the mixture by filtration. The raw material receiving unit 22 receives a mixture from a well-known hydrothermal synthesizer (not shown). The raw material receiving unit 22 is also a unit that separates the mixture into a supernatant portion and a portion that does not. The supernatant portion is discharged to the drainage secondary receiving unit 40. Thereby, a part of the liquid component of the mixture is removed from the mixture as the supernatant portion is discharged. The mixture from which the supernatant portion has been removed is supplied to the liquid take-out device 20 by the raw material receiving unit 22. The purified water supply unit 24 supplies purified water to the liquid take-out device 20. The purified water supply unit 24 receives the purified water discharged from the liquid take-out device 20. The cleaning liquid supply unit 26 supplies the cleaning liquid to the liquid take-out device 20. In the present embodiment, this cleaning liquid is ethanol. The drainage primary receiving unit 28 receives the used cleaning liquid and the drainage discharged from the liquid take-out device 20. The drainage primary receiving unit 28 discharges the cleaning liquid to the cleaning liquid regenerator 34. The drainage primary receiving unit 28 discharges the drainage to the drainage secondary receiving unit 40 through a flow path (not shown). The carbon dioxide supply device 30 brings carbon dioxide into a supercritical state by heating and pressurization. The carbon dioxide supply device 30 supplies the carbon dioxide in a supercritical state to the liquid take-out device 20. The carbon dioxide regenerator 32 removes the liquid component from the carbon dioxide. This carbon dioxide is discharged from the liquid take-out device 20. The carbon dioxide from which the liquid has been removed is supplied to the carbon dioxide supply device 30. The cleaning liquid regenerator 34 removes impurities from the used cleaning liquid. In this embodiment, the impurities include water and hexylamine. The cleaning liquid from which the impurities are removed is supplied to the cleaning liquid supply unit 26. The cleaning liquid regenerator 34 discharges impurities to the drainage secondary receiving unit 40. The chiller unit 36 supplies cold water. The specific structure of the chiller unit 36 is well known. Therefore, detailed description thereof will not be repeated here. The product receiving unit 38 receives solid components. This solid component is supplied from the liquid take-out device 20. In the case of this embodiment, this solid component becomes a product. The drainage secondary receiving unit 40 includes the supernatant liquid discharged from the raw material receiving unit 22, the drainage discharged from the drainage primary receiving unit 28, the water and hexylamine (water and hexylamine) discharged from the cleaning liquid regenerating device 34. Is separated into two layers, the lower layer is water and the upper layer is hexylamine). The wastewater secondary receiving unit 40 extracts hexylamine from the wastewater and impurities.

<Description of the structure of the liquid take-out device>
With reference to FIG. 2, the liquid extraction device 20 according to the present embodiment will be described. The liquid take-out device 20 according to the present embodiment includes a cylinder unit 180, a pressure pump 182, a purified water supply path check valve 184, a purified water supply path opening / closing valve 186, a purified water discharge path opening / closing valve 188, It has a purified water discharge passage check valve 190, a carbon dioxide discharge passage opening / closing valve 192, a pressure transmitter 194, a carbon dioxide discharge passage pressure reducing valve 196, a carbon dioxide exhaust valve 198, and a carbon dioxide needle valve 200.

  The cylinder unit 180 performs a cleaning process and a drying process on the mixture supplied from the raw material receiving unit 22. Its structure will be described later. The pressurizing pump 182 supplies purified water to the cylinder unit 180. In this embodiment, this purified water is used as a transmission fluid. The transmission fluid in the present embodiment is a fluid for transmitting pressure to the partition member 460 described later. The purified water supply path check valve 184 is provided in the flow path from the purified water supply unit 24 to the cylinder unit 180. The purified water supply path check valve 184 prevents the flow from flowing back. Thereby, purified water flows from the purified water supply unit 24 toward the cylinder unit 180 in the flow path. The purified water supply path opening / closing valve 186 is also provided in the flow path from the purified water supply unit 24 to the cylinder unit 180. The purified water supply passage opening / closing valve 186 opens and closes the passage. The purified water discharge path opening / closing valve 188 is provided in the flow path from the cylinder unit 180 to the purified water supply unit 24. The purified water discharge passage opening / closing valve 188 opens and closes the passage. The purified water discharge path check valve 190 is also provided in the flow path from the cylinder unit 180 to the purified water supply unit 24. The purified water discharge channel check valve 190 prevents the flow from flowing back. Thereby, purified water flows from the cylinder unit 180 toward the purified water supply unit 24 in the flow path. The carbon dioxide discharge path opening / closing valve 192 is provided in the flow path from the cylinder unit 180 to the carbon dioxide regeneration device 32. The carbon dioxide discharge passage opening / closing valve 192 opens and closes the passage. The pressure transmitter 194 detects the pressure in the flow path and thus the pressure in the cylinder unit 180. The carbon dioxide discharge path pressure reducing valve 196 reduces the pressure of carbon dioxide that has passed through the carbon dioxide discharge path opening / closing valve 192. The carbon dioxide exhaust valve 198 is provided in a flow path from the cylinder unit 180 to the outside of the liquid take-out device 20. The carbon dioxide exhaust valve 198 opens and closes the flow path. A carbon dioxide needle valve 200 is also provided in the flow path. The carbon dioxide needle valve 200 adjusts the amount of carbon dioxide released when the carbon dioxide exhaust valve 198 is opened.

  FIG. 3 is a cross-sectional view of the cylinder unit 180 according to the present embodiment. The structure of the cylinder unit 180 according to the present embodiment will be described with reference to FIG. The cylinder unit 180 according to the present embodiment includes a storage unit 450, a filtration extraction unit 452, a transmission fluid pipe 454, a mixture pipe 456, a carbon dioxide supply pipe 458, and a carbon dioxide discharge pipe 459. The storage unit 450 stores the above-described mixture, purified water, and cleaning liquid. The accommodating part 450 accommodates a supercritical fluid with the mixture after filtration of the mixture. In this embodiment, the supercritical fluid is carbon dioxide in a supercritical state. The filter extraction part 452 filters the mixture in the storage part 450. Thereby, the filtration extraction part 452 will take out a liquid component from the mixture. Moreover, the filtration extraction part 452 will leave a solid component in the accommodating part 450. FIG. In addition, the filtration extraction part 452 divides the inside of the accommodation part 450 into a fluid chamber 470 and a mixture chamber 472. The fluid chamber 470 is a space where purified water enters and exits. The fluid chamber 470 does not enter the mixture except for leakage. That is, the fluid chamber 470 is a space in which intrusion of the mixture is suppressed. The mixture chamber 472 is a space where the mixture and the supercritical fluid enter and exit. A cleaning liquid (that is, ethanol in this embodiment) also enters and leaves the mixture chamber 472 for cleaning. The transmission fluid pipe 454 communicates with the fluid chamber 470. The purified water passes through the transmission fluid pipe 454 and flows into the fluid chamber 470 or flows out of the fluid chamber 470. Mixture tube 456 communicates with mixture chamber 472. The mixed fluid flows through the mixture tube 456 and into the mixture chamber 472. The carbon dioxide supply pipe 458 communicates with the mixture chamber 472. The supercritical carbon dioxide passes through the carbon dioxide supply pipe 458 and flows into the mixture chamber 472. The carbon dioxide discharge pipe 459 communicates with the mixture chamber 472 when the liquid component is replaced with the supercritical fluid. Further, the carbon dioxide discharge pipe 459 communicates with the carbon dioxide discharge path opening / closing valve 192. Accordingly, when the liquid component is replaced with the supercritical fluid, the carbon dioxide in the supercritical state flows out of the mixture chamber 472 through the carbon dioxide discharge pipe 459.

  The accommodating part 450 includes a cylindrical part 480, a plug 482, and a sealing ring 484. The cylindrical portion 480 according to the present embodiment is a member having a circular cross section. The tubular part 480 has a bottom part 490 and a mouth part 492. The bottom portion 490 is provided with a mixture passage 494 and a carbon dioxide inflow passage 496. The mixture tube 456 described above communicates with the mixture chamber 472 via the mixture passage 494. That is, the mixture enters and exits from the mixture path 494. The carbon dioxide supply pipe 458 described above communicates with the mixture chamber 472 via the carbon dioxide inflow passage 496. That is, carbon dioxide in a supercritical state flows from the carbon dioxide inflow path 496. Further, the cylindrical portion 480 is provided with a carbon dioxide discharge path 498. The carbon dioxide discharge pipe 459 described above communicates with the inside of the housing portion 450 through the carbon dioxide discharge path 498. That is, supercritical carbon dioxide flows out from the carbon dioxide discharge channel 498. The plug 482 is inserted into the back of the mouth 492 of the tubular portion 480. A tube slide hole 500 is provided at the center of the plug 482. A discharge pipe 510 to be described later passes through the pipe slide hole 500. A seal 502 is formed in the tube slide hole 500. Since the seal 502 is provided, leakage from the gap between the inner peripheral surface of the tube slide hole 500 and the outer peripheral surface of the discharge pipe 510 is suppressed. The plug 482 is also provided with a transmission fluid path 504. The above-described transmission fluid pipe 454 communicates with the fluid chamber 470 through the transmission fluid path 504. That is, purified water enters and exits from the transmission fluid path 504. The sealing ring 484 is an annular member. The transmission fluid pipe 454 and the discharge pipe 510 penetrate therethrough. A male screw is formed on the outer peripheral surface of the sealing ring 484. A female thread is formed on the inner peripheral surface of the mouth 492 of the cylindrical portion 480. The sealing ring 484 is attached to the cylindrical portion 480 by screwing the male screw of the sealing ring 484 into the female screw on the inner peripheral surface of the mouth portion 492 of the cylindrical portion 480 in a state where the plug 482 is accommodated. Since it has such a structure, the discharge pipe 510 penetrates the accommodating portion 450.

  The filter extraction part 452 includes a partition member 460, a filter medium 462, a protective material 464, and a re-mixing prevention part 466. A filter medium 462 is attached to the partition member 460. The partition member 460 slides inside the accommodating portion 450 along the inner peripheral surface of the cylindrical portion 480. The partition member 460 of the filter extraction unit 452 partitions the storage unit 450 into a fluid chamber 470 and a mixture chamber 472. The filter medium 462 filters the mixture in the container 450. The material and structure of the filter medium 462 itself are well known. Therefore, detailed description thereof will not be repeated here. The protective material 464 prevents the filter medium 462 from being damaged by the magnetic stirrer rotor 600 described later. In the case of this embodiment, a hole is provided in the central portion of the protective material 464. The mixture enters the filter outlet 452 through the pores. The re-mixing prevention unit 466 prevents the filtrate from re-mixing into the mixture.

  The re-mixing prevention unit 466 includes a discharge pipe 510, a cleaning liquid supply path check valve 512, a cleaning liquid supply path opening / closing valve 514, a drainage discharge path opening / closing valve 516, and a drainage discharge path check valve 518. The discharge pipe 510 discharges the filtrate out of the storage unit 450. The discharge pipe 510 is attached to the partition member 460. As a result, the discharge pipe 510 moves together with the partition member 460. The discharge pipe 510 communicates with the gap between the filter medium 462 and the partition member 460. As a result, the filtrate that has passed through the filter medium 462 enters the discharge pipe 510. The discharge pipe 510 allows the filtrate to pass through. The cleaning liquid supply path check valve 512 is provided in a flow path from the cleaning liquid supply unit 26 to the cylinder unit 180. The cleaning liquid supply path check valve 512 prevents the flow in the flow path from flowing backward. Accordingly, the cleaning liquid flows from the cleaning liquid supply unit 26 toward the cylinder unit 180 in the flow path. The cleaning liquid supply path opening / closing valve 514 is also provided in the flow path from the cleaning liquid supply unit 26 to the cylinder unit 180. The cleaning liquid supply passage opening / closing valve 514 opens and closes the passage. The drainage discharge path opening / closing valve 516 is provided in a flow path from the cylinder unit 180 to the drainage primary receiving unit 28. The drainage discharge path opening / closing valve 516 opens and closes the flow path. A drainage discharge path check valve 518 is also provided in the flow path from the cylinder unit 180 to the drainage primary receiving unit 28. The drainage discharge path check valve 518 prevents the flow in the flow path from flowing backward. Thereby, the drainage flows from the cylinder unit 180 toward the primary drainage receiving unit 28 in the flow path. The cleaning liquid supply path check valve 512, the cleaning liquid supply path opening / closing valve 514, the drainage discharge path opening / closing valve 516, and the drainage discharge path check valve 518 are connected to the discharge pipe 510. By providing these, the state where the average pressure in the accommodating part 450 is high can be maintained.

  An indicia 520 is attached to the discharge pipe 510. A bracket 530 is attached to the sealing ring 484. A first proximity sensor 540, a second proximity sensor 542, and a third proximity sensor 544 are attached to the bracket 530. When the first proximity sensor 540, the second proximity sensor 542, and the third proximity sensor 544 detect the indicia 520 of the discharge pipe 510, the position of the filtration extraction portion 452 in the housing portion 450 can be detected. In the present embodiment, the position of the third proximity sensor 544 can be arbitrarily set as long as it is between the first proximity sensor 540 and the second proximity sensor 542.

  In this embodiment, a magnetic stirrer rotor 600 is accommodated in the cylinder unit 180. The magnetic stirrer rotor 600 is accommodated in order to prevent precipitation of solid components contained in the mixture. In the present embodiment, the cylinder unit 180 includes two pressure sensors (not shown). One of these pressure sensors detects the pressure inside the fluid chamber 470. The other of these pressure sensors senses the pressure inside the mixture chamber 472.

<Description of the structure of the raw material receiving unit>
FIG. 4 is a diagram showing a configuration of the raw material receiving unit 22 according to the present embodiment. The configuration of the raw material receiving unit 22 according to this embodiment will be described with reference to FIG. The raw material receiving unit 22 includes a raw material receiving tank 210, a stirrer 212, a supernatant discharge passage opening / closing valve 214, a mixture supply pump 216, a mixture supply passage opening / closing valve 218, a mixture discharge passage opening / closing valve 220, and a mixture level. A sensor 222 and a turbidity sensor 224 are included. The raw material receiving tank 210 temporarily stores raw materials. The “raw material” in the present embodiment is the mixture described above. The stirrer 212 stirs the above-mentioned mixture inside the raw material receiving tank 210. Thereby, the mixture after the supernatant is removed will be stirred. The supernatant discharge path opening / closing valve 214 is provided in the flow path from the raw material receiving tank 210 to the drainage secondary receiving unit 40. The supernatant discharge passage opening / closing valve 214 opens and closes the passage. When the supernatant discharge path opening / closing valve 214 is open, the above-described supernatant is discharged to the drainage secondary receiving unit 40. The mixture supply pump 216 supplies the above-described mixture (with the supernatant removed) to the cylinder unit 180. The mixture supply path opening / closing valve 218 is provided in a flow path from the mixture supply pump 216 to the cylinder unit 180. The mixture supply passage opening / closing valve 218 opens and closes the passage. The mixture discharge path opening / closing valve 220 is provided in the flow path from the mixture supply pump 216 to the drainage secondary receiving unit 40. The mixture discharge passage opening / closing valve 220 opens and closes the passage. The mixture level sensor 222 detects the amount of the mixture in the raw material receiving tank 210. The turbidity sensor 224 is disposed in the raw material receiving tank 210 in the vicinity of the supernatant liquid inlet. The turbidity sensor 224 detects the turbidity of the supernatant liquid.

<Description of the configuration of the purified water supply unit>
FIG. 5 is a diagram showing the configuration of the purified water supply unit 24 and the cleaning liquid supply unit 26 according to this embodiment. The configuration of the purified water supply unit 24 will be described with reference to FIG. The purified water supply unit 24 has a purified water storage tank 230. The purified water storage tank 230 stores purified water. This purified water is supplied to the cylinder unit 180.

<Description of configuration of cleaning liquid supply unit>
The configuration of the cleaning liquid supply unit 26 will be described with reference to FIG. The cleaning liquid supply unit 26 includes a cleaning liquid storage tank 240, a cleaning liquid supply pump 242, and a supply path switching valve 244. The cleaning liquid storage tank 240 stores the cleaning liquid. The cleaning liquid supply pump 242 supplies the cleaning liquid to the cylinder unit 180 in principle. In the fluid removal system according to this embodiment, the cleaning liquid supply pump 242 can also supply purified water. The supply path switching valve 244 switches the flow path. By this switching, it is determined whether the cleaning liquid supply pump 242 supplies purified water or cleaning liquid.

<Description of the configuration of the primary drainage receiving unit>
FIG. 6 is a diagram showing the configuration of the drainage primary receiving unit 28 according to the present embodiment. The configuration of the drainage primary receiving unit 28 will be described with reference to FIG. The drainage primary receiving unit 28 includes a drainage storage tank 250, a cleaning drainage storage tank 252, and a receiving path switching valve 254. The drainage storage tank 250 stores purified water that has become wastewater. The cleaning waste water storage tank 252 stores used cleaning liquid. The receiving path switching valve 254 switches the flow path. Thereby, it is determined whether the liquid discharged from the cylinder unit 180 flows into the drainage storage tank 250 or the cleaning drainage storage tank 252.

<Description of configuration of carbon dioxide supply device>
FIG. 7 is a diagram illustrating a configuration of the carbon dioxide supply device 30 according to the present embodiment. The configuration of the carbon dioxide supply device 30 will be described with reference to FIG. The carbon dioxide supply device 30 includes an additional cooler 260, a carbon dioxide supply pump 262, a heating device 264, and a carbon dioxide supply path opening / closing valve 266. The additional cooler 260 cools the carbon dioxide supplied from the carbon dioxide regeneration device 32. The additional cooler 260 cools the carbon dioxide because the carbon dioxide supplied from the carbon dioxide regeneration device 32 removes the heat received from the outside of the flow path (as a result, the carbon dioxide is once liquefied). . The carbon dioxide supply pump 262 applies pressure to the carbon dioxide. The heating device 264 heats carbon dioxide. Thereby, the carbon dioxide is in a supercritical state. The carbon dioxide supply path opening / closing valve 266 is provided in a flow path from the heating device 264 to the cylinder unit 180. The carbon dioxide supply channel opening / closing valve 266 opens and closes this channel.

<Description of configuration of carbon dioxide regenerator>
FIG. 8 is a diagram showing a configuration of the carbon dioxide regeneration device 32 according to the present embodiment. The configuration of the carbon dioxide regeneration device 32 will be described with reference to FIG. The carbon dioxide regeneration device 32 includes a separator 270, a liquefaction cooler 272, a carbon dioxide collector 274, a carbon dioxide replenishment path 276, a drain pressure reducing valve 278, a drain on-off valve 280, and a drain level sensor 282. And have. The separator 270 separates the carbon dioxide discharged from the liquid take-out device 20 into waste water and gaseous carbon dioxide. The liquefier cooler 272 cools the carbon dioxide discharged from the separator 270. Thereby, at least a part of the carbon dioxide is liquefied. The carbon dioxide recovery unit 274 recovers a liquid carbon dioxide discharged from the liquefaction cooler 272. The carbon dioxide replenishment path 276 supplies the liquefied carbon dioxide stored in the gas cylinder 700 in advance to the carbon dioxide collector 274. This replenishes carbon dioxide. The drain pressure reducing valve 278 reduces the pressure of the drainage. The drain opening / closing valve 280 is provided in the flow path from the separator 270 to the cleaning liquid regenerating device 34. The drain opening / closing valve 280 opens and closes the flow path. The drainage level sensor 282 detects the level of drainage in the separator 270. The carbon dioxide replenishment path 276 includes a replenishment path pressure reducing valve 277 and a replenishment path opening / closing valve 279. The replenishment path pressure reducing valve 277 reduces the pressure of the gas cylinder 700. The replenishment path opening / closing valve 279 opens and closes the carbon dioxide replenishment path 276.

<Description of configuration of cleaning liquid regenerating device>
FIG. 9 is a diagram showing a configuration of the cleaning liquid regenerating apparatus 34 according to the present embodiment. The configuration of the cleaning liquid regenerating device 34 will be described with reference to FIG. The cleaning liquid regenerating apparatus 34 includes a distillation apparatus 290, a waste heat utilization oil heat exchanger 292, an electric heat exchanger 294, a viewing window 298, a cold water heat exchanger 300, a cold water passage opening / closing valve 302, and a drain opening / closing valve. 304. The distillation apparatus 290 distills the waste water. As described above, the cleaning liquid according to this embodiment is ethanol. Since the cleaning liquid is ethanol, when the waste water is heated, the ethanol will be distilled. As a result, the cleaning liquid can be regenerated. The waste heat utilization oil heat exchanger 292 supplies high-temperature oil heat (this heat is waste heat generated from the heat source 710) to the distillation apparatus 290. The electric heat exchanger 294 supplies heat obtained from the electric power to the distillation apparatus 290. The viewing window 298 is for a person to look into the ethanol flow path vaporized by distillation. The cold water heat exchanger 300 takes heat from the vaporized ethanol by cold water. As a result, ethanol is liquefied. The cold water used in the cold water heat exchanger 300 is supplied from the chiller unit 36. The cold water channel opening / closing valve 302 opens and closes the ethanol channel. The drain open / close valve 304 is provided in a flow path from the distillation apparatus 290 to the drain secondary receiving unit 40. The drain opening / closing valve 304 opens and closes the flow path.

<Description of configuration of product receiving unit>
FIG. 10 is a diagram showing a configuration of the product receiving unit 38 according to the present embodiment. The configuration of the product receiving unit 38 will be described with reference to FIG. The product receiving unit 38 includes a product receiving tank 310, an exhaust pump 312, a leak valve 314, a product discharge path on / off valve 316, a product receiving path on / off valve 318, and a product level sensor 320. The product receiving tank 310 temporarily stores products. This product is supplied from the product receiving tank 310 to the container 702. The exhaust pump 312 exhausts gas from the product receiving tank 310. The leak valve 314 is provided in a flow path that connects the inside and the outside of the product receiving tank 310. The leak valve 314 opens and closes the flow path. Thereby, air | atmosphere will flow into the inside of the product receiving tank 310 from which the atmospheric pressure fell from the outside. Since the atmosphere flows in, the air pressure inside the product receiving tank 310 becomes equal to the atmospheric pressure. The product discharge path opening / closing valve 316 is provided in a flow path from the product receiving tank 310 to the product discharge port. The product discharge passage opening / closing valve 316 opens and closes the passage. The product receiving path opening / closing valve 318 is provided in a flow path from the cylinder unit 180 to the product receiving tank 310. The product receiving path opening / closing valve 318 opens and closes the flow path. The product level sensor 320 detects the amount of product in the product receiving tank 310.

<Description of the configuration of the secondary drainage receiving unit>
FIG. 11 is a diagram showing a configuration of the drainage secondary receiving unit 40 according to the present embodiment. The structure of the drainage secondary receiving unit 40 will be described with reference to FIG. The drainage secondary receiving unit 40 includes a drainage separation tank 330, a separation water channel opening / closing valve 332, an organic matter storage tank 334, a wastewater storage tank 336, and an organic matter discharge valve 338. The drainage separation tank 330 temporarily stores drainage. In the meantime, an organic substance (hexylamine in the case of this embodiment) is separated from the waste water as a supernatant (in the case of this embodiment, this organic substance is used as a modifier). The separation water channel opening / closing valve 332 is provided in a flow path from the waste water separation tank 330 to the waste water storage tank 336. The separation water channel opening / closing valve 332 opens and closes the channel. Drainage after the supernatant is separated flows through this channel. The organic matter storage tank 334 stores the organic matter (hexylamine) separated as a supernatant in the drainage separation tank 330. The waste water storage tank 336 stores the waste water after the supernatant is separated. The waste water storage tank 336 also stores waste water discharged from the raw material receiving unit 22. The organic matter discharge valve 338 is provided in a flow path from the drainage separation tank 330 to the organic matter storage tank 334. The organic matter discharge valve 338 opens and closes the flow path. Thereby, when the organic matter (hexylamine) is stored in the wastewater separation tank 330, the organic matter separated in the wastewater separation tank 330 can be stored in the organic matter storage tank 334.

<Description of fluid removal method>
FIG. 12 is a diagram illustrating a procedure of the fluid removal method according to the present embodiment. The fluid removal method according to the present embodiment will be described with reference to FIG. Note that the fluid removal system according to the present embodiment requires control. The control may be manual, automatic control by a sequencer or the like, or a combination of manual control and automatic control. In the following description, a case where automatic control by a sequencer (not shown) and manual control are used together will be described.

  In S320, the raw material mixture is discharged from the above-described hydrothermal synthesizer. The mixture flows into the raw material receiving tank 210. At this time, the stirrer 212 is stopped. This is to wait for the solid component of the mixture to settle. Thereafter, the turbidity sensor 224 detects the turbidity of the supernatant liquid. The turbidity sensor 224 transmits a signal indicating the detected turbidity to the sequencer. As a result of sedimentation of the solid component, when the detected turbidity is below a predetermined value (when the supernatant liquid is clear), and when the liquid volume of the mixture is equal to or higher than the predetermined amount (in this case, turbidity) The sequencer controls this so that the supernatant discharge path opening / closing valve 214 opens the flow path. As a result, the supernatant liquid is discharged to the waste water storage tank 336. In parallel with this, the mixture level sensor 222 detects the amount of the mixture in the raw material receiving tank 210. The mixture level sensor 222 transmits a signal indicating the liquid amount of the mixture detected by itself to the sequencer.

  In S322, the sequencer controls the purified water discharge path opening / closing valve 188 to close the flow path. The sequencer controls the purified water supply path opening / closing valve 186 to open the flow path. The sequencer controls the carbon dioxide supply path opening / closing valve 266 to close the flow path. The sequencer controls the carbon dioxide discharge path opening / closing valve 192 to close the flow path. The sequencer controls the carbon dioxide exhaust valve 198 to close the flow path. The sequencer controls the mixture supply path opening / closing valve 218 to close the flow path. The sequencer controls the mixture discharge path opening / closing valve 220 to open the flow path. The sequencer controls the cleaning liquid supply path opening / closing valve 514 to close the flow path. The sequencer controls the drainage discharge path opening / closing valve 516 to open the flow path. The sequencer controls the receiving path switching valve 254 so that the drainage discharge path opening / closing valve 516 and the drainage storage tank 250 can communicate with each other. When these valves are controlled, the sequencer controls the pressurization pump 182 to start. The activated pressurizing pump 182 supplies purified water from the purified water storage tank 230 into the transmission fluid pipe 454 of the cylinder unit 180. The purified water flows into the fluid chamber 470 through the transmission fluid pipe 454. As a result, the air in the fluid chamber 470 is initially released. Thereafter, the filter extraction part 452 is pushed by the purified water and moves toward the bottom part 490 of the cylindrical part 480. Thereafter, when the first proximity sensor 540 detects the indicia 520, the first proximity sensor 540 transmits a signal indicating that to the sequencer. The sequencer that has received the signal controls the pressurizing pump 182 to stop. When the pressurizing pump 182 stops, the movement of the filter take-out part 452 also stops. Thereafter, the sequencer controls the purified water supply path opening / closing valve 186 to close the flow path. When the purified water supply path opening / closing valve 186 is closed, the sequencer controls the agitator 212 to start. When the agitator 212 is activated, the mixture in the raw material receiving tank 210 is agitated. When the agitator 212 is activated, the sequencer controls the mixture supply pump 216 to activate. The sequencer controls the mixture supply path opening / closing valve 218 to open the flow path. The sequencer controls the mixture discharge path opening / closing valve 220 so as to close the flow path. The sequencer controls the purified water discharge path opening / closing valve 188 to open the flow path. The mixture supply pump 216 is activated, the mixture supply path opening / closing valve 218 is opened, the mixture discharge path opening / closing valve 220 is closed, the cleaning liquid supply path opening / closing valve 514 is closed, the drainage discharge path opening / closing valve 516 is opened, and the purified water discharge path When the on-off valve 188 is opened, the mixture in the raw material receiving tank 210 is supplied into the mixture chamber 472 of the cylinder unit 180. A part of the liquid component in the mixture supplied into the mixture chamber 472 passes through the filter medium 462 of the filter extraction unit 452 and moves into the discharge pipe 510. The moved liquid component finally flows into the drainage storage tank 250. The solid component of the mixture remains in the mixture chamber 472 because it is blocked by the filter medium 462. Further, the filter take-out part 452 moves inside the accommodating part 450 by being pushed by the mixture. As a result, the purified water originally in the fluid chamber 470 flows out of the fluid chamber 470 through the transmission fluid pipe 454. The purified water that has flowed out returns to the purified water storage tank 230 via the purified water discharge passage opening / closing valve 188 and the purified water discharge passage check valve 190. When the second proximity sensor 542 detects the indicia 520 as a result of the filter take-out unit 452 approaching the plug 482 of the housing unit 450, the second proximity sensor 542 transmits a signal indicating that to the sequencer. Filtration continues after receiving the signal. When the mixture level sensor 222 reaches a predetermined level, the sequencer controls the drainage discharge path opening / closing valve 516 to close the flow path. The mixture supply pump 216 is controlled to be stopped by a sequencer when a predetermined time has elapsed since the start. In the case of the present embodiment, the magnetic stirrer rotor 600 does not operate until the mixture supply pump 216 starts and stops. This is to promote sedimentation of solid components in the mixture. By facilitating sedimentation, the mixture can be filtered more easily than when sedimentation is not promoted. When the mixture supply pump 216 stops, the sequencer controls the mixture supply path opening / closing valve 218 to close the flow path.

  In S324, the sequencer controls the purified water discharge path opening / closing valve 188 to close the flow path. The sequencer controls the pressurization pump 182 to start. The sequencer controls the purified water supply path opening / closing valve 186 to open the flow path. When the purified water supply passage opening / closing valve 186 is opened, the purified water flows into the fluid chamber 470 through the transmission fluid pipe 454 of the cylinder unit 180. The sequencer controls the drainage discharge path opening / closing valve 516 to open the flow path. The sequencer controls the receiving path switching valve 254 so that the drainage discharge path opening / closing valve 516 and the drainage storage tank 250 can communicate with each other. When the pressure pump 182 supplies purified water, a force is applied to the partition member 460 of the cylinder unit 180. The filtered extraction part 452 to which force is applied moves toward the bottom part 490 of the cylindrical part 480. The mixture is filtered by the filter medium 462 in accordance with the movement of the filter extraction unit 452. The extracted liquid component moves into the discharge pipe 510. The moved liquid component finally flows into the drainage storage tank 250. The filtration removes liquid components from the mixture. At that time, pressure is applied to the mixture via the filter extraction part 452. As the liquid component is taken out, the solid component and a small amount of liquid component remain in the mixture chamber 472. The magnetic stirrer rotor 600 remains stopped after the mixture supply pump 216 is stopped until the mixture is completely filtered. This is to promote sedimentation of the mixture. Thereafter, when the first proximity sensor 540 detects the indicia 520, the first proximity sensor 540 transmits a signal indicating that to the sequencer. The sequencer that has received the signal controls the purified water supply path opening / closing valve 186 to close the flow path. The sequencer controls the pressurizing pump 182 to stop. This ends the filtration of the mixture. As is clear from this description, in the present embodiment, the pressure pump 182 applies pressure to the mixture via the filter extraction unit 452 when the filter extraction unit 452 filters the mixture.

  In S326, the sequencer controls the cleaning liquid supply pump 242 to start. The sequencer controls the cleaning liquid supply path opening / closing valve 514 to open the flow path. In addition, the sequencer controls the drainage discharge path opening / closing valve 516 to close the flow path. The sequencer controls the purified water discharge path opening / closing valve 188 to open the flow path. When the cleaning liquid supply pump 242 is activated, the cleaning liquid supply path on / off valve 514 opens the flow path, the drainage discharge path on / off valve 516 closes the flow path, and the purified water discharge path on / off valve 188 opens the flow path, It flows into the mixture chamber 472 through the discharge pipe 510 of the cylinder unit 180, the filter medium 462, and the protective material 464. Along with this, the filter extraction part 452 is pushed by the cleaning liquid and moves toward the mouth 492 of the cylindrical part 480. At the same time, the sequencer controls the magnetic stirrer rotor 600 to start. Thereby, the mixture after the liquid component is taken out and the cleaning liquid are mixed. Thereafter, when the third proximity sensor 544 detects the indicia 520, the third proximity sensor 544 transmits a signal indicating that to the sequencer. The sequencer that has received the signal controls the cleaning liquid supply pump 242 to stop. When the cleaning liquid supply pump 242 stops, the sequencer controls the cleaning liquid supply path opening / closing valve 514 to close the flow path. The sequencer controls the purified water discharge path opening / closing valve 188 to close the flow path. Thereafter, when a predetermined time elapses after the magnetic stirrer rotor 600 is started, the sequencer controls the magnetic stirrer rotor 600 to stop.

  In S328, the sequencer controls the pressurizing pump 182 to start. The sequencer controls the purified water supply path opening / closing valve 186 to open the flow path. When the purified water supply passage opening / closing valve 186 is opened, the purified water in the purified water storage tank 230 flows into the fluid chamber 470 through the transmission fluid pipe 454 of the cylinder unit 180. The sequencer controls the drainage discharge path opening / closing valve 516 to open the flow path. The sequencer controls the receiving path switching valve 254 so that the drainage discharge path opening / closing valve 516 and the cleaning drainage storage tank 252 communicate with each other. Thereby, the filtration extraction part 452 is pushed by purified water and moves in the direction of the bottom part 490 of the cylindrical part 480. The filter medium 462 filters the fluid in the mixture chamber 472 with the movement of the filter take-out part 452. The cleaning liquid is taken out from the fluid by the filtration. The removed cleaning liquid moves into the discharge pipe 510. The moved cleaning liquid finally flows into the cleaning waste water storage tank 252. Thereafter, when the first proximity sensor 540 detects the indicia 520, the first proximity sensor 540 transmits a signal indicating that to the sequencer. The sequencer that has received the signal controls the pressurizing pump 182 to stop. When the pressurizing pump 182 stops, the sequencer controls the purified water supply path opening / closing valve 186 to close the flow path. Thereby, the process of taking out the cleaning liquid from the fluid in the mixture chamber 472 is completed. By this step, the solid component in the mixture is washed. More specifically, in this step, hexylamine adhering to the surface of the solid component is removed by the cleaning liquid.

  In S330, the sequencer performs a series of controls for once flowing the cleaning liquid into the mixture chamber 472 and taking it out. As is apparent from the above description, this control is aimed at cleaning the solid components in the mixture. Since the specific procedure for this is the same as S326 and S328, detailed description thereof will not be repeated here. In the case of this embodiment, the number of repetitions of the series of control is determined in advance.

  In S332, the sequencer controls the cleaning liquid supply path opening / closing valve 514 to close the flow path. The sequencer controls the drainage discharge path opening / closing valve 516 to close the flow path. The sequencer controls the purified water supply path opening / closing valve 186 to close. The sequencer controls the carbon dioxide exhaust valve 198 to close the flow path. The sequencer controls the mixture discharge path opening / closing valve 220 to close the flow path. The sequencer controls the product receiving path opening / closing valve 318 to close the flow path. The sequencer controls the purified water discharge path opening / closing valve 188 to open the flow path. The sequencer controls the carbon dioxide discharge path opening / closing valve 192 to open the flow path. The sequencer controls the carbon dioxide supply channel opening / closing valve 266 to open the channel. The sequencer controls the chiller unit 36 to start up. When the chiller unit 36 is activated, both the liquefaction cooler 272 and the additional cooler 260 are activated. The sequencer controls the replenishment path opening / closing valve 279 to open the carbon dioxide replenishment path 276. When the replenishment path opening / closing valve 279 opens the carbon dioxide replenishment path 276, the carbon dioxide in the gas cylinder 700 flows into the carbon dioxide supply device 30 through the carbon dioxide replenishment path 276 and the carbon dioxide collector 274. The carbon dioxide flowing into the carbon dioxide supply device 30 enters the additional cooler 260. In the additional cooler 260, the carbon dioxide is cooled. The reason why the carbon dioxide is cooled is that the heat received by the carbon dioxide from the outside before flowing into the carbon dioxide supply device 30 is once removed before entering the carbon dioxide supply pump 262, and the liquid carbon dioxide is reliably sent. Because. When carbon dioxide flows into the carbon dioxide supply device 30, the sequencer controls the carbon dioxide supply pump 262 to start. The carbon dioxide supply pump 262 applies pressure to the carbon dioxide cooled by the additional cooler 260. The carbon dioxide pressurized by the carbon dioxide supply pump 262 is heated by the heating device 264. When pressure is applied and heated, carbon dioxide enters a supercritical state. Carbon dioxide in a supercritical state, that is, the supercritical fluid in the present embodiment flows into the mixture chamber 472 of the cylinder unit 180. When the supercritical fluid flows into the mixture chamber 472, the filter take-out part 452 moves inside the accommodating part 450 by being pushed by the supercritical fluid. Thereby, the purified water originally in the fluid chamber 470 returns to the purified water storage tank 230. At this time, a part of the cleaning liquid remaining in the mixture chamber 472 and a part of hexylamine are dissolved in the supercritical fluid. When the second proximity sensor 542 detects the indicia 520 as a result of the filter take-out unit 452 approaching the plug 482 of the housing unit 450, the second proximity sensor 542 transmits a signal indicating that to the sequencer. The sequencer that has received the signal controls the purified water discharge path opening / closing valve 188 to close the flow path. The carbon dioxide supply pump 262 supplies the supercritical fluid into the cylinder unit 180 even after the purified water discharge passage opening / closing valve 188 is closed. Thereby, the pressure in the mixture chamber 472 gradually increases. The pressure transmitter 194 repeatedly transmits a signal indicating the pressure in the flow path and the pressure in the cylinder unit 180 to the sequencer. The carbon dioxide discharge passage pressure reducing valve 196 depressurizes carbon dioxide containing water, ethanol, and hexylamine. The depressurized carbon dioxide flows into the separator 270. Carbon dioxide becomes a gas inside the separator 270. Within the separator 270, water, ethanol and hexylamine remain liquid. As a result, the gas and the liquid are separated inside the separator 270. The separated gas (carbon dioxide) flows into the liquefaction cooler 272. After reaching such a state, the sequencer continues control for the carbon dioxide supply passage opening / closing valve 266 to open and close the passage for a predetermined time. Meanwhile, the supercritical fluid in the cylinder unit 180 is replaced little by little. The cleaning liquid and hexylamine are dissolved in the supercritical fluid. Thereby, the water | moisture content in a cylinder unit 180, a hexylamine, and a washing | cleaning liquid are removed from a solid component little by little. The water, hexylamine, and cleaning liquid dissolved in the supercritical fluid go out of the cylinder unit 180 together with the supercritical fluid. Thus, the solid component is washed. At the same time, the solid components are dried. The dried solid component becomes the product. In the case of this embodiment, the pressure in the cylinder unit 180 while the supercritical fluid is changed is 25 megapascals. However, the pressure in the cylinder unit 180 is not particularly limited. Similarly, how many Kelvin the heating device 264 raises the temperature of carbon dioxide is not particularly limited. In the case of this embodiment, it is 313 Kelvin (about 40 degrees Celsius) where carbon dioxide is in a supercritical state.

  In S334, when the time during which the carbon dioxide supply path opening / closing valve 266 continues the control for opening and closing the flow path exceeds a predetermined value, the sequencer controls the carbon dioxide supply pump 262 to stop. When the carbon dioxide supply pump 262 stops, the sequencer controls the carbon dioxide discharge path opening / closing valve 192 to close the flow path. The sequencer controls the carbon dioxide supply path opening / closing valve 266 to close the flow path. The sequencer controls the product receiving path opening / closing valve 318 to close the flow path. The sequencer controls the carbon dioxide exhaust valve 198 to open the flow path. When the carbon dioxide exhaust valve 198 opens the flow path, the supercritical fluid in the cylinder unit 180 is discharged out of the liquid extraction device 20 through this. The released supercritical fluid is vaporized. At that time, the discharge speed of the supercritical fluid is adjusted by the carbon dioxide needle valve 200. Thereby, it becomes possible to discharge | release a supercritical fluid slowly. At this time, the product discharge passage opening / closing valve 316 has closed the passage in advance. The sequencer controls the leak valve 314 to close the flow path. The sequencer controls the exhaust pump 312 to activate it. Thereby, the degree of vacuum inside the product receiving tank 310 gradually increases. That is, the atmospheric pressure inside the product receiving tank 310 gradually decreases. When a predetermined time elapses after the exhaust pump 312 is activated, the sequencer controls the product receiving path opening / closing valve 318 so that it opens. Thereby, the product in the cylinder unit 180 is discharged into the product receiving tank 310. The product level sensor 320 detects the amount of product discharged into the product receiving tank 310. The product level sensor 320 transmits a signal indicating the detected amount of product to the sequencer. The sequencer determines whether the product has been sufficiently discharged into the product receiving tank 310 based on the signal. When the product is sufficiently discharged into the product receiving tank 310, the sequencer controls the leak valve 314 to open the flow path. Thus, when the leak valve 314 is opened, the air pressure in the product receiving tank 310 becomes equal to the atmospheric pressure. After the leak valve 314 opens the flow path, the sequencer controls the product discharge path opening / closing valve 316 so that it opens. When the product discharge path opening / closing valve 316 is opened, the product in the product receiving tank 310 is discharged into the container 702.

  In S340, the carbon dioxide that has entered the separator 270 is vaporized. The cleaning solution, hexylamine and water dissolved in carbon dioxide are condensed. Condensed cleaning liquid, water and hexylamine accumulate at the bottom of separator 270.

  In S342, the waste water level sensor 282 detects the water level of the waste water in the separator 270. The drainage level sensor 282 transmits a signal indicating the detected water level to the sequencer. The sequencer controls the drain on / off valve 280 to open the flow path when the water level indicated by the signal exceeds a predetermined value. When the drainage on / off valve 280 opens the flow path, the drainage in the separator 270 flows out to the cleaning liquid regenerator 34. The cleaning liquid regenerator 34 distills the waste water. As a result, a cleaning liquid having a low boiling point is extracted from the waste water. The extracted cleaning liquid flows into the cleaning liquid storage tank 240. As a result, the cleaning liquid can be reused. The cleaning liquid regenerator 34 is provided with a temperature sensor (not shown). The temperature sensor continuously detects the temperature of the waste water. Information indicating temperature is continuously transmitted to the sequencer. When the distillation is completed, the temperature detected by the temperature sensor starts to increase. Therefore, the sequencer determines whether the distillation is completed based on the temperature increase. The end of distillation is realized by controlling the waste heat utilization oil heat exchanger 292 and the electric heat exchanger 294 so that they are stopped. Note that the cleaning liquid collected in the cleaning wastewater storage tank 252 is also reused after being processed by the cleaning liquid regenerator 34 in the same manner.

  In S344, a mixture of water and hexylamine remains in the cleaning liquid regenerator 34. The operator opens the drain opening / closing valve 304 when the mixture is cooled. As a result, the entire amount of the mixture remaining in the cleaning liquid regenerator 34 is discharged to the waste water separation tank 330. In the mixture, water and hexylamine are separated. The lower layer is water. The upper layer is hexylamine. Both have different dielectric constants. Thereby, the boundary part of water and hexylamine is detectable by detecting the dielectric constant of the various places of a mixture using a known electrostatic capacitance type level detection sensor. When the water and hexylamine are separated, the sequencer controls the separated water channel opening / closing valve 332 to open the channel. When the level of the mixture (height from the bottom of the drainage separation tank 330 to the surface of the liquid) falls to a predetermined height after the separation water channel opening / closing valve 332 is opened, the sequencer causes the separation water channel opening / closing valve 332 to flow. This is controlled to close the road. Thereby, water can be discharged | emitted to the wastewater storage tank 336 among the mixtures in the waste_water | drain separation tank 330. FIG. At this time, it may be determined whether or not water has been discharged based on the capacitance detected by the capacitance level detection sensor described above. The waste water discharged in this way may be returned to the hydrothermal synthesizer described above. Thereby, the waste water can be reused as heating water for hydrothermal synthesis. At this time, hexylamine containing water remains in the waste water separation tank 330. The operator opens the organic matter discharge valve 338. As a result, hexylamine in the upper layer of the wastewater separation tank 330 is discharged to the organic matter storage tank 334. Similarly, the wastewater collected in the drainage storage tank 250 is separated into hexylamine separated into layers in the upper layer and water separated into layers in the lower layer.

  In S350, the carbon dioxide vaporized in the separator 270 exits the separator 270. The carbon dioxide exiting the separator 270 flows into the liquefaction cooler 272.

  In S352, the carbon dioxide flowing into the liquefaction cooler 272 is cooled. As a result, the carbon dioxide is liquefied again. The liquefied carbon dioxide flows into the carbon dioxide supply device 30. Thereby, the carbon dioxide can be reused.

<Description of effects>
As described above, according to the liquid take-out device 20 according to the present embodiment, energy consumption can be suppressed by taking out the liquid components of the mixture and applying pressure to the mixture during filtration.

  Further, according to the liquid extraction device 20 according to the present embodiment, the filtration extraction unit 452 includes the filtering material 462 and the re-mixing prevention unit 466, and therefore, the filtrate easily re-mixes into the mixture. As compared with the above, the amount of the mixture after filtration can be reduced. Thereby, energy consumption can be suppressed.

  Further, according to the liquid take-out device 20 according to the present embodiment, the re-mixing prevention unit 466 includes the discharge pipe 510, the cleaning liquid supply path check valve 512, the cleaning liquid supply path opening / closing valve 514, the drainage discharge path opening / closing valve 516, and the drainage discharge path. Since the check valve 518 is provided, the state in which the average pressure in the container 450 is high can be maintained when the liquid component in the mixture is replaced. As a result, energy consumption when replacing the liquid component of the mixture with a supercritical fluid can be suppressed.

  Moreover, since the filtration extraction part 452 concerning this embodiment has the division member 460, after extracting a filtrate from a mixture, the volume of the mixture can be restrained. If the volume of the mixture can be reduced, the amount of supercritical fluid can be reduced during replacement. As a result, energy consumption when replacing the liquid component of the mixture with a supercritical fluid can be suppressed.

  Moreover, since the liquid extraction apparatus 20 concerning this embodiment has the 3rd proximity sensor 544, the quantity of the supercritical fluid used for substitution can be adjusted suitably by adjusting the position. Thereby, the suppression amount of the loss of energy consumption can be adjusted suitably.

  Further, according to the fluid removal system according to the present embodiment, the supernatant is removed prior to the filtration, so that the energy consumed for the filtration can be reduced.

  Moreover, according to the fluid removal method concerning this embodiment, energy consumption can be suppressed by taking out the liquid component of a mixture and applying a pressure to a mixture in the case of filtration.

<Description of modification>
The liquid take-out device described above is illustrated in order to embody the technical idea of the present invention. The liquid take-out device described above can be variously modified within the scope of the technical idea of the present invention.

  For example, the valve connected to the discharge pipe 510 is not limited to that described above. The valve may be, for example, at least one of a throttle valve and a pressure reducing valve. Any of the above-described valves connected to the discharge pipe 510 may not be provided.

  Moreover, the structure of the filter extraction part 452 is not limited to what was mentioned above. What drives the filter extraction part 452 is not limited to the structure as described above. For example, the filter extraction part 452 may be driven by a screw pair. However, it is desirable that what drives the filter extraction part 452 applies pressure to the mixture via the filter extraction part 452 by supplying purified water or other transmission fluid to the inside of the accommodating part 450. In this case, the filter extraction part 452 desirably has a partition member for partitioning the interior of the storage part 450 into a space in which the mixture is stored and a space in which the fluid is stored. Needless to say, the transmission fluid that transmits the pressure to the filter extraction unit 452 is not limited to purified water.

  In addition, the method for applying pressure to the mixture is not limited to that described above. For example, the filter extraction part 452 may be fixed, and the accommodating part 450 may be driven by the movement of the link. In this case, the sealing ring 484 is not always necessary. In this case, the accommodating part 450 is not limited to what is driven by the motion of a link.

  Moreover, the specific kind of on-off valve mentioned above is not limited. Examples of the on-off valve include a ball valve, a gate valve, and a butterfly valve. Examples of the on-off valve include an electric valve and a pneumatic valve (a valve that can be controlled by supplying air).

  In addition, the fluid removal system according to the present invention may remove other liquid organic substances instead of the above-described hexylamine.

  In addition, when the mixture mentioned above contains microparticles | fine-particles as a solid component, the microparticles require a long time for precipitation. In such a case, the amount of the liquid component replaced by the supercritical fluid can be reduced by using the above-described fluid removal system with the following three additional changes. The first of the three points is to provide a well-known dielectric constant detection sensor (not shown) between the discharge pipe 510 and the cleaning liquid supply passage opening / closing valve 514 and the drainage discharge passage opening / closing valve 516. The second point is that a fine particle dispersion tank (not shown) is provided (this fine particle dispersion tank can communicate with the cylinder unit 180 via the discharge pipe 510). The third point is that liquid is discharged from the fine particle dispersion tank to the cylinder unit 180 through the discharge pipe 510 by providing a pump (not shown) (this liquid is discharged from the cylinder unit 180 through the discharge pipe 510, The above-mentioned fine particles are dispersed). When making these changes, it is not necessary to remove the supernatant from the mixture in the raw material receiving tank 210. Hereinafter, a method for cleaning and drying a mixture containing fine particles using the fluid removal system will be described.

  In carrying out this method, first, an additive solution is added to the mixture. The additive liquid has a dielectric constant different from that of the liquid component of the mixture, has a specific gravity different from that of the liquid component of the mixture, and does not dissolve in each other (if the liquid component of the mixture and the additive liquid are left to mix, they are separated into two layers) It is necessary that the solubility is as low as possible). Here, the case where toluene is used as the additive solution will be described. Note that the amount of the additive liquid is reduced compared to the amount of the liquid component. The amount of the additive solution is preferably as small as possible.

  Next, the mixture to which the additive liquid has been added is supplied to the cylinder unit 180. When the mixture is fed, wait. During that time, the mixture is not vibrated as much as possible. Of course, stirring by the magnetic stirrer rotor 600 is not performed. Thereby, the liquid component and additive liquid in a mixture isolate | separate into two layers. The upper layer is a layer of additive liquid (toluene). The lower layer is a layer of liquid component (water). The fine particles dispersed in the mixture gather in the upper layer.

  When the liquid component of the mixture is separated into two layers, the filter extraction unit 452 is driven so that the upper layer (toluene in which fine particles are dispersed) is discharged to the fine particle dispersion tank through the discharge pipe 510. The upper layer discharge destination is the fine particle dispersion tank described above. Since the mixture is separated into two layers, the upper layer is discharged first. By stopping the filter extraction unit 452 immediately before the lower layer (water) is discharged, only the upper layer can be discharged to the fine particle dispersion tank. The filter extraction part 452 can be stopped immediately before the lower layer is discharged by providing a known dielectric constant detection sensor (not shown) between the discharge pipe 510 and the cleaning liquid supply path on / off valve 514 and the drainage discharge path on / off valve 516. Because it is. This dielectric constant detection sensor detects the dielectric constant of the mixture passing through the discharge pipe 510. When the passage of the upper layer is completed and the discharge of the lower layer starts, a large change in the dielectric constant occurs. Accordingly, when a large change in the dielectric constant occurs (for example, when the dielectric constant exceeds a predetermined threshold value), it is possible to discharge only the upper layer by stopping the discharge of the mixture.

  When only the upper layer is discharged from the cylinder unit 180, the lower tank (water) remaining in the cylinder unit 180 is discharged. Although the discharge destination is not particularly limited, the wastewater storage tank 336 is an example. Thereby, the liquid component was taken out from the mixture. Thereafter, the upper layer is returned from the fine particle dispersion tank to the cylinder unit 180.

  When the upper layer returns, the steps after S332 described above are performed. That is, the upper layer is washed with supercritical carbon dioxide and stirred. As a result, the liquid component (in this case, water) is taken out when the fine particles are washed and dried. Since the liquid component can be taken out, the energy spent for cleaning and drying can be reduced.

20 ... Liquid take-out device,
22 ... Raw material receiving unit,
24 ... Purified water supply unit,
26: Cleaning liquid supply unit,
28 ... Drainage primary receiving unit,
30 ... carbon dioxide supply device,
32 ... carbon dioxide regenerator,
34 ... Cleaning liquid regenerating device,
36 ... Chiller unit,
38 ... Product receiving unit,
40 ... Secondary drainage receiving unit,
180 ... cylinder unit,
182: Pressurizing pump,
184 ... purified water supply path check valve,
186 ... purified water supply path on-off valve,
188 ... purified water discharge path on-off valve,
190 ... purified water discharge passage check valve,
192: Carbon dioxide discharge path opening / closing valve,
194 ... Pressure transmitter,
196: Carbon dioxide discharge passage pressure reducing valve,
198 ... CO2 exhaust valve,
200 ... needle valve for carbon dioxide,
210 ... Raw material receiving tank,
212 ... Agitator,
214 ... Supernatant drain opening / closing valve,
216 ... mixture feed pump,
218 ... Mixture supply path opening / closing valve,
220 ... Mixture discharge passage opening / closing valve,
222 ... Mixture level sensor,
224 ... Turbidity sensor,
230 ... purified water storage tank,
240 ... cleaning liquid storage tank,
242 ... Cleaning liquid supply pump,
244 ... Supply path switching valve,
250 ... Drainage tank,
252 ... Washing waste water storage tank,
254 ... Acceptance path switching valve,
260 ... additional cooler,
262 ... carbon dioxide supply pump,
264 ... heating device,
266 ... Carbon dioxide supply path opening / closing valve,
270 ... separator,
272 ... Liquefaction cooler,
274: Carbon dioxide collector,
276 ... carbon dioxide replenishment path,
277 ... Reducing passage pressure reducing valve,
278 ... Pressure reducing valve for drainage,
279 ... replenishment path opening / closing valve,
280 ... Drain open / close valve,
282: Waste water level sensor,
290 ... distillation apparatus,
292 ... waste heat oil heat exchanger,
294 ... Electric heat exchanger,
298 ... Peeping window,
300 ... cold water heat exchanger,
302 ... cold water on-off valve,
304 ... Drain open / close valve,
310 ... Product receiving tank,
312 ... exhaust pump,
314 ... Leak valve,
316 ... Product discharge path on-off valve,
318 ... Product receiving path on-off valve,
320 ... Product level sensor,
330: Waste water separation tank,
332: Separate water channel opening / closing valve,
334 ... Organic storage tank,
336: Waste water storage tank,
338 ... Organic discharge valve,
450 ... accommodating part,
452 ... Filtration extraction part,
454 ... Transmission fluid pipe,
456 ... Mixture tube,
458 ... carbon dioxide supply pipe,
459 ... carbon dioxide exhaust pipe,
460 ... partition member,
462: Filter material,
464 ... protective material,
466 ... Re-mixing prevention unit,
470 ... Fluid chamber,
472 ... the mixture chamber,
480 ... cylindrical portion,
482 ... Plug,
484 ... sealing ring,
490 ... the bottom,
492 ... Mouth,
494 ... mixture path,
496 ... carbon dioxide inflow path,
498 ... carbon dioxide emission path,
500 ... Tube slide hole,
502 ... Seal,
504 ... a transmission fluid path,
510 ... discharge pipe,
512 ... cleaning liquid supply path check valve,
514 ... Cleaning liquid supply passage opening / closing valve,
516: Drain discharge passage opening / closing valve,
518 ... Drain discharge check valve,
520 ...
530 ... Bracket,
540 ... 1st proximity sensor,
542 ... second proximity sensor,
544 ... Third proximity sensor,
600 ... Magnetic stirrer rotor,

Claims (7)

A liquid take-out device for taking out a part of the liquid component from a mixture containing a solid component and a liquid component,
A housing for housing the mixture and the supercritical fluid;
Filtering out the liquid component from the mixture by filtering the mixture in the container; and
A liquid extraction apparatus comprising: a pressure unit that applies pressure to the mixture when the filter extraction unit filters the mixture. The filter take-out part is
A filter medium for filtering the mixture in the container;
2. The liquid according to claim 1, further comprising a re-mixing prevention unit configured to prevent re-mixing of the filtrate, which is the liquid component extracted from the mixture by the filter medium, into the mixture. Take-out device. The re-mixing prevention unit is
A discharge pipe for discharging the filtrate to the outside of the storage unit;
The liquid take-out device according to claim 2, further comprising a valve connected to the discharge pipe. A partition member for partitioning the filter take-out section into a space in which the filter medium is attached and which can move in the storage section, and into which the mixture is stored and a space in which the mixture is prevented from entering; Have
The liquid extraction device according to claim 2, wherein the pressure unit applies the pressure to the mixture through the filtration extraction unit by applying a force to the partition member. The accommodating portion has a cylindrical portion;
The liquid extraction device according to claim 4, wherein the partition member slides in the storage portion along an inner peripheral surface of the cylindrical portion. Replacing the liquid component of the mixture comprising the solid component and the liquid component with a supercritical fluid;
A fluid removal method comprising a vaporization step of vaporizing the supercritical fluid,
The fluid removal method further includes a removal step of extracting a part of the liquid component from the mixture prior to the replacement step. The removal step is a step of removing a part of the liquid component from the mixture while applying pressure to the mixture in an apparatus;
The fluid removing method according to claim 6, wherein the replacing step includes a step of replacing the liquid component with the supercritical fluid in the apparatus.

Images