CN116688839A - Supercritical fluid preparation device, mixed fluid preparation device and preparation method - Google Patents
Supercritical fluid preparation device, mixed fluid preparation device and preparation method Download PDFInfo
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- CN116688839A CN116688839A CN202310993711.2A CN202310993711A CN116688839A CN 116688839 A CN116688839 A CN 116688839A CN 202310993711 A CN202310993711 A CN 202310993711A CN 116688839 A CN116688839 A CN 116688839A
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- 239000012530 fluid Substances 0.000 title claims abstract description 273
- 238000002360 preparation method Methods 0.000 title claims abstract description 95
- 238000002156 mixing Methods 0.000 claims description 92
- 238000003860 storage Methods 0.000 claims description 81
- 238000005057 refrigeration Methods 0.000 claims description 19
- 238000007599 discharging Methods 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 238000013022 venting Methods 0.000 claims description 4
- 239000007789 gas Substances 0.000 description 81
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 18
- 230000001276 controlling effect Effects 0.000 description 18
- 239000007788 liquid Substances 0.000 description 16
- 229910052786 argon Inorganic materials 0.000 description 9
- 229910052757 nitrogen Inorganic materials 0.000 description 9
- 230000001105 regulatory effect Effects 0.000 description 9
- 238000001816 cooling Methods 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 238000013461 design Methods 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000007774 longterm Effects 0.000 description 3
- 238000012423 maintenance Methods 0.000 description 3
- PWKWDCOTNGQLID-UHFFFAOYSA-N [N].[Ar] Chemical compound [N].[Ar] PWKWDCOTNGQLID-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 238000000194 supercritical-fluid extraction Methods 0.000 description 2
- 230000001960 triggered effect Effects 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
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- 238000007906 compression Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
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- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004808 supercritical fluid chromatography Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/20—Measuring; Control or regulation
- B01F35/22—Control or regulation
- B01F35/221—Control or regulation of operational parameters, e.g. level of material in the mixer, temperature or pressure
- B01F35/2213—Pressure
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
- B01F33/70—Mixers specially adapted for working at sub- or super-atmospheric pressure, e.g. combined with de-foaming
- B01F33/71—Mixers specially adapted for working at sub- or super-atmospheric pressure, e.g. combined with de-foaming working at super-atmospheric pressure, e.g. in pressurised vessels
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/20—Measuring; Control or regulation
- B01F35/22—Control or regulation
- B01F35/221—Control or regulation of operational parameters, e.g. level of material in the mixer, temperature or pressure
- B01F35/2215—Temperature
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Filling Or Discharging Of Gas Storage Vessels (AREA)
Abstract
The application relates to a supercritical fluid preparation device, a mixed fluid preparation device and a preparation method, and belongs to the field of fluid preparation devices. Comprising the following steps: the gas source is used for outputting a preset type of gas; the first channel is used for conveying the gas output by the gas source outwards; one end of the first channel is connected with an output port of the air source; a pressure controller for controlling the pressure of the gas output from the gas source to meet the pressure requirement of the supercritical fluid; the adjusting end of the pressure controller is connected with the first channel; the first temperature controller is used for controlling the temperature of the gas output from the gas source so as to meet the temperature requirement of the supercritical fluid; the first temperature controller comprises a heat exchanger, and the heat exchanger is connected with the first channel. The supercritical fluid preparation device, the mixed fluid preparation device and the preparation method have lower cost.
Description
Technical Field
The application relates to the field of fluid preparation devices, in particular to a supercritical fluid preparation device, a mixed fluid preparation device and a preparation method.
Background
Supercritical state is a special fluid. Near the critical point, it has great compressibility, and proper pressure increase can make its density approach that of general liquid, so that it has good property of dissolving other substances. On the other hand, the viscosity in the supercritical state is only 1/12 to 1/4 of that of the common liquid, but the diffusion coefficient is 7 to 24 times greater than that of the common liquid, which approximates to that of gas. Supercritical fluids are widely used, such as supercritical extraction, supercritical fluid chromatography, chemical reactions in supercritical fluids, and the like, but are most widely used in supercritical fluid extraction.
The physical properties of nitrogen and argon are close, the supercritical state parameters are also relatively close, and the medical industry utilizes mixed fluid composed of supercritical nitrogen and supercritical argon to carry out related extraction and other works. At present, the preparation device of supercritical nitrogen argon has the problem of high cost.
Disclosure of Invention
In view of the above, an embodiment of the present application provides a supercritical fluid preparation apparatus, a mixed fluid preparation apparatus and a preparation method for solving at least one of the problems in the background art.
In order to achieve the above purpose, the technical scheme of the application is realized as follows:
in a first aspect, an embodiment of the present application provides a supercritical fluid preparation apparatus, including:
the gas source is used for outputting a preset type of gas;
the first channel is used for conveying the gas output by the gas source outwards; one end of the first channel is connected with an output port of the air source;
a pressure controller for controlling the pressure of the gas output from the gas source to meet the pressure requirement of the supercritical fluid; the adjusting end of the pressure controller is connected with the first channel;
the first temperature controller is used for controlling the temperature of the gas output from the gas source so as to meet the temperature requirement of the supercritical fluid; the first temperature controller comprises a heat exchanger, and the heat exchanger is connected with the first channel.
Optionally, the supercritical fluid preparation apparatus further comprises:
a fluid storage container for storing the fluid after being controlled by the pressure controller and the first temperature controller;
and a second channel for outputting the supercritical fluid in the fluid storage container to the outside.
Optionally, the gas source comprises a bottle storing compressed gas, and the pressure controller comprises a pressure reducing valve.
Optionally, the supercritical fluid preparation apparatus further comprises:
a tank pressure control valve for venting fluid from the fluid storage vessel if the pressure in the fluid storage vessel is above a threshold.
Optionally, the first temperature controller includes:
a first GM refrigerator having a refrigeration head in thermal contact with the heat exchanger;
a first heater is in thermal contact with the refrigeration head.
Optionally, the supercritical fluid preparation apparatus further comprises:
a second temperature controller is located in the fluid storage vessel to control the temperature within the fluid storage vessel.
Optionally, the supercritical fluid preparation apparatus further comprises:
the temperature sensor is used for detecting the temperature in the fluid storage container and is used as a basis for controlling the first temperature controller;
and the pressure sensor is used for detecting the pressure in the fluid storage container and is used as the basis for controlling by the pressure controller.
Optionally, the supercritical fluid preparation apparatus further comprises:
the first vacuum cavity capable of forming a vacuum environment, the fluid storage container is located in the vacuum cavity of the first vacuum cavity, and the first temperature controller, the first channel and the second channel are located in the vacuum cavity of the first vacuum cavity.
In a second aspect, an embodiment of the present application provides a supercritical fluid preparation method, which is applied to any one of the supercritical fluid preparation apparatuses described above, including:
controlling the pressure of the gas output from the gas source to be a first preset value larger than the critical pressure through a pressure controller;
and discharging the fluid in the fluid storage container through a tank pressure control valve, so that the pressure in the fluid storage container is larger than the critical pressure by a second preset value, and the second preset value is smaller than the first preset value.
Optionally, the supercritical fluid preparation method further comprises:
controlling the temperature of the gas output from the gas source to be less than a critical temperature by a first temperature controller;
and controlling, by a second temperature controller, a temperature within the fluid storage container to be greater than the critical temperature.
In a third aspect, an embodiment of the present application provides a supercritical mixed fluid preparation apparatus, including:
at least two supercritical fluid preparation apparatuses of any one of the above;
a mixing vessel for connecting at least two of the second channels in the supercritical fluid preparation apparatus;
a third temperature controller for controlling the temperature within the mixing vessel;
and a third passage for outputting the supercritical fluid in the mixing vessel to the outside.
Optionally, the supercritical mixed fluid preparation apparatus further comprises:
a tank pressure control valve for venting fluid from the mixing vessel if the pressure in the mixing vessel is above a threshold.
Optionally, the third temperature controller includes:
a second GM refrigerator having a refrigeration head in thermal contact with the mixing vessel;
a third heater is located in the mixing vessel to control the temperature within the mixing vessel.
Optionally, the supercritical mixed fluid preparation apparatus further comprises:
the second vacuum cavity capable of forming a vacuum environment, wherein the fluid storage container, the mixing container and the second channel in the supercritical fluid preparation device are all positioned in the vacuum cavity of the second vacuum cavity, and the first temperature controller, the third temperature controller, the first channel and part of the third channel are positioned in the vacuum cavity of the second vacuum cavity.
In a fourth aspect, an embodiment of the present application provides a method for preparing a supercritical mixed fluid, which is applied to any one of the above supercritical mixed fluid preparing apparatuses, including:
the pressure in the mixing container is controlled to be a third preset value larger than the critical pressure through a tank pressure control valve;
and discharging the fluid in the mixing container through a tank pressure control valve, so that the pressure in the mixing container is larger than the critical pressure by a fourth preset value, and the fourth preset value is smaller than the third preset value.
Optionally, the supercritical mixed fluid preparation method further comprises:
setting the temperature of the refrigeration head of the second GM refrigerator to be less than a critical temperature;
the temperature in the mixing vessel is controlled to be greater than the critical temperature by a third heater.
The supercritical fluid preparation device, the mixed fluid preparation device and the preparation method comprise the following steps: the gas source is used for outputting a preset type of gas; the first channel is used for conveying the gas output by the gas source outwards; one end of the first channel is connected with an output port of the air source; a pressure controller for controlling the pressure of the gas output from the gas source to meet the pressure requirement of the supercritical fluid; the adjusting end of the pressure controller is connected with the first channel; the first temperature controller is used for controlling the temperature of the gas output from the gas source so as to meet the temperature requirement of the supercritical fluid; the first temperature controller comprises a heat exchanger, and the heat exchanger is connected with the first channel. Therefore, the supercritical fluid preparation device, the mixed fluid preparation device and the preparation method adopt reverse engineering, directly use normal-temperature gas as a raw material to cool down, realize the supercritical fluid, have the characteristics of being convenient for long-term storage and low cost, and the arrangement of a gas pipeline does not need expensive parts, so that the cost is further reduced. Therefore, the supercritical fluid preparation device, the mixed fluid preparation device and the preparation method have lower cost.
Additional aspects and advantages of the application will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the application.
Drawings
The accompanying drawings, which are included to provide a further understanding of the application and are incorporated in and constitute a part of this specification, illustrate embodiments of the application and together with the description serve to explain the application and do not constitute a limitation on the application. In the drawings:
FIG. 1 is a schematic view of a supercritical fluid preparing apparatus according to an embodiment of the present application;
FIG. 2 is a schematic flow chart of a supercritical fluid preparation method according to an embodiment of the present application;
FIG. 3 is a detailed schematic flow chart of a supercritical fluid preparation method according to an embodiment of the present application;
fig. 4 is a schematic flow chart of a method for preparing a supercritical fluid according to an embodiment of the present application.
Reference numerals illustrate:
11. a gas source; 12. a first channel; 121. a pressure controller; 122. a flow meter; 13. a first temperature controller; 131. a heat exchanger; 132. a first GM refrigerator; 133. a first heater; 14. a fluid storage container; 141. a tank pressure control valve; 142. a safety valve; 15. a second heater; 16. a temperature sensor; 17. a pressure sensor; 18. a second channel; 21. a mixing vessel; 22. a third temperature controller; 221. a second GM refrigerator; 222. a third heater; 223. a flexible heat conducting strip; 23. a third channel; 241. a flow control valve; 242. a check valve; 251. a second cavity; 252. a second chamber cover plate.
Detailed Description
In order to make the technical scheme and the beneficial effects of the application more obvious and understandable, the following detailed description is given by way of example. Wherein the drawings are not necessarily to scale, and wherein local features may be exaggerated or reduced to more clearly show details of the local features; unless defined otherwise, technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
In the description of the present application, the terms "center", "longitudinal", "transverse", "length", "width", "thickness", "height", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", etc. refer to the orientation or positional relationship based on the orientation or positional relationship shown in the drawings, and are merely for convenience of simplifying the description of the present application, and do not indicate that the apparatus or element referred to must have a specific orientation, be constructed and operated in a specific orientation, i.e., are not to be construed as limiting the present application.
In the present application, the terms "first", "second" are used for descriptive purposes only and are not to be construed as relative importance of the features indicated or the number of technical features indicated. Thus, a feature defining "first", "second" may explicitly include at least one such feature. In the description of the present application, "plurality" means at least two, for example, two, three, etc.; "plurality" means at least one, such as one, two, three, etc.; unless otherwise specifically defined.
In the present application, the terms "mounted," "connected," "secured," "disposed," and the like are to be construed broadly, unless otherwise specifically limited. For example, "connected" may be either fixedly connected or detachably connected, or integrally formed; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium, or can be communicated between two elements or the interaction relationship between the two elements. The specific meaning of the above terms in the present application can be understood by those of ordinary skill in the art according to the specific circumstances.
In the present application, unless explicitly defined otherwise, a first feature "on", "above", "over" and "above", "below" or "under" a second feature may be that the first feature and the second feature are in direct contact, or that the first feature and the second feature are in indirect contact via an intermediary. Moreover, a first feature "above," "over" and "on" a second feature may be that the first feature is directly above or obliquely above the second feature, or simply indicates that the level of the first feature is higher than the level of the second feature. The first feature being "under", "below" and "beneath" the second feature may be the first feature being directly under or obliquely below the second feature, or simply indicating that the level of the first feature is less than the level of the second feature.
In order to provide a thorough understanding of the present application, detailed steps and detailed structures will be presented in the following description in order to explain the technical solution of the present application. Preferred embodiments of the present application are described in detail below, however, the present application may have other embodiments in addition to these detailed descriptions.
In the prior art, for example, the application number is: 202221003824.0, the application name is: in the application patent of the supercritical nitrogen-argon mixed fluid generating system, liquid nitrogen and liquid argon are used as raw materials, and are directly conveyed to a buffer tank (the buffer tanks 140 and 240 are in a high-pressure liquid state, and the temperature is lower than the critical state temperature) through a low-temperature fluid pump. High-pressure liquid nitrogen and liquid argon are sent into the mixing tank 300, and heated in the mixing tank, so that the mixed liquid nitrogen and liquid argon are heated, vaporized and heated continuously to reach the supercritical temperature, and finally the mixed fluid reaches the supercritical state. Because the liquid volatilizes fast, can't store for a long time, not only use inconvenient, storage cost is also high, and the low temperature liquid pump cost that the liquid pipeline used in addition is higher, leads to whole device cost high. In addition, the patent has the defects that the temperature cannot be precisely controlled, the supercritical state of the fluid is unstable and the time for forming the supercritical fluid is not controllable because the temperature can be raised only by heating and the temperature cannot be lowered. For mixed fluids, the mixing ratio cannot be precisely controlled, and the use value is not high.
Example 1
The embodiment provides a supercritical fluid preparation device, fig. 1 is a schematic diagram of the supercritical mixed fluid preparation device provided by the embodiment of the application, the supercritical fluid preparation device of the embodiment is a part of the structure in fig. 1, as shown in fig. 1, and the supercritical fluid preparation device includes:
a gas source 11 for outputting a predetermined kind of gas;
a first channel 12, configured to convey the gas output from the gas source 11 to the outside; one end of the first channel 12 is connected with an output port of the air source 11;
a pressure controller 121 for controlling the pressure of the gas outputted from the gas source 11 to meet the pressure requirement of the supercritical fluid; the adjusting end of the pressure controller 121 is connected with the first channel 12;
a first temperature controller 13 for controlling the temperature of the gas outputted from the gas source 11 to meet the temperature requirement of the supercritical fluid; the first temperature controller 13 includes a heat exchanger 131, and the heat exchanger 131 is connected to the first channel 12.
Compared with the prior art, the embodiment adopts gas as the raw material, and has the characteristics of lower cost and convenient use. The gas source 11 is a gas generating member or a container for storing a gas, and the kind of the gas can be selected as required. In the present embodiment, various components are arranged by taking nitrogen or argon as an example, and it is understood that other gases may be used, and the components to be arranged may be adjusted accordingly.
It is understood that the pressure herein may be pressure, and in the engineering field, the pressure (pressure) of a unit area and the total pressure are indicated by pressure, so that the reader can determine a specific meaning according to a specific situation.
It will be appreciated that the pressure controller 121 may control the pressure of the gas within the conduit by controlling the pressure of the conduit as the gas is conveyed through the conduit. The first channel 12 described above may be comprised of one or more pipes.
It will be appreciated that the first temperature controller 13 may control the temperature of the gas by means of refrigeration or heating. It should be noted that, after the gas is cooled to a certain degree, it may be converted into a liquid. And the supercritical fluid of the present application is a state similar to the gas-liquid indiscriminate state, so in the description herein, the gas and the liquid are not strictly distinguished, and the reader can judge which state is according to the specific situation.
It will be appreciated that the heat exchanger 131 is connected to the first channel 12, and that the heat exchanger 131 is in communication with the first channel 12, and heat can be exchanged. Other references to being connected to channels or conduits are also meant to indicate communication with each other, exchanging heat, regulating pressure, etc.
The supercritical fluid preparation device adopts reverse engineering, directly uses normal-temperature gas as a raw material, and reduces the temperature to reach a supercritical state. The gas has the characteristics of being convenient for long-term storage and low in cost, and the arrangement of the gas pipeline does not need expensive parts, so that the cost is further reduced.
In some embodiments, the supercritical fluid preparation apparatus may further include:
a fluid storage container 14 for storing the fluid after being controlled by the pressure controller 121 and the first temperature controller 13;
a second passage 18 for outputting the supercritical fluid in the fluid storage container 14 to the outside.
It will be appreciated that the fluid storage container 14 is a device having a relatively closed chamber for storing gas that better maintains pressure and temperature stability of the fluid.
As described above, the second channel 18 may be comprised of one or more pipes. Specifically, a valve can be provided, and the valve can be automatically opened after the pressure and the temperature of the supercritical fluid meet certain requirements, or the valve can be manually operated.
In some embodiments, the gas source 11 comprises a bottle that stores compressed gas, and the pressure controller 121 may comprise a pressure reducing valve.
It will be appreciated that the bottle storing the compressed gas may be a high pressure bottle. On the one hand, in the form of compressed gas, more capacity gas can be stored, on the other hand, the pressure of the gas output by the high-pressure bottle body is higher, the pressure of fluid reaching the supercritical state can be met, supercharging equipment is not required, the structure is simplified, and the cost is reduced.
It can be understood that the output end of the high-pressure bottle body is required to be provided with a pressure reducing valve, so that the pressure of the output gas can be controlled through the pressure reducing valve, the structure is simplified, and the cost is reduced.
In particular, the body may be a steel cylinder capable of withstanding high pressures.
Specifically, the gas source 11 may further include a switch valve, which is used for switching the output gas of the gas source 11, and the switch valve and the pressure reducing valve are used in cooperation.
In some embodiments, the supercritical fluid preparation apparatus may further include:
a tank pressure control valve 141 for discharging the fluid in the fluid storage container 14 in the case where the pressure in the fluid storage container 14 is higher than a threshold value.
In one aspect, the pressure within fluid storage vessel 14 may be more precisely controlled to facilitate the formation of supercritical fluid. On the other hand, damage to the fluid storage container 14 due to excessive pressure may also be reduced, resulting in greater safety.
Specifically, the supercritical fluid preparation apparatus may further include:
a safety valve 142 for discharging the fluid in the fluid storage container 14 to secure the fluid storage container 14 in case that the pressure in the fluid storage container 14 is higher than a safety value. The relief valve 142 may be used in conjunction with the canister pressure control valve 141 to make the fluid storage container 14 safer.
Specifically, the tank pressure control valve 141 may be a back pressure valve. The back pressure valve can act to regulate and over-flow, i.e., regulate the pressure within the fluid storage container 14, or passively release in the event that the pressure within the fluid storage container 14 is above a threshold, as well as acting as part of the relief valve 142, which can stabilize the pressure within the fluid storage container 14.
In some embodiments, the first temperature controller 13 includes:
a first GM refrigerator 132, the refrigeration head of the first GM refrigerator 132 being in thermal contact with the heat exchanger 131;
a first heater 133 is in thermal contact with the refrigeration head.
GM refrigerators, also known as G-M refrigerators, were invented by two persons, gifford (Gifford) and Mcmahon (Mcmahon), by the initials of the two inventors. The minimum ultralow temperature below 4.2K of the GM refrigerator can be obtained, the compression end and the expansion end are separated, the structure is compact, the use is convenient, the service life is long, the maintenance is simple, and the GM refrigerator is one of the refrigeration sources commonly used in small ultralow temperature equipment.
Note that, the GM refrigerator cooling capacity varies depending on the cooling temperature, and therefore, by providing the first heater 133, the refrigerator cooling capacity is balanced by heating, thereby precisely controlling the temperature and the cooling capacity. The supercritical fluid preparation device provided by the embodiment of the application has the functions of refrigeration and heating, and further improves the stability of a supercritical state.
Kelvin temperature, also known as Kelvin temperature scale, absolute temperature scale, is one of seven basic physical quantities produced by international units, the unit is Kelvin, (symbol is K) for short, and the conversion relation between Kelvin and Centigrade temperature is: t (K) =t (° C) +273.15, T being absolute temperature scale.
In some embodiments, the supercritical fluid preparation apparatus further comprises:
a second temperature controller is located in the fluid storage container 14 to control the temperature within the fluid storage container 14.
Further temperature control is required because the temperature may also change due to the fluid storage container 14 after the fluid enters the fluid storage container 14.
In particular, the second temperature controller may include a second heater disposed within the fluid storage container 14. In this way, the temperature of the fluid outside the fluid storage container 14 may be controlled to be slightly lower and then the temperature may be trimmed by heating after entering the fluid storage container 14. To reduce the occurrence of: the temperature of the fluid after entering the fluid storage container 14 is too high to be regulated. And refrigeration facilities are not needed to be arranged on the fluid storage container 14, so that the structure is simpler and the cost is lower.
In some embodiments, the supercritical fluid preparation apparatus further comprises:
a temperature sensor 16 for detecting the temperature in the fluid storage container 14 as a basis for control by the first temperature controller 13;
a pressure sensor 17 for detecting the pressure in the fluid storage container 14 as a basis for control by the pressure controller 121.
In this way, dynamic feedback and regulation is possible, allowing for more precise temperatures and pressures within the fluid storage container 14.
In some embodiments, the supercritical fluid preparation apparatus further comprises:
a flow meter 122 for measuring the flow rate of the gas outputted from the gas source 11, wherein the flow meter 122 is disposed at one end of the first channel 12 near the gas source 11.
Therefore, the flow of the gas can be accurately controlled and measured, and the flow is converted into the fluid quantity in the supercritical state through the corresponding conversion ratio, so that the fluid quantity in the supercritical state can be more accurately obtained.
In some embodiments, the supercritical fluid preparation apparatus further comprises:
a first vacuum chamber capable of forming a vacuum environment, the fluid storage container 14 being located within the vacuum chamber of the first vacuum chamber, and portions of the first temperature controller 13, the first channel 12, and the second channel 18 being located within the vacuum chamber of the first vacuum chamber.
The vacuum environment can reduce the loss of cold (heat), on one hand, the state of the supercritical fluid and the fluid in the inlet and outlet pipelines can be kept stable; on the other hand, the heat insulation protection or vacuum jacket design necessary for the separate design of the fluid storage container 14 and the pipeline can be avoided, the manufacturing difficulty is reduced, and the cost is low.
Specifically, the first vacuum chamber may include a first chamber and a first chamber cover, the fluid storage container 14 is located in the first chamber, the uniform ends of the temperature controller, the first channel 12 and the second channel 18 are located outside the first chamber, and the other end passes through the first chamber cover and enters the first chamber. Thus, the manufacturing and the maintenance are convenient.
Since fig. 1 shows the fluid storage container 14 and the mixing container 21 (see description below) together within the second vacuum chamber, the drawing does not show a separate first vacuum chamber.
Example two
The present embodiment provides a supercritical fluid preparation method applied to the supercritical fluid preparation apparatus according to the first embodiment, as shown in fig. 2, the method includes:
step 601: the gas pressure outputted from the gas source 11 is controlled to be greater than a first preset value of the critical pressure by the pressure controller 121;
step 602: the fluid in the fluid storage container 14 is discharged through the tank pressure control valve 141, so that the pressure in the fluid storage container 14 is greater than the critical pressure by a second preset value, which is smaller than the first preset value.
It will be appreciated that, since the temperature is regulated and controlled by the first temperature controller 13 and the second temperature controller during the flow of the gas into the fluid storage container 14, the pressure of the fluid will vary with the temperature, and the pressure will also vary accordingly when the gas flows into the fluid storage container 14 from the pipeline, so that fine adjustment of the pressure of the fluid storage container 14 into the fluid is required.
Therefore, the gas pressure output from the gas source 11 can be controlled to be greater than the critical pressure by a first preset value that leaves a margin so that after the fluid flows into the fluid storage container 14, the container pressure is also greater than the critical pressure, and the fine tuning is performed in a reduced pressure manner. In this way, only one means of regulating pressure need be maintained within fluid storage container 14, simplifying the structure, and reducing pressure is easier to implement and reduces costs as compared to increasing pressure.
Further, the fluid in the fluid storage container 14 is discharged through the tank pressure control valve 141, and on the one hand, the pressure in the fluid storage container 14 can be more accurate to facilitate the formation of the supercritical fluid. On the other hand, damage to the fluid storage container 14 due to excessive pressure may also be reduced, resulting in greater safety.
The second preset value is determined according to the related requirements for forming the supercritical fluid, and the first preset value can be determined experimentally according to a specific supercritical fluid preparation device.
In some embodiments, the method further comprises:
step 603: the temperature of the gas outputted from the gas source 11 is controlled to be less than the critical temperature by the first temperature controller 13;
step 604: the temperature within the fluid storage container 14 is controlled to be greater than the critical temperature by a second temperature controller.
It will be appreciated that fine tuning of the temperature of the fluid storage vessel 14 into which fluid flows is required as there will be a corresponding change in temperature during the flow of gas into the fluid storage vessel 14, for example, a temperature difference between the flow of gas from the conduit into the fluid storage vessel 14.
Therefore, the temperature of the fluid before flowing into the fluid storage container 14 can be controlled to be lower than the critical temperature, and a certain margin is left, so that the temperature in the container after the fluid flows into the fluid storage container 14 is also lower than the critical temperature, and the fine tuning mode is to raise the temperature. In this way, only one means of regulating temperature need be maintained within the fluid storage container 14, simplifying construction, and reducing costs as compared to refrigeration, and warming is easier to implement.
For a more detailed understanding of the supercritical fluid preparation method according to an embodiment of the present application, a further description will be given below with reference to fig. 3, and as shown in fig. 3, the method includes:
step 701: setting supercritical state parameters. Parameters include temperature and pressure.
Step 702: the high-pressure gas cylinder outputs gas.
Step 703: the pressure reducing valve regulates the pressure. The regulated pressure is slightly higher than the target pressure.
Step 704: whether the target pressure is reached. No, step 705 and step 703 are entered, yes, and step 710 is entered.
Step 705: the tank pressure control valve passively regulates pressure. The tank pressure control valve can automatically reduce the pressure when the pressure is larger than the set pressure.
Step 706: the relief valve 142 is passively opened. While the tank pressure control valve is triggered, the relief valve 142 may also be triggered for passive venting if the pressure is too great.
Step 707: the vent valve is opened manually. The staff can open the exhaust valve manually according to the specific circumstances.
Step 708: and (5) actively regulating the temperature. Can be a combination of a refrigerator and a heater.
Step 709: whether the target temperature is reached. If not, step 708 is entered, and if yes, step 710 is entered.
Step 710: forming supercritical fluid.
Step 711: fluid output. And outputting the supercritical fluid through the long-handle low-temperature valve.
Example III
The present embodiment provides a supercritical mixed fluid preparation apparatus, as shown in fig. 1, including:
the supercritical fluid preparation apparatus according to at least two embodiments;
a mixing vessel 21 for connecting at least two of the second channels 18 in the supercritical fluid preparation apparatus;
a third temperature controller 22 for controlling the temperature inside the mixing vessel 21;
and a third passage 23 for outputting the supercritical fluid in the mixing vessel 21 to the outside.
It will be appreciated that the mixing vessel 21 is used to mix two supercritical fluids into a supercritical mixed fluid, i.e. the gases in at least two supercritical fluid preparation devices are different gases. In this embodiment, two supercritical fluid preparing apparatuses are taken as an example, that is, two fluids are mixed into a supercritical mixed fluid, and the two fluids are nitrogen and argon respectively. The physical properties of nitrogen and argon are close, the supercritical state parameters are also relatively close, and the medical industry utilizes mixed fluid composed of supercritical nitrogen and supercritical argon to carry out related extraction and other works. It will be appreciated that other fluids are possible, as well as three or more supercritical fluid preparation apparatuses to mix three or more fluids.
It will be appreciated that, due to the difference in supercritical state of the two fluids, the temperature and pressure of the supercritical fluids after mixing will affect each other, and even the respective supercritical state will be broken. The temperature and pressure in the mixing tank need to be fine-tuned again. Therefore, the third temperature controller 22 is provided to finely adjust the temperature in the mixing vessel 21.
The pressure in the mixing container 21 can be controlled to be higher before mixing, a certain margin is reserved, and after the mixture enters the mixing container 21 for mixing, part of fluid is discharged through the arranged tank pressure control valve 141, so that the pressure in the mixing container 21 is reduced to meet the pressure requirement of the supercritical mixed fluid.
The supercritical mixed fluid preparation device provided by the embodiment of the application adopts reverse engineering, directly uses normal-temperature gas as a raw material to cool, realizes supercritical fluid, has the characteristics of convenience for long-term storage and low cost, and further reduces the cost by arranging a gas pipeline without expensive parts.
In some embodiments, the supercritical mixed fluid preparation apparatus further comprises:
a tank pressure control valve 141 for discharging the fluid in the mixing vessel 21 in case the pressure in the mixing vessel 21 is higher than a threshold value.
On the one hand, the pressure within the mixing vessel 21 may be more precisely controlled to facilitate the formation of supercritical fluid. On the other hand, damage to the mixing vessel 21 due to excessive pressure can also be reduced, making it safer.
Specifically, the supercritical mixed fluid preparation apparatus may further include:
a safety valve 142 for discharging the fluid in the mixing container 21 to secure the safety of the mixing container 21 in case that the pressure in the mixing container 21 is higher than a safety value. The safety valve 142 may be used in combination with the tank pressure control valve 141 to make the mixing vessel 21 safer.
In some embodiments, the supercritical mixed fluid preparation apparatus further comprises:
a flow control valve 241 for controlling the amount of gas flowing into the mixing vessel 21, the flow control valve 241 being provided in the second passage 18 near one end of the mixing vessel 21.
It will be appreciated that the flow rate of the fluid will vary from one pressure state to another, from one temperature state to another, and from one state to another after mixing. However, the output flow rate of the mixing vessel 21 is proportional to the input flow rate, and thus the output amount of the mixing vessel 21 can be controlled by adjusting the flow rate of the fluid flowing into the mixing vessel 21 through the flow control valve 241. In this way, a more accurate acquisition of the fluid quantity in the supercritical state is facilitated.
Specifically, the supercritical mixed fluid preparation device further comprises:
a check valve 242 for controlling the reverse flow of fluid within the mixing vessel 21.
I.e. the fluid in the mixing vessel 21 is not allowed to flow in the opposite direction to the input end, so as not to confuse the mixing ratio of the mixed gas and to inaccuracy of the mixing amount.
Specifically, the flow control valve 241 may be a long-handle low-temperature valve, which is suitable for a low-temperature environment, and is convenient to operate because of the long operating handle.
In some embodiments, the third temperature controller 22 includes:
a second GM refrigerator 221, the refrigeration head of the second GM refrigerator 221 being in thermal contact with the mixing vessel 21;
a third heater 222 is located in the mixing vessel 21 to control the temperature within the mixing vessel 21.
As described above, since the GM refrigerator has a good cooling effect but cannot be precisely controlled, the temperature is finely adjusted by the third heater 222, so that the temperature in the mixing container 21 is more precise.
In some embodiments, the refrigeration head of the second GM refrigerator 221 is in thermal contact with the mixing vessel 21 via a flexible thermal conductive tape 223.
The flexible heat conduction band 223 can maintain good heat transfer effect, and can better maintain thermal contact between the two due to flexibility, and cannot be separated from thermal contact due to vibration and the like.
In some embodiments, the supercritical fluid preparation apparatus further comprises a second vacuum chamber capable of forming a vacuum environment, wherein the fluid storage container 14, the mixing container 21 and the second channel 18 are all located in the vacuum chamber of the second vacuum chamber, and the first temperature controller 13, the third temperature controller 22, the first channel 12 and the third channel 23 are partially located in the vacuum chamber of the second vacuum chamber.
As described above, the vacuum environment can reduce the loss of cold (heat), and on one hand, can keep the state of supercritical fluid and fluid in the inlet and outlet pipelines stable; on the other hand, the heat insulation protection or vacuum jacket design necessary for the separate design of the fluid storage container 14 and the pipeline can be avoided, the manufacturing difficulty is reduced, and the cost is low.
Specifically, the second vacuum chamber may include a second chamber 251 and a second chamber cover 252, where the fluid storage container 14, the mixing container 21 and the second channel 18 are all located in the vacuum chamber of the second chamber 251, and the uniform ends of the first temperature controller 13, the third temperature controller 22, the first channel 12 and the third channel 23 are located outside the vacuum chamber of the second chamber 251, and the other ends pass through the second chamber cover 252 and enter the vacuum chamber of the second chamber 251. Thus, the manufacturing and the maintenance are convenient.
It is understood that the first vacuum chamber may be separately provided for each supercritical fluid preparing apparatus, and the second vacuum chamber of the supercritical mixed fluid preparing apparatus may accommodate only the mixing vessel 21 and a part of the piping required to be connected to the mixing vessel 21, and the like.
Example IV
The present embodiment provides a method for preparing a supercritical mixed fluid, which is applied to the supercritical mixed fluid preparing apparatus according to the third embodiment, as shown in fig. 4, and the method for preparing a supercritical mixed fluid includes:
step 801: the pressure in the mixing vessel 21 is controlled to be greater than a third preset value of the critical pressure by the tank pressure control valve 141;
step 802: the fluid in the mixing container 21 is discharged through the tank pressure control valve 141, so that the pressure in the mixing container 21 is greater than the critical pressure by a fourth preset value, which is less than the third preset value.
It will be appreciated that, due to the difference in supercritical state of the two fluids, the temperature and pressure of the supercritical fluids after mixing will affect each other, and even the respective supercritical state will be broken. The temperature and pressure in the mixing tank need to be fine-tuned again.
Therefore, the pressure before mixing can be controlled to be high, a certain margin is left, and after the mixture enters the mixing container 21 for mixing, the pressure of the mixing container 21 is also larger than the critical pressure, and the fine adjustment can be performed by decompression. In this way, only one means of regulating the pressure needs to be maintained in the mixing vessel 21, simplifying the structure, and reducing the pressure is easier to implement than increasing the pressure, reducing the cost.
Further, the fluid in the mixing vessel 21 is discharged through the tank pressure control valve 141, and on the one hand, the pressure in the mixing vessel 21 can be more precisely controlled to facilitate the formation of the supercritical fluid. On the other hand, damage to the mixing vessel 21 due to excessive pressure can also be reduced, making it safer.
As described above, the fourth preset value is determined according to the requirements related to the formation of the supercritical fluid, and the third preset value may be determined experimentally according to the specific supercritical mixed fluid preparation apparatus.
Specifically, the tank pressure control valve 141 may be a back pressure valve. The back pressure valve can function to regulate and overflow, i.e. to regulate the pressure in the mixing vessel 21, or to passively release in case the pressure in the mixing vessel 21 is above a threshold value, and also to function as part of the safety valve 142, which can stabilize the pressure in the mixing vessel 21.
In some embodiments, the supercritical mixed fluid preparation method further comprises:
step 803: setting the temperature of the refrigeration head of the second GM refrigerator 221 to be less than the critical temperature;
step 804: the temperature in the mixing vessel 21 is controlled to be greater than the critical temperature by a third heater 222.
It will be appreciated that, due to the difference in supercritical state of the two fluids, the temperature and pressure of the supercritical fluids after mixing will affect each other, and even the respective supercritical state will be broken. The temperature and pressure in the mixing tank need to be fine-tuned again.
Therefore, the temperature of the cooling head of the second GM refrigerator 221 may be set to be less than the critical temperature, with a certain margin, so that the temperature in the mixing vessel 21 is also less than the critical temperature after the fluid flows into the mixing vessel 21, and the trimming is performed by heating. In this way, only one means for regulating and controlling the temperature is needed to be reserved in the mixing container 21, the structure is simplified, and compared with refrigeration, the temperature rise is easier to implement, and the cost is reduced.
It should be understood that the above examples are illustrative and are not intended to encompass all possible implementations encompassed by the claims. Various modifications and changes may be made in the above embodiments without departing from the scope of the disclosure. Likewise, the individual features of the above embodiments can also be combined arbitrarily to form further embodiments of the application which may not be explicitly described. Therefore, the above examples merely represent several embodiments of the present application and do not limit the scope of protection of the patent of the present application.
Claims (16)
1. A supercritical fluid preparation apparatus, comprising:
the gas source is used for outputting a preset type of gas;
the first channel is used for conveying the gas output by the gas source outwards; one end of the first channel is connected with an output port of the air source;
a pressure controller for controlling the pressure of the gas output from the gas source to meet the pressure requirement of the supercritical fluid; the adjusting end of the pressure controller is connected with the first channel;
the first temperature controller is used for controlling the temperature of the gas output from the gas source so as to meet the temperature requirement of the supercritical fluid; the first temperature controller comprises a heat exchanger, and the heat exchanger is connected with the first channel.
2. The supercritical fluid preparation apparatus according to claim 1, further comprising:
a fluid storage container for storing the fluid after being controlled by the pressure controller and the first temperature controller;
and a second channel for outputting the supercritical fluid in the fluid storage container to the outside.
3. The supercritical fluid manufacturing apparatus according to claim 1 or 2, wherein the gas source comprises a bottle storing compressed gas, and the pressure controller comprises a pressure reducing valve.
4. The supercritical fluid preparation apparatus according to claim 2, further comprising:
a tank pressure control valve for venting fluid from the fluid storage vessel if the pressure in the fluid storage vessel is above a threshold.
5. The supercritical fluid manufacturing apparatus according to claim 1 or 2, wherein the first temperature controller comprises:
a first GM refrigerator having a refrigeration head in thermal contact with the heat exchanger;
a first heater is in thermal contact with the refrigeration head.
6. The supercritical fluid preparation apparatus according to claim 2, further comprising:
a second temperature controller is located in the fluid storage vessel to control the temperature within the fluid storage vessel.
7. The supercritical fluid preparation apparatus according to claim 2, further comprising:
the temperature sensor is used for detecting the temperature in the fluid storage container and is used as a basis for controlling the first temperature controller;
and the pressure sensor is used for detecting the pressure in the fluid storage container and is used as the basis for controlling by the pressure controller.
8. The supercritical fluid preparation apparatus according to claim 2, further comprising:
the first vacuum cavity capable of forming a vacuum environment, the fluid storage container is located in the vacuum cavity of the first vacuum cavity, and the first temperature controller, the first channel and the second channel are located in the vacuum cavity of the first vacuum cavity.
9. A supercritical fluid preparation method applied to the supercritical fluid preparation apparatus according to any one of claims 1 to 8, comprising:
controlling the pressure of the gas output from the gas source to be a first preset value larger than the critical pressure through a pressure controller;
and discharging the fluid in the fluid storage container through a tank pressure control valve, so that the pressure in the fluid storage container is larger than the critical pressure by a second preset value, and the second preset value is smaller than the first preset value.
10. The supercritical fluid preparation method according to claim 9, further comprising:
controlling the temperature of the gas output from the gas source to be less than a critical temperature by a first temperature controller;
and controlling, by a second temperature controller, a temperature within the fluid storage container to be greater than the critical temperature.
11. A supercritical mixed fluid preparation apparatus, comprising:
at least two supercritical fluid preparation apparatuses according to any one of claims 1 to 8;
a mixing vessel for connecting at least two of the second channels in the supercritical fluid preparation apparatus;
a third temperature controller for controlling the temperature within the mixing vessel;
and a third passage for outputting the supercritical fluid in the mixing vessel to the outside.
12. The supercritical mixed fluid preparation apparatus according to claim 11, further comprising:
a tank pressure control valve for discharging the fluid in the mixing vessel in case the pressure in the mixing vessel is above a threshold value.
13. The supercritical mixed fluid preparation apparatus according to claim 11 wherein the third temperature controller comprises:
a second GM refrigerator having a refrigeration head in thermal contact with the mixing vessel;
a third heater is located in the mixing vessel to control the temperature within the mixing vessel.
14. The supercritical mixed fluid preparation apparatus according to any one of claims 11 to 13, further comprising:
the second vacuum cavity capable of forming a vacuum environment, wherein the fluid storage container, the mixing container and the second channel in the supercritical fluid preparation device are all positioned in the vacuum cavity of the second vacuum cavity, and the first temperature controller, the third temperature controller, the first channel and part of the third channel are positioned in the vacuum cavity of the second vacuum cavity.
15. A method for preparing a supercritical mixed fluid, applied to the supercritical mixed fluid preparation apparatus as claimed in any one of claims 11 to 14, comprising:
the pressure in the mixing container is controlled to be a third preset value larger than the critical pressure through a tank pressure control valve;
and discharging the fluid in the mixing container through a tank pressure control valve, so that the pressure in the mixing container is larger than the critical pressure by a fourth preset value, and the fourth preset value is smaller than the third preset value.
16. The method of preparing a supercritical mixed fluid according to claim 15, further comprising:
setting the temperature of the refrigeration head of the second GM refrigerator to be less than a critical temperature;
the temperature in the mixing vessel is controlled to be greater than the critical temperature by a third heater.
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