JP5567449B2 - Component extraction method - Google Patents

Description

The present invention, example varying the predetermined material to any of the supercritical fluid or subcritical, after extracting a predetermined component from a contained object using any of the fluid, the fluid supercritical or sub The present invention relates to a component extraction method for returning to a material before becoming critical.

  A fluid supply channel for supplying a supercritical carbon dioxide cleaning fluid; a cleaning channel for circulating the carbon dioxide cleaning fluid; a cleaning container for receiving the carbon dioxide cleaning fluid connected to the channels; and a fluid supply channel There is a cleaning device formed by a booster pump installed, a circulation pump installed in a cleaning channel, and a filtration filter installed in a cleaning channel extending downstream of the cleaning container (see Patent Document 1). The booster pump raises the carbon dioxide flowing into the cleaning container to a predetermined temperature and increases the pressure to a predetermined pressure. The circulation pump circulates the cleaning fluid through the cleaning flow path while maintaining a constant pressure of the carbon dioxide cleaning fluid flowing inside the cleaning container during the cleaning of the object to be cleaned. The filtration filter filters impurities contained in the cleaning fluid. Since this cleaning apparatus circulates the supercritical carbon dioxide cleaning fluid through the cleaning flow path and cleans the object to be cleaned contained in the cleaning container, the cleaning time of the object to be cleaned can be shortened. In addition, by installing the filter in the cleaning flow path, fine impurities contained in the cleaning fluid can be removed, and the cleaning fluid can be kept clean.

JP-A-8-206485

  The cleaning system disclosed in the above publication uses a booster pump to change carbon dioxide to a supercritical carbon dioxide cleaning fluid, supplies the fluid from a fluid supply channel to the cleaning container, and uses the fluid to clean the cleaning container. It is necessary to return the fluid to carbon dioxide after cleaning the object to be cleaned housed inside. In order to return the cleaning fluid to carbon dioxide, it is necessary to depressurize the fluid at a constant depressurization rate to atmospheric pressure, but during the depressurization of the fluid, the temperature of the fluid drops all at once and the inside of the cleaning container becomes negative temperature. There is a case. If the temperature inside the cleaning container becomes negative while the cleaning fluid is depressurized, the object to be cleaned is exposed to a severe temperature environment, causing damage to the object to be cleaned, and the object to be cleaned may be damaged during the process of depressurizing the fluid. is there. In addition, during the depressurization of the cleaning fluid, the fluid may return to the carbon dioxide through the gas-liquid mixing region, and when the cleaning fluid passes through the gas-liquid mixing region, the carbon dioxide is frozen during the depressurization of the fluid and the cleaning container Dry ice may be generated inside. When dry ice is generated inside the cleaning container, the decompression operation must be interrupted until the dry ice disappears, and it takes a long time to return the cleaning fluid to carbon dioxide. Cannot be performed and the number of cleanings cannot be increased.

An object of the present invention is to change a predetermined substance into either a supercritical or subcritical fluid, extract a predetermined component from the contained material using either of the fluids, It is another object of the present invention to provide a component extraction method for returning to a material before becoming subcritical, and an object of the present invention is to supercritical or subcritical fluids without supercritical or subcritical fluid damage. It is an object of the present invention to provide a component extraction method capable of returning to a substance before becoming.

  A feature of the component extraction method according to the present invention is a hermetic container having a predetermined volume for containing an object containing a predetermined component, and a vacuum separation installed after the hermetic container and connected to the hermetic container via the first conduit. Unit, recovery supply unit installed after the decompression separation unit and connected to the decompression separation unit via the first conduit, and booster pump installed after the recovery supply unit and connected to the recovery supply unit via the first conduit And a heater installed after the booster pump and connected to the booster pump via the first pipeline, and a first pump line extending between the hermetic container and the vacuum separation unit, A second pipe connected to the first pipe extending in between, and a circulation pump installed in the second pipe, and using a booster pump and a heater to raise the temperature and pressure of a predetermined substance, Supercritical or After the fluid is introduced into the hermetic container and the components contained in the contained material are extracted, the fluid is introduced into the first pipeline and the fluid is introduced into the second pipeline using a circulation pump. Then, while heating the fluid to a predetermined temperature using a heater, the fluid is decompressed using a vacuum separation unit to return the fluid to a substance.

  As an example of the component extraction method of the present invention, in the component extraction method, the flow rate of the circulation pump is larger than that of the booster pump, and when the fluid is depressurized, the flow rate of the fluid that flows into the second pipe using the circulation pump More than the flow rate of the fluid flowing into the first conduit, and the fluid is circulated through a circulation route that passes through the hermetic vessel, the circulation pump, and the heater, and the fluid is decompressed to a substance using a decompression separation unit. Return and collect the material using the recovery supply unit.

  As another example of the component extraction method of the present invention, in the component extraction method, when the fluid is decompressed, the fluid decompression time is divided into a plurality of times, and the fluid is decompressed stepwise in a decompression range set for each decompression time. To do.

  As another example of the component extraction method of the present invention, in the component extraction method, when the fluid is decompressed, the decompression time in the vicinity of the critical point of the fluid is more than the decompression time other than the critical point and the vicinity thereof. It is long.

  As another example of the component extraction method of the present invention, in the component extraction method, when the fluid is decompressed, the fluid returns from the critical region to the substance through the gas phase region.

  As another example of the component extraction method of the present invention, the component extraction method branches from a second pipeline extending between the circulation pump and the heater, and the first pipeline extends between the heater and the airtight container. When the fluid is depressurized, the fluid is circulated to the circulation route passing through the hermetic container, the circulation pump, and the heater, and the fluid is passed through the hermetic container and the circulation pump via the bypass line. Circulate to the bypass route.

  According to the component extraction method of the present invention, a predetermined substance is heated and pressurized using a booster pump and a heater, the substance is changed to a supercritical or subcritical fluid, and the fluid is allowed to flow into an airtight container. After extracting the components contained in the object to be contained, the fluid is allowed to flow into the first conduit, the fluid is allowed to flow into the second conduit using a circulation pump, and the fluid is heated to a predetermined temperature using a heater. Since the fluid is decompressed using the decompression separation unit while being heated to return the fluid to the substance, the fluid flowing into the second pipe during the decompression of the fluid is heated by the heater, and the fluid temperature during the decompression of the fluid The extraction of components contained in the containment using the fluid can be prevented, and the inside of the airtight container can be prevented from having a negative temperature while keeping the fluid at a predetermined temperature. The fluid becomes supercritical or subcritical It can be returned to the material. In the component extraction method, the inside of the hermetic container does not become minus temperature in the process of decompressing the fluid, and the contained object is not exposed to a severe temperature environment. Can be returned to the material before becoming supercritical or subcritical.

  Fluid whose flow rate of the circulation pump is larger than that of the booster pump and when the supercritical or subcritical fluid is depressurized, the flow rate of the fluid that flows into the second pipeline using the circulation pump is allowed to flow into the first pipeline The fluid is circulated through a circulation route that passes through the hermetic container, the circulation pump, and the heater, while the fluid is decompressed using the decompression separation unit and returned to the substance, and the recovery supply unit is utilized. A component extraction method for recovering a substance uses a circulation pump and a heater by flowing a fluid having a flow rate larger than the flow rate of the fluid flowing into the first pipeline using a circulation pump. While a large amount of fluid is heated, the fluid is decompressed using the decompression separation unit, so that the fluid is surely heated by the heater during decompression of the fluid, and the fluid temperature is rapidly decreased during decompression of the fluid. Prevent After extracting the components contained in the containment using the fluid, the fluid is kept in a supercritical or subcritical state while preventing the inside of the hermetic container from becoming a negative temperature while maintaining the fluid at a predetermined temperature. You can return to the material before it became critical. In the component extraction method, the inside of the hermetic container does not become minus temperature in the process of decompressing the fluid, and the contained object is not exposed to a severe temperature environment. Can be returned to the material before becoming supercritical or subcritical.

  The component extraction method in which the pressure reduction time of a supercritical or subcritical fluid is divided into a plurality of time periods and the fluid is reduced stepwise by the pressure reduction width set for each pressure reduction time. If the fluid is continuously depressurized within a certain depressurization range, the density of the fluid changes greatly in a short time, and the temperature of the fluid may drop at a stretch and the inside of the hermetic container may become negative temperature. Since the pressure is reduced step by step with the pressure reduction range set every hour, the density change of the fluid can be moderated, and the temperature of the fluid does not decrease at a stretch during the pressure reduction of the fluid. After extracting the components contained in the product, return the fluid to the material before becoming supercritical or subcritical while preventing the inside of the hermetic container from becoming negative temperature while keeping the fluid at a predetermined temperature. Can do. In the component extraction method, the inside of the hermetic container does not become minus temperature in the process of decompressing the fluid, and the contained object is not exposed to a severe temperature environment. Can be returned to the material before becoming supercritical or subcritical.

  When a supercritical or subcritical fluid is depressurized, the component extraction method in which the depressurization time in the vicinity of the critical point of the fluid is longer than other depressurization times excluding the critical point and the vicinity thereof is the critical point. The fluid density changes drastically at and near the critical point.If the fluid is depressurized in the short time at the critical point and in the vicinity thereof, the fluid density greatly changes in a short time, the temperature of the fluid drops rapidly, and the inside of the airtight container Although the temperature may be negative, the fluid is depressurized step by step within the depressurization range set for each depressurization time, so the density change of the fluid can be moderated, and the temperature of the fluid is reduced all at once After the components contained in the containment are extracted using the fluid, the fluid is kept at a predetermined temperature while preventing the inside of the airtight container from becoming a negative temperature, Super critical It can be returned to the previous material to be subcritical. In the component extraction method, the inside of the hermetic container does not become minus temperature in the process of decompressing the fluid, and the contained object is not exposed to a severe temperature environment. Can be returned to the material before becoming supercritical or subcritical.

  During the depressurization of a supercritical or subcritical fluid, the component extraction method in which the fluid returns from the critical region to the substance through the gas phase region is performed when the fluid returns to the substance through the gas-liquid mixing region. When the fluid freezes and dry ice is generated inside the hermetic container, if dry ice is generated inside the hermetic container, the decompression operation must be interrupted until the dry ice disappears. Although it takes a long time to return to the material before becoming critical or subcritical, the fluid returns from the critical region to the material through the gas phase region, so that dry ice is not generated inside the hermetic container, and the fluid The decompression of the fluid can be continued without interrupting the decompression of the fluid, and the fluid can be returned to the substance in a short time. Since this component extraction method can quickly return the fluid to the substance after extracting the components contained in the object to be contained, the number of component extractions per unit time can be increased.

  When a supercritical or subcritical fluid is depressurized, including a bypass line branched from a second line extending between the circulation pump and the heater and connected to a first line extending between the heater and the hermetic vessel In the component extraction method, the fluid is circulated to the circulation route passing through the hermetic container, the circulation pump, and the heater, and the fluid is circulated to the bypass route passing through the hermetic container and the circulation pump via the bypass pipe. By circulating the fluid not only in the circulation route but also in the bypass route at the time of depressurization, the temperature of the fluid can be adjusted more quickly than in the case where the temperature of the fluid is adjusted only by the heater. After the components contained in the contained material are extracted using the fluid, the inside of the airtight container becomes a negative temperature with the fluid held at a predetermined temperature. While preventing the door can be returned to the previous material comprising the fluid in a supercritical or subcritical.

The block diagram of the fluid production | generation apparatus shown as an example. The flowchart which shows an example of the procedure from washing | cleaning operation to pressure reduction operation. The flowchart explaining an example of a pressure reduction means. The figure which shows an example of the flow of the cleaning fluid at the time of pressure reduction. The figure which shows an example of the relationship between a pressure reduction width and pressure reduction time. The Mollier diagram which shows the relationship between a pressure (MPa) and enthalpy (kj / kg). The figure which shows an example of the relationship between the pressure change at the time of depressurizing, heating a cleaning fluid, and a temperature change. The figure which shows an example of the relationship between the pressure change at the time of decompressing without heating a cleaning fluid, and a temperature change. The figure which shows another example of the flow of the carbon dioxide at the time of pressure reduction.

The details of the component extraction method according to the present invention will be described with reference to the accompanying drawings such as FIG. 1 which is a configuration diagram of a fluid generating apparatus shown as an example. The component extraction method of the present invention and the fluid generating apparatus 10 used in this method are used to clean a used air filter (contained object) (contained object) after filtering gas (extraction of dirt components (impurities)). It is preferably used for cleaning (extracting dirt components (impurities)) of a used liquid filter (contained object) (contained object) after the liquid has been filtered. For cleaning these filters, carbon dioxide (substance) (note that the substance may be in a gas state, a liquid state, or a gas-liquid mixed state) is heated to a predetermined temperature and pressure. Either a supercritical or subcritical cleaning fluid (fluid) obtained by is used.

  Examples of the air filter to be cleaned include a separator type air filter and a mini-pleat type air filter. The air filter is mainly used as an air conditioning filter, an air cleaning filter, an exhaust treatment filter, or a vehicle air filter. A liquid filter as an object to be cleaned is used as a filter for a water purifier or a filter for a membrane device using osmotic pressure. Air filters and liquid filters are used by being housed in a filter cartridge using glass fibers, adsorbents, and synthetic resin fibers as filter media. These filters have a quadrangular prism-like three-dimensional structure folded into a bellows. In addition, the filter cleaned by this apparatus 10 includes a substantially flat filter in addition to that having a three-dimensional structure, and further includes a columnar or polygonal column.

  Either supercritical or subcritical cleaning fluids have the properties of gas and liquid, easily enter the fine gaps of the filter media forming the air filter or liquid filter, and dissolve impurities adhering to the filter media surface. At the same time, it penetrates into the filter medium and dissolves the impurities that have penetrated into the filter medium. By using the cleaning fluid, not only can the impurities attached to the surface of the filter medium be removed, but also the impurities that have penetrated into the filter medium can be removed.

The objects to be cleaned by this component extraction method include not only filters but also all objects to be cleaned that can be cleaned by supercritical and subcritical cleaning fluids. In addition, supercritical and subcritical fluids easily enter the containment and penetrate into the object (containment) to dissolve the components contained in the object. Thus, components contained in the object can be extracted. Therefore, this component extraction method not only cleans the filter, but also extracts a predetermined component from the object such as extracting caffeine (component) from coffee beans (object) or nicotine from tobacco. It can also be used when extracting. In this component extraction method , the object (contained object) from which the component is extracted is not particularly limited, and includes all objects from which the component can be extracted by a supercritical or subcritical fluid.

In this component extraction method , a predetermined volume of the cleaning container 11 (airtight container) (note that the cleaning container 11 (airtight container) has a volume of 100 liters or more), the vacuum separation unit 12, and the recovery It is composed of a supply unit 13, a booster pump 14, a heater 15, a circulation pump 16, and a controller 17. The cleaning container 11, the decompression / separation unit 12, the recovery supply unit 13, the booster pump 14, and the heater 15 are connected via a first pipe 18. The cleaning container 11, the heater 15, and the circulation pump 16 are connected via a first pipe line 18 and a second pipe line 19. An airtight structure cleaning chamber (not shown) is formed in the cleaning container 11.

  Although not shown, the cleaning container 11 is provided with a temperature sensor and a pressure sensor. The temperature sensor and the pressure sensor are connected to the controller 17 via an interface (wired or wireless) (not shown). The temperature sensor measures the temperature of the outlet of the cleaning container 11. The measured temperature of the outlet of the cleaning container 11 is input to the controller 17 from the temperature sensor. The pressure sensor measures the pressure inside the cleaning container 11. The measured pressure inside the cleaning container 11 is input to the controller 17 from the pressure sensor.

  The vacuum separation unit 12 is installed after the airtight container 11 and is connected to the airtight container 11 via the first pipe line 18. Although not shown, the decompression / separation unit 12 is formed of a pressure control valve, a gas-liquid separator, and a filter. The pressure control valve, the gas-liquid separator, and the filter are connected via the first pipe line 18.

  The pressure control valve can adjust the pressure of carbon dioxide or the cleaning fluid inside the cleaning container 11 by changing the opening of the valve mechanism, and can open and close the cleaning container 11 by opening and closing the valve mechanism. The 1st pipe line 18 extended between liquid separators can be opened and closed. The pressure control valve is connected to the controller 17 via an interface (not shown). The opening degree of the valve mechanism of the pressure control valve is input from the pressure control valve to the controller 17. The controller 17 outputs an opening setting signal for the valve mechanism of the pressure control valve to the pressure control valve.

  The gas-liquid separator of the vacuum separation unit 12 separates impurities contained in the cleaning fluid from the cleaning fluid using the difference in vapor pressure of the impurities. A recovery tank (not shown) is attached to the gas-liquid separator. The gas-liquid separator is connected to the controller 17 via an interface (not shown). The internal temperature and internal pressure of the gas / liquid separator are input to the controller 17 from the gas / liquid separator. Impurities (liquid) separated by the gas-liquid separator are collected in the collection tank.

  When the cleaning fluid that has flowed out of the gas-liquid separator contains a small amount of impurities, the filter of the vacuum separation unit 12 removes (filters) the impurities and purifies the cleaning fluid. The filter is formed of a housing, a filter, and a filter cartridge that fixes the filter. In the filtration apparatus, after the filter is attached to the filter cartridge, the cartridge is attached to the housing. It is preferable to use a porous material such as activated carbon for the filter used in the filter.

  The recovery supply unit 13 is installed after the vacuum separation unit 12 and is connected to the vacuum separation unit 12 via the first pipe line 18. Although not shown, the recovery supply unit 13 is formed of a liquefier (cooler and condenser), a pressure control valve, and a buffer tank, and a liquefied carbon dioxide storage tank is attached. The liquefier, the pressure control valve, and the buffer tank are connected via the first pipe line 18.

  The pressure control valve can adjust the pressure of the cleaning fluid inside the liquefier by changing the opening of the valve mechanism, and it can be opened and closed between the liquefier and the buffer tank by opening and closing the valve mechanism. The extending first pipe line 17 can be opened and closed. The pressure control valve is connected to the controller 17 via an interface (not shown). The opening degree of the valve mechanism of the pressure control valve is input from the pressure control valve to the controller 17. The controller 17 outputs an opening setting signal for the valve mechanism of the pressure control valve to the pressure control valve.

  The liquefier of the recovery supply unit 13 cools and condenses the cleaning fluid to return it to liquefied carbon dioxide, and the buffer tank temporarily stores the liquefied carbon dioxide. The liquefier and the buffer tank are connected to the controller 17 via an interface (not shown). The controller 17 outputs a liquefier output setting signal (cooling temperature setting signal) to the liquefier. The controller 17 outputs a carbon dioxide supply amount setting signal for the buffer tank to the buffer tank.

  Although not shown, the liquefied carbon dioxide storage tank is connected to the buffer tank via a spare line. The liquefied carbon dioxide storage tank stores liquefied carbon dioxide, and supplies the liquefied carbon dioxide to the buffer tank at the start of cleaning. Further, liquefied carbon dioxide is recovered after the operation of the apparatus 10 is completed. A transfer pump (not shown) is installed in the preliminary pipeline. The transfer pump is connected to the controller 17 via an interface (not shown). The controller 17 outputs a transfer pump output setting signal to the transfer pump.

  The booster pump 14 is installed after the recovery supply unit 13 and is connected to the recovery supply unit 13 via the first pipe 18. The booster pump 14 boosts the carbon dioxide supplied from the recovery supply unit 13 (buffer tank) to a predetermined pressure. The heater 15 is installed after the booster pump 14 and is connected to the booster pump 14 via the first pipe line 18. The heater 15 heats carbon dioxide to a predetermined temperature. The booster pump 14 and the heater 15 are connected to the controller 17 via an interface (not shown). The controller 17 outputs an output setting signal of the booster pump 14 to the booster pump 14 and outputs an output setting signal (heating temperature) of the heater 15 to the heater 15.

  A shutoff valve 27 and a flow meter 20 for measuring the flow rate of carbon dioxide and cleaning fluid flowing therethrough are installed in the first pipeline 18 extending between the booster pump 14 and the heater 15. The shut-off valve 27 can open and close the first pipe line 18 by opening and closing its valve mechanism. The shutoff valve 27 and the flow meter 20 are connected to the controller 17 via an interface (not shown). The opening degree of the valve mechanism of the cutoff valve 27 is input from the cutoff valve 27 to the controller 17. The controller 17 outputs an opening setting signal for the valve mechanism of the shutoff valve 27 to the shutoff valve 27. A flow rate signal (flow rate of the booster pump) of the first pipeline 18 is input from the flow meter 20 to the controller 17.

  A first pipe 18 extending between the heater 15 and the cleaning container 11 is provided with a flow meter 21 for measuring the flow rate of carbon dioxide and cleaning fluid flowing therethrough. The flow meter 21 is connected to the controller 17 via an interface (not shown). The flow rate signals of the first and second pipes 18 and 19 (flow rates of the booster pump 14 and the circulation pump 16) are input from the flow meter 21 to the controller 17.

  The circulation pump 16 is installed in a second pipeline 19 branched from the first pipeline 18. The circulation pump 16 is connected to the controller 17 via an interface (not shown). The controller 17 outputs an output setting signal of the circulation pump 16 to the circulation pump 16. The circulation pump 16 has a larger flow rate per unit time than that of the booster pump 14 per unit time. The second pipe line 19 branches from the first pipe line 18 that extends between the hermetic container 11 and the vacuum separation unit 12 and is connected to the first pipe line 18 that extends between the booster pump 14 and the heater 15. .

A flow meter 22 for measuring the flow rate of carbon dioxide and cleaning fluid flowing therethrough is installed in the second pipe line 19 extending between the circulation pump 16 and the heater 15. The flow meter 22 is connected to the controller 17 via an interface (not shown).
A flow rate signal of the second pipe line 19 (flow rate of the circulation pump 16) is input from the flow meter 22 to the controller 17. A bypass pipeline 23 is installed in the second pipeline 19. The bypass line 23 branches from a second line 19 that extends between the circulation pump 16 and the heater 15, and is connected to a first line 18 that extends between the heater 15 and the airtight container 11.

  A switching valve 24 is installed in the second pipeline 19 that extends between the first pipeline 18 and the circulation pump 16. A switching valve 25 is installed in the second pipe line 19 extending between the circulation pump 16 and the heater 15. A switching valve 26 is installed in the bypass line 23. The switching valves 24 to 26 can adjust the flow rate of the cleaning fluid flowing through the second pipeline 19 and the bypass pipeline 23 by adjusting the opening degree of the valve mechanism. Moreover, the 2nd pipe line 19 and the bypass pipe line 23 can be opened and closed by opening and closing the valve mechanism, and the path | route of a carbon dioxide or a cleaning fluid can be changed. These switching valves 24 to 26 are connected to the controller 17 via an interface (not shown). The opening degrees of the valve mechanisms of the switching valves 24 to 26 are input to the controller 17 from the switching valves 24 to 26. The controller 17 outputs opening degree setting signals of the valve mechanisms of the switching valves 24 to 26 to the switching valves 24 to 26.

  In this fluid generator 10, the hermetic container 11 → the decompression / separation unit 12 → the recovery supply unit 13 → the booster pump 14 → the heater 15 forms the first route, and the hermetic container 11 → the circulation pump 16 → the heater 15 is the second. In addition to forming a route (circulation route), the hermetic container 11 → the circulation pump 16 forms a third route (bypass route). Those devices forming the first route are connected via the first pipeline 18, and those devices forming the second route are connected via the first and second pipelines 18 and 19. The devices forming the third route are connected via the first and second pipelines 18 and 19 and the bypass pipeline 23.

  The controller 17 is a computer including a central processing unit (CPU or MPU) and a memory. In the filter cleaning, the controller 17 repeatedly executes an operation cycle of temperature increase / decrease / cleaning / depressurization. The central processing unit of the controller 17 starts an application stored in the memory based on control by the operating system, and executes the following means according to the application. The central processing unit of the controller 17 executes fluid generation means for converting carbon dioxide into a supercritical or subcritical cleaning fluid, and executes component extraction means for extracting dirt components (impurities) contained in the filter to be cleaned. Then, the depressurizing means for depressurizing the cleaning fluid flowing into the cleaning container 11 to the atmospheric pressure after a predetermined time has elapsed since the execution of the component extracting means is executed.

  The controller 17 includes the temperature of the liquefier, the amount of carbon dioxide supplied from the buffer tank and the carbon dioxide storage tank, the output of the booster pump 14 and the circulation pump 16, the output of the heater 15, the pressure control valve and the switching valves 24 to 26, and the cutoff. The opening degree of the valve 27 is monitored. Based on the measurement results output from the temperature sensor, the pressure sensor, and the flow sensors 20 to 22, the controller 17 supplies the carbon dioxide supply amount, the temperature and output of those devices, the pressure control valve, the switching valves 24 to 26, and the cutoff valve 27. Control the opening of. Although not shown, the controller 17 is connected to an input device such as an ON / OFF switch and a key unit, and an output device such as a printer and a display via an interface.

  FIG. 2 is a flowchart illustrating an example of a procedure from the cleaning operation to the decompression operation in the fluid generating device 10. First, a cleaning operation pattern is selected using the controller 17 (S-10), and a reduced pressure operation pattern is selected (S-11). The cleaning operation pattern includes a first cleaning operation pattern for circulating the cleaning fluid in the first route, a second cleaning operation pattern for circulating the cleaning fluid in the first route and the second route (circulation route), and the second route. There are a third cleaning operation pattern for circulating the cleaning fluid, and a fourth cleaning operation pattern for circulating the cleaning fluid in the second route and the third route (bypass route). In the selection of the cleaning operation pattern, one of the first to fourth cleaning operation patterns is selected using the input device of the controller 17. The controller 17 stores the selected cleaning operation pattern in the memory.

  The depressurization operation pattern includes a first depressurization operation pattern for depressurizing the cleaning fluid using the first route and the second route, and a first depressurizing operation for the cleaning fluid using the first route, the second route, and the third route. There are two decompression operation patterns. In the selection of the decompression operation pattern, the input device of the controller 17 is used to select one of the first and second decompression operation patterns, and the number of segments of decompression time in the selected decompression operation pattern is input. Enter the decompression time and decompression range (decompression value). The controller 17 stores the selected decompression operation pattern, the number of sections, the decompression time, and the decompression width in the memory.

  The controller 17 extracts the selected cleaning operation pattern from the memory, and operates the apparatus 10 with the operation pattern. In the washing operation, the carbon dioxide supplied from the buffer tank is heated to a predetermined temperature by the booster pump 14 and the heater 15 and is increased to a predetermined pressure (note that the valve of the pressure control valve of the vacuum separation unit 12). The opening of the mechanism is adjusted, thereby adjusting the pressure of carbon dioxide). The controller 17 confirms that the measured temperature from the temperature sensor or pressure sensor attached to the cleaning container 11 and the measured pressure have increased the temperature of the carbon dioxide to the set temperature and the set pressure (the temperature increase pressure increase time has elapsed). After) (S-12), the cleaning operation is started (S-13). Carbon dioxide is pressurized to a pressure in the range of 5.0 to 30.0 MPa by the booster pump 14, heated to a temperature of 30 to 50 ° C. by the heater 15, and cleaned either supercritical or subcritical. It turns into a fluid.

  In the case of the first cleaning operation pattern in which the cleaning fluid is circulated in the first route, the controller 17 opens the valve mechanism of the pressure control valve of the decompression separation unit 12 and the recovery supply unit 13 and opens the valve mechanism of the shut-off valve 27. At the same time, after the valve mechanisms of the switching valves 24 to 26 are closed, the cleaning fluid is forcibly supplied to the cleaning container 11 by the booster pump 14, and the cleaning operation is started (S-13). The cleaning fluid flows into the airtight structure cleaning chamber of the cleaning container 11 and cleans the filter accommodated in the cleaning chamber. In this cleaning operation, the cleaning fluid circulates through the first route by the booster pump 14.

  In the first route, the cleaning fluid flows from the cleaning container 11 through the first pipeline 18 into the vacuum separation unit 12 and from the vacuum separation unit 12 through the first pipeline 18 into the recovery supply unit 13. It flows into the booster pump 14 from the recovery supply unit 13 through the first pipe 18. Furthermore, it flows into the heater 15 from the booster pump 14 through the first pipe 18, and again flows into the cleaning container 11 from the heater 15 through the first pipe 18. The cleaning fluid removes dirt components contained in the filter (component extraction means). The soil component is mixed into the cleaning fluid.

  In the vacuum separation unit 12, the cleaning fluid flows into the gas-liquid separator and also flows from the gas-liquid separator to the filter. In the vacuum separation unit 12, the dirt component (impurities) contained in the cleaning fluid is separated by the gas-liquid separator or the filter, and the dirt component separated from the cleaning fluid is collected in the collecting device. In the recovery supply unit 13, the cleaning fluid flows from the liquefier into the buffer tank. During the cleaning operation of the filter, the controller 17 maintains the cleaning fluid circulating in the first route at a constant temperature while maintaining the heating temperature of the heater 15 at the set temperature.

  In the case of the second cleaning operation pattern in which the cleaning fluid is circulated in the first and second routes, the controller 17 opens the valve mechanisms of the pressure control valves of the decompression separation unit 12 and the recovery supply unit 13, and the switching valves 24, 25, After opening the valve mechanism of the shutoff valve 27 and closing the valve mechanism of the switching valve 26, the cleaning fluid is forcibly supplied to the cleaning container 11 by the booster pump 14 and the circulation pump 16, and the cleaning operation is started (S). -13). The cleaning fluid flows into the airtight structure cleaning chamber of the cleaning container 11 and cleans the filter accommodated in the cleaning chamber. In this cleaning operation, the cleaning fluid circulates in the first route by the booster pump 14 and circulates in the second route by the circulation pump 16.

  In the first route, the cleaning fluid flows from the cleaning container 11 through the first pipeline 18 into the vacuum separation unit 12 and from the vacuum separation unit 12 through the first pipeline 18 into the recovery supply unit 13. It flows into the booster pump 14 from the recovery supply unit 13 through the first pipe 18. Furthermore, it flows into the heater 15 from the booster pump 14 through the first pipe 18, and again flows into the cleaning container 11 from the heater 15 through the first pipe 18.

  In the vacuum separation unit 12, the cleaning fluid flows into the gas-liquid separator and also flows from the gas-liquid separator to the filter. In the vacuum separation unit 12, the dirt component (impurities) contained in the cleaning fluid is separated by the gas-liquid separator or the filter, and the dirt component separated from the cleaning fluid is collected in the collecting device. In the recovery supply unit 13, the cleaning fluid flows from the liquefier into the buffer tank.

  In the second route, the cleaning fluid flows from the cleaning container 11 through the first pipeline 18 and the second pipeline 19 into the circulation pump 16, and from the circulation pump 16 through the second pipeline 19 and the first pipeline 18. After flowing into the heater 15, it flows again from the heater 15 through the first pipe line 18 into the cleaning container 11. The flow rate per unit time of the cleaning fluid passing through the circulation pump 16 is larger than that per unit time of the cleaning fluid passing through the booster pump 14, and the amount of the cleaning fluid circulating in the second route circulates in the first route. More than that of the cleaning fluid. During the filter cleaning operation, the controller 17 maintains the cleaning fluid circulating in the first route and the second route at a constant temperature while maintaining the heating temperature of the heater 15 at the set temperature.

  In the case of the third cleaning operation pattern in which the cleaning fluid is circulated in the second route, the controller 17 opens the valve mechanisms of the switching valves 24 and 25, closes the valve mechanism of the shutoff valve 27, and valve mechanism of the switching valve 26. Then, the cleaning fluid is forcibly supplied to the cleaning container 11 by the circulation pump 16 and the cleaning operation is started (S-13). The cleaning fluid flows into the airtight structure cleaning chamber of the cleaning container 11 and cleans the filter accommodated in the cleaning chamber. In the third cleaning operation pattern, the cleaning fluid is circulated through the second route by the circulation pump 16. The controller 17 circulates a large amount of cleaning fluid per unit time in the second route.

  In the second route, the cleaning fluid flows from the cleaning container 11 through the first pipeline 18 and the second pipeline 19 into the circulation pump 16, and from the circulation pump 16 through the second pipeline 19 and the first pipeline 18. After flowing into the heater 15, it flows again from the heater 15 through the first pipe line 18 into the cleaning container 11. During the filter cleaning operation, the controller 17 maintains the cleaning fluid circulating in the second route at a constant temperature while maintaining the heating temperature of the heater 15 at the set temperature.

  In the case of the fourth cleaning operation pattern in which the cleaning fluid is circulated in the second route and the third route, the controller 17 opens the valve mechanism of the switching valves 24 to 26 and closes the valve mechanism of the shutoff valve 27, and then the circulation pump. 16 forcibly supplies the cleaning fluid to the cleaning container 11 and starts the cleaning operation (S-13). The cleaning fluid flows into the airtight structure cleaning chamber of the cleaning container 11 and cleans the filter accommodated in the cleaning chamber. In this cleaning operation, the cleaning fluid circulates through the second route and the third route by the circulation pump 16. The controller 17 circulates a large amount of cleaning fluid per unit time in the second route and the third route.

  In the second route, the cleaning fluid flows from the cleaning container 11 through the first pipeline 18 and the second pipeline 19 into the circulation pump 16, and from the circulation pump 16 through the second pipeline 19 and the first pipeline 18. After flowing into the heater 15, it flows again from the heater 15 through the first pipe line 18 into the cleaning container 11. Further, in the third route, the cleaning fluid flows from the cleaning container 11 through the first pipeline 18 and the second pipeline 19 into the circulation pump 16, and from the circulation pump 16 through the bypass pipeline 23 and the first pipeline 18. It passes through the washing container 11 again. The cleaning fluid removes dirt components contained in the filter (component extraction means). The soil component is mixed into the cleaning fluid. During the filter cleaning operation, the controller 17 controls the mixing ratio of the cleaning fluid circulating in the second and third routes while maintaining the heating temperature of the heater 15 at the set temperature, and maintains the cleaning fluid at a constant temperature. .

  During the cleaning operation of the filter, the flow rate of carbon dioxide flowing through each route is input from the flow meters 20 to 22 to the controller 17, and the temperature and pressure of the cleaning container 11 are input from the temperature sensor and the pressure sensor. During the filter cleaning operation, the controller 17 executes the feedback control while the cleaning container 11, the decompression separation unit 12, the recovery supply unit 13, the booster pump 14, and the circulation pump 16 are in the optimum operation state (the filter is most efficiently cleaned). In a possible state). In the cleaning operation, the controller 17 adjusts the flow rate (output) of the booster pump 14 and the circulation pump 16 to adjust the flow rate of the cleaning fluid flowing through the first to third routes, and the inflow amount of the cleaning fluid into the cleaning container 11. And the outflow amount from the cleaning container 11 is adjusted. In addition, the controller 17 adjusts the valve mechanism of the pressure control valve of the decompression / separation unit 12 to adjust the pressure of the cleaning fluid flowing through the first to third routes, and adjust the pressure of the cleaning fluid flowing into the cleaning container 11. To do.

  When a predetermined time (cleaning time) has elapsed since the start of the cleaning operation (S-14), the controller 17 determines that the cleaning has been completed (S-15). When it is determined that the cleaning is completed, the controller 17 starts a pressure reduction operation (pressure reduction means) for reducing the cleaning fluid flowing into the cleaning container 11 to atmospheric pressure (pressure reduction means) (S-16). In the decompression operation, the cleaning fluid is decompressed and cooled by the pressure control valve of the decompression / separation unit 12, condensed and cooled by the liquefier of the recovery supply unit 13, returned to liquefied carbon dioxide (substance), and stored in the buffer tank. When it is confirmed that the predetermined time has elapsed from the start of the decompression operation and the pressure inside the cleaning container 11 has become atmospheric pressure (S-17), the controller 17 determines that the decompression has been completed (S-18). ). When the fluid generation unit, the component extraction unit, and the decompression unit are completed, one cleaning cycle is completed.

  FIG. 3 is a flowchart for explaining an example of the decompression means, and FIG. 4 is a diagram showing an example of the flow of the cleaning fluid during decompression. FIG. 5 is a diagram illustrating an example of the relationship between the decompression width and the decompression time. FIG. 4 shows a first decompression operation pattern in which the cleaning fluid is decompressed using the first and second routes. Based on FIGS. 3 to 5, an example of the decompression means executed by the fluid generation device 10 will be described as follows. After the cleaning of the filter is completed, the controller 17 performs a depressurization operation (decompression unit) of the cleaning fluid according to the first depressurization operation pattern shown in FIG.

  In the decompression operation, the controller 17 extracts the selected decompression operation pattern (first decompression operation pattern) from the memory, extracts the input number of sections, decompression time, decompression width (decompression value) from the memory, and decompression time. And the opening degree (first to third set opening degrees) of the pressure control valve of the pressure reduction separation unit 12 corresponding to the pressure reduction width is extracted from the memory. The controller 17 sets the number of sections, the decompression time, and the decompression width in the first decompression operation pattern (S-30), and sets the decompression route corresponding to the first decompression operation pattern (S-31).

  In the first decompression operation pattern, as shown in FIG. 5, the time from the start of decompression to the end of decompression (total decompression time) is divided into three stages (first decompression time t1 to third decompression time t3). The pressure is reduced stepwise by a pressure reduction range (pressure reduction value) set for each pressure reduction time t1 to t3. For example, in the first decompression time t1, the cleaning fluid is decompressed to 20 MPa to 10 MPa (depressurization width (decompression value): 10 MPa) between the start of decompression and 30 minutes. In the second depressurization time t2, the cleaning fluid is depressurized to 10 MPa to 8 MPa (depressurization width (decompression value): 2 MPa) from the end of the first depressurization time t1 to 40 minutes. In the third decompression time t3, the cleaning fluid is decompressed to 8 MPa to 2.0 MPa (decompression width (decompression value): 6 MPa) within 30 minutes from the end of the second decompression time t2.

  The second decompression time t2 is a decompression time in the vicinity of the critical point of the cleaning fluid, and is longer than the first decompression time t1 and the third decompression time t3. In the first decompression operation pattern, the total decompression time from the start of decompression to the end of decompression is divided into three stages, but the number of sections of the total decompression time is not limited to three stages, and the total decompression time is 4 It may be divided into more stages. Even when the total depressurization time is divided into four or more stages, it is preferable that the depressurization time in the vicinity of the critical point of the cleaning fluid is longer than other depressurization times excluding the critical point and the vicinity thereof.

  The controller 17 adjusts the valve mechanism of the pressure control valve of the decompression separation unit 12 to the first set opening (the first decompression time t1 and the opening corresponding to the decompression width at the time t1) (S-32). Open the valve mechanism of the pressure control valve. The controller 17 opens the valve mechanisms of the switching valves 24 and 25 and closes the valve mechanisms of the switching valve 26 and the shutoff valve 27. Furthermore, the operation of the booster pump 14 is stopped, and the circulation pump 16 is continuously operated (when the cleaning is performed only in the first route, the circulation pump 16 is operated) (S-33). The controller 17 sets the depressurization route of the cleaning fluid in the first depressurization operation pattern to the first and second routes (S-34).

  In the first depressurization operation pattern, the cleaning fluid flows into the first route (route indicated by arrow L1) as shown by arrows L1 and L2 in FIG. 4, and the second route (route indicated by arrow L2) by the circulation pump. Is circulated (S-34). The controller 17 maintains the valve mechanism of the pressure control valve at the first set opening during the first pressure reduction time t1. In the first reduced pressure operation pattern, the flow rate of the fluid circulated to the second route using the circulation pump 16 is made larger than the flow rate of the fluid flowing into the first route.

  In the second route, the cleaning fluid flows from the cleaning container 11 through the first pipeline 18 and the second pipeline 19 into the circulation pump 16, and from the circulation pump 16 through the second pipeline 19 and the first pipeline 18. After flowing into the heater 15, it flows again from the heater 15 through the first pipe line 18 into the cleaning container 11. In this apparatus 10, the cleaning fluid circulating through the second route through the circulation pump 16 circulates through the second route while being heated to a predetermined temperature by the heater 15 (S-35), and the portion of the cleaning fluid is circulated during the circulation. A fixed amount of fluid gradually flows into the first route, which has a lower pressure than the second route.

  The cleaning fluid that has flowed into the first route flows from the cleaning container 11 through the first pipeline 18 into the vacuum separation unit 12 and from the vacuum separation unit 12 through the first pipeline 18 into the recovery supply unit 13. . The cleaning fluid flowing into the first route is depressurized and cooled by the pressure control valve of the depressurization separation unit 12 (S-36), condensed and cooled by the liquefier of the recovery supply unit 13, and returned to liquefied carbon dioxide. Stored in buffer tank.

  When the first pressure reduction time t1 elapses and the first pressure reduction time t1 ends (S-37), the controller 17 moves the valve mechanism of the pressure control valve of the pressure reduction separation unit 12 to the second set opening (second pressure reduction time t2). And the opening degree corresponding to the reduced pressure width at time t2) (S-38). The cleaning fluid that circulates through the second route through the circulation pump 16 circulates through the second route while being heated to a predetermined temperature by the heater 15 (S-39), as in the first decompression time t1. A predetermined amount of the fluid gradually flows into the first route having a pressure lower than that of the second route.

  The controller 17 holds the valve mechanism of the pressure control valve at the second set opening during the second pressure reduction time t2. The cleaning fluid flows into the first route while circulating through the second route, is depressurized and cooled by the pressure control valve of the depressurization separation unit 12 (S-40), and is condensed and cooled by the liquefier of the recovery supply unit 13. Then, it returns to liquefied carbon dioxide and is stored in the buffer tank.

  When the second decompression time t2 elapses and the second decompression time t2 ends (S-41), the controller 17 moves the valve mechanism of the pressure control valve of the decompression separation unit 12 to the third set opening (third decompression time t3). And the opening degree corresponding to the decompression width at time t3) (S-42). The cleaning fluid circulating through the second route through the circulation pump 16 circulates through the second route while being heated to a predetermined temperature by the heater 15 as in the first decompression time t1 and the second decompression time t2 (S -43), a predetermined amount of the fluid gradually flows into the first route having a lower pressure than the second route during the circulation.

  The controller 17 holds the valve mechanism of the pressure control valve at the third set opening degree during the third pressure reduction time t3. The cleaning fluid flows into the first route while circulating through the second route, is depressurized and cooled by the pressure control valve of the depressurization separation unit 12 (S-44), and is condensed and cooled by the liquefier of the recovery supply unit 13. Then, it returns to liquefied carbon dioxide and is stored in the buffer tank. When the first to third pressure reduction times t1 to t3 have elapsed and the pressure in the cleaning container 11 input from the pressure sensor has become atmospheric pressure, the controller 17 determines that the pressure reduction has ended, and the operation of the apparatus 10 Pause.

  Although not shown, the cleaning fluid may be decompressed without heating using only the first route. In this case, the controller 17 opens the valve mechanisms of the pressure control valves of the decompression separation unit 12 and the recovery supply unit 13, closes the valve mechanisms of the switching valves 24 to 26 and the shutoff valve 27, and operates the booster pump 14. Stop. The cleaning fluid flows into the low-pressure separation unit 12 having a low pressure, is decompressed and cooled by the pressure control valve of the decompression separation unit 12, is condensed and cooled by the liquefier of the recovery supply unit 13, and returns to liquefied carbon dioxide. Stored in buffer tank.

  FIG. 6 is a Mollier diagram showing the relationship between pressure (MPa) and enthalpy (kj / kg). FIG. 7 is a diagram illustrating an example of a relationship between a pressure change and a temperature change when the cleaning fluid is depressurized while being heated, and FIG. 8 is a pressure change and a temperature change when the cleaning fluid is depressurized without being heated. FIG. In FIG. 6, the pressure change of the fluid when the cleaning fluid is depressurized without heating the cleaning fluid (without using the second route) is indicated by a dotted line, and the cleaning fluid is heated (using the second route). D) The change in pressure of the fluid when the cleaning fluid is depressurized is indicated by a one-dot chain line.

  In the first decompression operation pattern, the cleaning fluid returns from the critical region to the carbon dioxide gas (substance) through the gas phase region during the decompression, as indicated by a one-dot chain line in FIG. When only the first route is used and the pressure is reduced without using the second route, as shown by the dotted line in FIG. 6, the criticality that is the boundary between the supercritical region and the gas phase region (liquid phase region) is obtained. At and near the point, the cleaning fluid returns to the carbon dioxide gas (substance) through the gas-liquid mixing region.

  When the cleaning fluid is depressurized while being heated in the fluid generating device 10 or the component extraction method that performs the first decompression operation pattern, the temperature of the fluid does not decrease to the vicinity of the critical point of the cleaning fluid and the fluid is high as shown in FIG. The temperature inside the cleaning container 11 (the temperature of the cleaning fluid) when the pressure inside the cleaning container 11 (airtight structure cleaning chamber) (pressure of the cleaning fluid) reaches atmospheric pressure is about 12 Held at ℃. When the cleaning fluid is depressurized while being heated in the first decompression operation pattern, the inside of the cleaning container 11 does not become minus temperature, and the filter accommodated in the cleaning container 11 (airtight structure cleaning chamber) is severe. There is no exposure to temperature.

  On the other hand, when the cleaning fluid is decompressed using only the first route without heating, as shown in FIG. 8, the pressure drop in the cleaning container 11 (airtight structure cleaning chamber) (pressure reduction of the cleaning fluid) The temperature inside the cleaning container 11 (the temperature of the cleaning fluid) decreases substantially in synchronization with the internal pressure of the cleaning container 11 when the pressure inside the cleaning container 11 (the pressure of the cleaning fluid) reaches atmospheric pressure ( The temperature of the airtight structure cleaning chamber (the temperature of the cleaning fluid) has dropped to about −5 ° C. When the pressure is reduced without heating the cleaning fluid using only the first route, the temperature inside the cleaning container 11 becomes negative, and the filter housed in the cleaning container 11 (airtight structure cleaning chamber) is severe. You will be exposed to a temperature environment.

  In the fluid generating device 10 and the component extraction method for performing the first decompression operation pattern shown in FIG. 4, the supercritical or subcritical cleaning fluid (fluid) is extracted after extracting the dirt component (component) contained in the filter (contained object). ) Into the first route, the fluid is caused to flow into the second route using the circulation pump 16, the fluid is heated to a predetermined temperature using the heater 15, and the fluid is used using the pressure control valve. Since the pressure of the fluid is reduced, the fluid temperature can be prevented from suddenly decreasing during the decompression of the fluid, and the inside of the cleaning container 11 (airtight structure cleaning chamber) does not become a negative temperature, and the fluid is maintained at a predetermined temperature. In the state, the cleaning fluid can be returned to liquefied carbon dioxide (substance).

  In the fluid generator 10 and the component extraction method, the temperature inside the cleaning container 11 (airtight structure cleaning chamber) does not become negative in the process of depressurizing the cleaning fluid, and the filter is not exposed to a severe temperature environment. The cleaning fluid can be returned to liquefied carbon dioxide without damaging the filter. In the fluid generation device 10 and the component extraction method, the circulation pump 16 is used to flow a fluid having a flow rate larger than the flow rate of the cleaning fluid that flows into the first route into the second route. Since a large amount of cleaning fluid is heated by using the fluid, the fluid can be reliably heated by the heater 15 during the decompression of the cleaning fluid, and a sudden drop in the fluid temperature during the decompression of the fluid can be reliably prevented. Can do.

  When depressurizing the cleaning fluid, if the fluid is continuously depressurized with a constant depressurization width, the density of the fluid greatly changes in a short time, and the temperature of the fluid is lowered at a stretch, and the inside of the cleaning container 11 (airtight structure cleaning chamber) However, in this fluid generating device 10 and component extraction method, when the cleaning fluid is decompressed, the fluid decompression time is divided into first to third decompression times t1 to t3. Since the pressure is reduced stepwise by the pressure reduction range (pressure reduction value) set every 1st to 3rd pressure reduction times t1 to t3, the change in the density of the fluid can be moderated, and the temperature of the fluid rapidly increases during the pressure reduction of the fluid. The cleaning fluid can be returned to the liquefied carbon dioxide while preventing the inside of the cleaning container 11 from having a negative temperature while keeping the fluid at a predetermined temperature without decreasing.

  When the fluid density changes drastically between the critical point and the vicinity thereof, and the fluid is depressurized in a short time at the critical point and the vicinity thereof, the density of the fluid greatly changes in a short time, and the temperature of the fluid is lowered at a stretch and the washing container 11 However, the fluid generating device 10 and the component extraction method can reduce the pressure reduction time (first step) in the vicinity of the critical point of the fluid when the pressure of the cleaning fluid is reduced. 2) The pressure reduction time t2) is longer than other pressure reduction times (first and third pressure reduction times t1, t3) excluding the critical point and the vicinity thereof, so that the density change of the fluid can be moderated. While the pressure of the fluid is reduced, the temperature of the fluid does not rapidly decrease, and the cleaning fluid is returned to the liquefied carbon dioxide while preventing the inside of the cleaning container 11 from becoming a negative temperature while maintaining the fluid at a predetermined temperature. It is possible.

  When the cleaning fluid returns to the substance through the gas-liquid mixing region during the decompression operation, the carbon dioxide is frozen during the decompression of the cleaning fluid, and dry ice may be generated inside the cleaning container 11 (airtight structure cleaning chamber). Yes, when dry ice is generated inside an airtight container, the decompression operation must be interrupted until the dry ice disappears, and before the fluid is returned to carbon dioxide (substance) before becoming supercritical or subcritical. Although it takes a long time, in the fluid generating apparatus 10 and the component extraction method, when the fluid is decompressed, the fluid returns from the critical region to the carbon dioxide through the gas phase region, so that dry ice is generated inside the cleaning container 11. The pressure reduction of the fluid can be continued without interrupting the pressure reduction of the fluid, and the fluid can be returned to carbon dioxide in a short time. Since the fluid generating apparatus 10 and the component extraction method can quickly return the cleaning fluid to carbon dioxide after cleaning the filter, the number of cleanings per unit time (the number of component extractions) can be increased.

  FIG. 9 is a diagram illustrating another example of the flow of the cleaning fluid (carbon dioxide) during decompression. FIG. 9 shows a second decompression operation pattern in which the cleaning fluid is decompressed using the first to third routes. While referring to FIGS. 3 and 5, another example of the decompression means executed by the fluid generation device 10 will be described based on FIG. 9 as follows. After the cleaning is completed, the controller 17 performs the pressure reduction operation (pressure reduction means) of the cleaning fluid according to the second pressure reduction operation pattern shown in FIG.

  In the decompression operation, the controller 17 extracts the selected decompression operation pattern (second decompression operation pattern) from the memory, extracts the inputted number of sections, decompression time, decompression width (decompression value) from the memory, and decompression time. And the opening degree (first to third set opening degrees) of the pressure control valve of the pressure reduction separation unit 12 corresponding to the pressure reduction width is extracted from the memory. The controller 17 sets the number of sections, the decompression time, and the decompression width in the second decompression operation pattern (S-30), and sets the decompression route corresponding to the second decompression operation pattern (S-31).

  In the second depressurization operation pattern, as in the first depressurization operation pattern, the total depressurization time from the start of depressurization to the end of depressurization is divided into three stages (first depressurization time t1 to third depressurization time t3), The pressure is reduced stepwise by the pressure reduction width set for each pressure reduction time t1 to t3 (in FIG. 5). In the second depressurization operation pattern, the first depressurization time t1 (depressurization from 20 MPa to 10 MP, depressurization width (decompression value): 10 MPa) from the start of depressurization to 30 minutes is second from the end of the first depressurization time t1 to 40 minutes. The pressure reduction time t2 (decompression from 10 MPa to 8MP, decompression width (decompression value): 2 MPa) and the third decompression time t3 (decompression from 8 MPa to 2.0MP, decompression width) from the end of the second decompression time t2 to 30 minutes (Reduced pressure value): 6 MPa). The second decompression time t2 is a decompression time in the vicinity of the critical point of the cleaning fluid, and is longer than the first decompression time t1 and the third decompression time t3. In the second decompression operation pattern, the total decompression time from the start of decompression to the end of decompression is divided into three stages, but the total decompression time may be divided into four or more stages.

  The controller 17 adjusts the valve mechanism of the pressure control valve of the decompression separation unit 12 to the first set opening (the opening corresponding to the first decompression time t1 and the decompression width of that time) (S-32), Open the valve mechanism of the control valve. The controller 17 opens the valve mechanism of the switching valves 24, 25, and 26 and closes the valve mechanism of the shut-off valve 27. Further, the operation of the booster pump 14 is stopped and the circulation pump 16 is operated (S-33). The controller 17 sets the depressurization route of the cleaning fluid in the second depressurization operation pattern to the first to third routes (S-34).

  In the second reduced pressure operation pattern, the cleaning fluid flows into the first route (route indicated by arrow L1) as shown by arrows L1, L2, and L3 in FIG. The route shown) and the third route (route shown by arrow L3) are circulated (S-34). The controller 17 holds the valve mechanism of the pressure control valve of the decompression / separation unit 12 at the first set opening for the first decompression time t1. In the second decompression operation pattern, the flow rate of the fluid circulated to the second route and the third route using the circulation pump 16 is larger than the flow rate of the fluid flowing into the first route.

  In the second pressure reducing operation pattern, the controller 17 adjusts the valve opening degree of the switching mechanisms 25 and 26 to adjust the flow rate of the cleaning fluid flowing into the second route and the flow rate of the cleaning fluid flowing into the third route. Thus, the mixing ratio of the cleaning fluid circulating through the second route and the third route is controlled, and the cleaning fluid is quickly adjusted to the set temperature. Specifically, when the flow rate of the cleaning fluid flowing into the second route is the same as the flow rate of the cleaning fluid flowing into the third route, the flow rate of the cleaning fluid flowing into the second route flows into the third route. When the flow rate is higher than the flow rate of the cleaning fluid, the flow rate of the cleaning fluid flowing into the third route may be set higher than the flow rate of the cleaning fluid flowing into the second route.

  In the second route, the cleaning fluid flows from the cleaning container 11 through the first pipeline 18 and the second pipeline 19 into the circulation pump 16, and from the circulation pump 16 through the second pipeline 19 and the first pipeline 18. After flowing into the heater 15, it flows again from the heater 15 through the first pipe line 18 into the cleaning container 11. Further, in the third route, the cleaning fluid flows from the cleaning container 11 through the first pipeline 18 and the second pipeline 19 into the circulation pump 16, and from the circulation pump 16 through the bypass pipeline 23 and the first pipeline 18. It passes through the washing container 11 again.

  In the fluid generation device 10, the cleaning fluid circulates through the third route via the circulation pump 16, circulates through the second route, and the cleaning fluid circulated through the second route is heated to a predetermined temperature by the heater 15. While circulating the route (S-35), a predetermined amount of the fluid gradually flows into the first route having a lower pressure than the second route and the third route during the circulation.

  The cleaning fluid that has flowed into the first route flows from the cleaning container 11 through the first pipeline 18 into the vacuum separation unit 12 and from the vacuum separation unit 12 through the first pipeline 18 into the recovery supply unit 13. . The cleaning fluid flowing into the first route is depressurized and cooled by the pressure control valve of the depressurization separation unit 12 (S-36), condensed and cooled by the liquefier of the recovery supply unit 13, and returned to liquefied carbon dioxide. Stored in buffer tank.

  When the first pressure reduction time t1 elapses and the first pressure reduction time t1 ends (S-37), the controller 17 moves the valve mechanism of the pressure control valve of the pressure reduction separation unit 12 to the second set opening (second pressure reduction time t2). And the opening degree corresponding to the reduced pressure width at time t2) (S-38). The cleaning fluid circulating through the second route through the circulation pump 16 is circulated through the second route while being heated to a predetermined temperature by the heater 15 (S-39). Further, the cleaning fluid circulates through the third route, and a predetermined amount of the fluid gradually flows into the first route having a lower pressure than the second route and the third route during the circulation.

  The controller 17 maintains the valve mechanism of the pressure control valve of the decompression / separation unit 12 at the second set opening for the second decompression time t2. The cleaning fluid flows into the first route while circulating through the second and third routes, is depressurized and cooled by the pressure control valve of the depressurization separation unit 12 (S-40), and is also liquefied by the recovery supply unit 13 It is condensed and cooled, returned to liquefied carbon dioxide, and stored in a buffer tank.

  When the second decompression time t2 elapses and the second decompression time t2 ends (S-41), the controller 17 moves the valve mechanism of the pressure control valve of the decompression separation unit 12 to the third set opening (third decompression time t3). And the opening degree corresponding to the decompression width at time t3) (S-42). The cleaning fluid circulating through the second route through the circulation pump 16 is circulated through the second route while being heated to a predetermined temperature by the heater 15 (S-43). Further, the cleaning fluid circulates through the third route, and a predetermined amount of the fluid gradually flows into the first route having a lower pressure than the second route and the third route during the circulation.

  The controller 17 holds the valve mechanism of the pressure control valve of the decompression / separation unit 12 at the third set opening for the third decompression time t3. The cleaning fluid flows into the first route while circulating through the second and third routes, is depressurized and cooled by the pressure control valve of the depressurization separation unit 12 (S-44), and is also liquefied by the recovery supply unit 13 It is condensed and cooled, returned to liquefied carbon dioxide, and stored in a buffer tank. When the first to third decompression times t1 to t3 have elapsed and the internal pressure of the cleaning container 11 input from the pressure sensor has become atmospheric pressure, the controller 17 determines that the decompression has ended, and the fluid generating device 10 is temporarily stopped.

  In the second decompression operation pattern, the cleaning fluid returns from the critical region to the liquefied carbon dioxide (substance) through the gas phase region during the decompression (assisted by FIG. 6). In addition, when the pressure is reduced without using the second route and the third route using only the first route, the critical point that is the boundary between the supercritical region and the gas phase region (liquid phase region) and the vicinity thereof The cleaning fluid returns to the liquefied carbon dioxide through the gas-liquid mixing region (see FIG. 6).

  When the cleaning fluid is depressurized while being heated in the fluid generating device 10 or the component extraction method that performs the second decompression operation pattern, the temperature of the fluid does not decrease to near the critical point of the cleaning fluid, and the fluid maintains a high temperature, The temperature inside the cleaning container 11 (temperature of the cleaning fluid) when the pressure inside the cleaning container 11 (airtight structure cleaning chamber) reaches the atmospheric pressure (temperature of the cleaning fluid) is maintained at about 12 ° C. ( FIG. 7 assistance). When the cleaning fluid is depressurized while being heated in the second decompression operation pattern, the inside of the cleaning container 11 does not become minus temperature, and the filter accommodated in the cleaning container 11 (airtight structure cleaning chamber) is severe. There is no exposure to temperature.

  The fluid generating apparatus 10 and the component extraction method for performing the second decompression operation pattern shown in FIG. 9 extract the dirt component (component) contained in the filter (contained object) and then the supercritical or subcritical cleaning fluid (fluid). ) Into the first route, the fluid is caused to flow into the second route and the third route using the circulation pump 16, and the pressure control valve is heated while heating the fluid to a predetermined temperature using the heater 15. Since the fluid is decompressed by using the fluid, it is possible to prevent a rapid decrease in the fluid temperature during the decompression of the fluid, the inside of the cleaning container 11 (airtight structure cleaning chamber) does not become a negative temperature, and the fluid is kept at a predetermined temperature. The cleaning fluid can be returned to liquefied carbon dioxide while maintaining the temperature.

  In the fluid generator 10 and the component extraction method, the temperature inside the cleaning container 11 (airtight structure cleaning chamber) does not become negative in the process of depressurizing the cleaning fluid, and the filter is not exposed to a severe temperature environment. The cleaning fluid can be returned to a non-supercritical or non-subcritical fluid (substance) or carbon dioxide (substance) without damaging the filter. The fluid generation device 10 and the component extraction method use the circulation pump 16 to flow a fluid having a flow rate larger than the flow rate of the cleaning fluid that flows into the first route into the second route and the third route. Since a large amount of cleaning fluid is heated in the second route by using the heater 15, the fluid can be reliably heated by the heater 15 during the decompression of the cleaning fluid, and the fluid temperature during the decompression of the fluid can be increased. A sudden drop can be reliably prevented.

  In addition to the effects of the fluid generation device 10 and the component extraction method that perform the first decompression operation pattern shown in FIG. 4, the fluid generation device 10 and the component extraction method that perform the second decompression operation pattern shown in FIG. 9 have the following effects. Have. When the cleaning fluid is circulated in the second route and the temperature of the fluid is controlled only by the heater 15, even if the output of the heater 15 is lowered, the temperature of the fluid does not decrease immediately, and the temperature of the fluid that has increased more than necessary Although it is difficult to control the temperature, the fluid generator 10 and the component extraction method circulate the cleaning fluid not only in the second route (circulation route) but also in the third route (bypass route) during the decompression operation. The temperature of the cleaning fluid is controlled by controlling the mixing ratio of the cleaning fluid that circulates, and the temperature of the fluid that has risen more than necessary can be immediately reduced using the heater 15 and the third route. Sometimes the temperature of the fluid can be quickly adjusted to the set temperature.

The component extraction method according to the present invention sets the temperature of the fluid rather than adjusting the temperature of the fluid only by the heater 15 by circulating the fluid not only in the second route but also in the third route when the cleaning fluid is depressurized. It is easy to adjust the temperature, it can prevent a sudden drop in the fluid temperature during decompression of the fluid, and after extracting the dirt component (component) contained in the filter using the fluid, the fluid is kept at a predetermined temperature It is possible to return the fluid to carbon dioxide before becoming supercritical or subcritical while preventing the inside of the cleaning container 11 (airtight structure cleaning chamber) from becoming a negative temperature in the state.

10 Fluid generator 11 Cleaning container (airtight container)
12 Vacuum Separation Unit 13 Recovery Supply Unit 14 Booster Pump 15 Heater 16 Circulation Pump 17 Controller 18 First Pipe Line 19 Second Pipe Line 23 Bypass Pipe Line 27 Shut-off Valve

Claims (6)

An airtight container having a predetermined volume for containing an object containing a predetermined component; a vacuum separation unit installed after the airtight container and connected to the airtight container via a first conduit; and after the vacuum separation unit A recovery supply unit installed and connected to the decompression / separation unit via the first conduit; a booster pump installed after the recovery supply unit and connected to the recovery supply unit via the first conduit; A heater installed after the booster pump and connected to the booster pump via the first conduit, and a branch from a first conduit extending between the hermetic container and the decompression separation unit, and the booster pump and the A second pipe connected to the first pipe extending between the heater and a circulation pump installed in the second pipe;
A predetermined substance is heated and pressurized using the boost pump and the heater, the substance is changed to a supercritical or subcritical fluid, and the fluid is allowed to flow into the hermetic container to be contained in the contained object. After extracting the components, the fluid is caused to flow into the first pipe, and the fluid is caused to flow into the second pipe using the circulation pump, and the fluid is heated to a predetermined temperature using the heater. However, the component extraction method is characterized in that the fluid is decompressed using the decompression separation unit and the fluid is returned to the substance . In the component extraction method, the flow rate of the circulation pump is larger than that of the booster pump, and when the fluid is depressurized, the flow rate of the fluid that flows into the second pipe using the circulation pump is set to the first flow rate. More than the flow rate of the fluid flowing into the pipeline, the fluid is decompressed using the decompression separation unit while circulating the fluid in a circulation route passing through the hermetic container, the circulation pump, and the heater. The component extraction method according to claim 1, wherein the substance is returned to the substance, and the substance is recovered using the recovery supply unit . In the component extraction method, when the fluid is decompressed, the fluid decompression time is divided into a plurality of times, and the fluid is decompressed stepwise in a decompression width set for each decompression time. 2. The component extraction method described in 1 . 4. The component extraction method according to claim 3, wherein when the fluid is decompressed, the decompression time in the vicinity of the critical point of the fluid is set longer than other decompression times excluding the critical point and the vicinity thereof. Component extraction method . 5. The component extraction method according to claim 1, wherein when the fluid is decompressed, the fluid returns from the critical region to the substance through the gas phase region . 6. The component extraction method includes a bypass line branched from a second line extending between the circulation pump and the heater and connected to a first line extending between the heater and the airtight container; At the time of decompression of the fluid, the fluid is circulated through a circulation route passing through the hermetic container, the circulation pump, and the heater, and the fluid is passed through the bypass conduit. The component extraction method according to claim 1, wherein the component extraction method is circulated in a bypass route .

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