CN105771310B - Experimental device and method for extraction and phase balance by using pressurized and easily-liquefied gas - Google Patents
Experimental device and method for extraction and phase balance by using pressurized and easily-liquefied gas Download PDFInfo
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- CN105771310B CN105771310B CN201610296323.9A CN201610296323A CN105771310B CN 105771310 B CN105771310 B CN 105771310B CN 201610296323 A CN201610296323 A CN 201610296323A CN 105771310 B CN105771310 B CN 105771310B
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- 238000000605 extraction Methods 0.000 title claims abstract description 50
- 239000002904 solvent Substances 0.000 claims abstract description 92
- 238000002474 experimental method Methods 0.000 claims abstract description 23
- 239000011343 solid material Substances 0.000 claims abstract description 15
- 238000000926 separation method Methods 0.000 claims description 54
- 239000007788 liquid Substances 0.000 claims description 50
- 239000000463 material Substances 0.000 claims description 27
- 238000000034 method Methods 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 239000007787 solid Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims 1
- 239000011344 liquid material Substances 0.000 abstract description 12
- 238000005259 measurement Methods 0.000 abstract description 4
- 238000007789 sealing Methods 0.000 description 17
- 238000004891 communication Methods 0.000 description 14
- 238000003825 pressing Methods 0.000 description 11
- 239000002184 metal Substances 0.000 description 9
- 229910052751 metal Inorganic materials 0.000 description 9
- 230000001276 controlling effect Effects 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 5
- 238000001704 evaporation Methods 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
- 230000003068 static effect Effects 0.000 description 4
- 230000008020 evaporation Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 238000005056 compaction Methods 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 238000003815 supercritical carbon dioxide extraction Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003139 buffering effect Effects 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 230000010349 pulsation Effects 0.000 description 1
- 238000000194 supercritical-fluid extraction Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0203—Solvent extraction of solids with a supercritical fluid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/028—Flow sheets
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0292—Treatment of the solvent
- B01D11/0296—Condensation of solvent vapours
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
- B01D11/0403—Solvent extraction of solutions which are liquid with a supercritical fluid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
- B01D11/0484—Controlling means
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
- B01D11/0488—Flow sheets
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Extraction Or Liquid Replacement (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The invention relates to an experimental device for extracting and balancing by using pressurized and easily-liquefied gas, which comprises a solvent tank, a refrigerator, a high-pressure pump, a balancing tank and a separating tank which are connected in an annular mode sequentially through pipelines, wherein a charging barrel is detachably arranged in the balancing tank, and an extraction area separated by a filter plate is arranged in the charging barrel. The invention also provides an experimental method for extracting and balancing phases by using the pressurized and easily-liquefied gas, aiming at solid materials or liquid materials, the charging barrel is selectively arranged or not arranged in the balancing tank, and the experimental method is suitable for extracting or balancing phases of solid or liquid materials, and has the advantages of simple structure, high experimental efficiency and high measurement precision.
Description
Technical Field
The invention relates to the technical field of subcritical extraction, in particular to an experimental device and method for carrying out extraction and phase balance by using pressurized and easily-liquefied gas.
Background
Supercritical carbon dioxide has become one of the most commonly used supercritical fluids because of its characteristics of no toxicity, no harm, low cost, no pollution to the environment, etc. Although the supercritical carbon dioxide extraction technology has a plurality of advantages, the problem of overhigh equipment cost caused by higher operation pressure limits the industrial application of the supercritical carbon dioxide extraction technology. Therefore, a new technology for green, low-consumption and efficient extraction is sought, and the technology becomes a research hot spot in the field of extraction in recent years. In recent years, techniques for extraction using pressurized liquefied gas have been developed, which are also commonly referred to as "subcritical" extraction techniques. As a potential scheme for replacing the supercritical extraction technology, the subcritical extraction technology has been developed under the efforts of scientific researchers at home and abroad. In order to realize industrialization of subcritical extraction technology, process indexes and equipment designs of subcritical solvent (pressurized liquefied gas) extraction form are established, research is conducted, and phase balance parameters in the extraction process are determined to be key to research. The experimental device for researching subcritical extraction and phase equilibrium determination at present has the defects of single function, complex structure, low efficiency and the like, and is mainly applicable to single solid or liquid materials.
Disclosure of Invention
The invention aims to provide an experimental device for extraction and phase balance by using pressurized and easily-liquefied gas, which can be suitable for extraction or phase balance experiments of solid or liquid materials, and has the advantages of simple structure, high experimental efficiency and high measurement accuracy. The invention also provides an experimental method for extraction and phase balance by using the pressurized and easily-liquefied gas.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows: the experimental device for carrying out extraction and phase balance by utilizing pressurized and easily-liquefied gas comprises a solvent tank, a refrigerator, a high-pressure pump, a balance tank and a separation tank which are connected in an annular mode sequentially through pipelines, wherein valves for controlling the on-off of the pipelines are arranged between the solvent tank and the refrigerator, between the high-pressure pump and the balance tank, between the balance tank and the separation tank and between the separation tank and the solvent tank, and water bath jackets are arranged on the balance tank and the separation tank; the upper end filter and the lower end filter are respectively arranged at the upper end and the lower end of the charging barrel, a solid material extraction area is formed in the charging barrel in an area between the upper end filter and the lower end filter, and liquid distribution holes are formed in the side face of the upper part of the charging barrel, which is positioned at the upper end filter.
According to the scheme, the preheating tank is further arranged between the high-pressure pump and the balancing tank, the high-pressure pump is connected with the preheating tank through the pipeline and the valve, and the preheating tank is connected with the balancing tank through the pipeline and the valve.
According to the scheme, the buffer tank, the compressor and the condenser are sequentially connected between the separation tank and the solvent tank, the separation tank is connected with the buffer tank through the pipeline and the valve, the buffer tank is connected with the compressor through the pipeline and the valve, the compressor is connected with the condenser through the pipeline and the valve, and the condenser is connected with the solvent tank through the pipeline and the valve.
According to the scheme, the device further comprises a vacuum pump, wherein the vacuum pump is connected with the balance tank, the separation tank, the preheating tank, the buffer tank and the condenser through pipelines and valves respectively.
According to the scheme, the bottom of the separation tank is detachably provided with the sample collector through threaded fit, and the sample collector can be selected and installed according to different capacities.
The invention provides a method for carrying out extraction and phase equilibrium experiments by using pressurized and easily-liquefied gas, which is characterized by comprising the following steps:
determining whether to install the material cylinder in the balance tank according to the state of the extracted material, and installing the material cylinder into the balance tank when the material is solid, and not installing the material cylinder into the balance tank when the material is liquid;
starting a refrigerator and a high-pressure pump, so that the solvent in the solvent tank is refrigerated and then is conveyed into the balance tank through the high-pressure pump, and the solute in the balance tank is extracted;
the solution from which the solute is extracted enters a separation tank for solvent and solute separation, the solute remains in the separation tank, and the solvent is transported to the solution tank again.
According to the scheme, before the solvent is conveyed to the balance tank, the solvent is conveyed to the preheating tank for preheating.
According to the scheme, before the solution separated from the separating tank enters the solvent tank, the solution is buffered through the buffer tank, pressurized through the compressor, cooled through the condenser and then conveyed into the solvent tank.
According to the scheme, before the refrigerator and the high-pressure pump are started, the vacuum pump is started to vacuumize the preheating tank, the balance tank, the separation tank, the buffer tank and the condenser.
According to the scheme, before the refrigerator and the high-pressure pump are started, the sample collector with proper capacity is selected and installed at the bottom of the separation tank.
According to the experimental device and method for extracting and balancing by using the pressurized and easily-liquefied gas, the detachably-installed charging barrel is designed in the balancing tank, and the two ends of the charging barrel are provided with the filter plates, so that an extraction area is formed between the filter plates in the charging barrel, and when solid materials are extracted, the materials can be directly placed in the extraction area of the charging barrel, and then the charging barrel is placed in the balancing tank for an extraction procedure; when extracting liquid materials, take the feed cylinder out from the balance tank, directly use the internal space of the balance tank as the extraction area to extract the materials. Therefore, the experimental device and the method can be suitable for extraction or phase balance experiments of solid or liquid materials, and have the advantages of simple structure, high experimental efficiency and high measurement accuracy.
Drawings
FIG. 1 is a schematic diagram of the structure of the present invention;
FIG. 2 is a schematic diagram of the tank structure of the balancing tank of the present invention;
FIG. 3 is a schematic diagram of the cartridge structure of the surge tank of the present invention;
FIG. 4 is a schematic diagram of an assembled structure of the balance tank of the present invention;
fig. 5 is a schematic structural view of the separator tank of the present invention.
In the figure: 10. a solvent tank; 20. a refrigerating machine; 30. a high pressure pump; 40. a balancing tank; 50. a separation tank; 60. a preheating tank; 70. a buffer tank; 80. a compressor; 90. a condenser; 100. and a vacuum pump.
Detailed Description
The technical scheme of the invention is described below with reference to the accompanying drawings and examples.
As shown in fig. 1 and 2, the experimental device for extracting and balancing by using pressurized and easily-liquefied gas comprises a solvent tank 10, a refrigerator 20, a high-pressure pump 30, a balancing tank 40 and a separating tank 50 which are connected in an annular manner sequentially through pipelines, wherein valves for controlling the on-off of the pipelines are arranged between the solvent tank 10 and the refrigerator 20, between the high-pressure pump 30 and the balancing tank 40, between the balancing tank 40 and the separating tank 50 and between the separating tank 50 and the solvent tank 10, water bath jackets are arranged on the balancing tank 40 and the separating tank 50, the balancing tank comprises a tank body 42, a top cover 43 and a charging barrel 44, and the charging barrel 44 is detachably inserted into the tank body 42 and is installed in the tank body 42 in a pressing manner through the top cover 43; the upper end and the lower end of the charging barrel 44 are respectively provided with an upper end filter plate 444 and a lower end filter plate 447, a solid material extraction area is formed in the charging barrel in an area between the upper end filter plate 444 and the lower end filter plate 447, and a liquid distribution hole 446 is formed in the side face of the upper end of the charging barrel 44, which is located above the upper end filter plate 444. The experimental device and the method can be suitable for extraction or phase balance experiments of solid or liquid materials, and have the advantages of simple structure, high experimental efficiency and high measurement accuracy.
Preferably, a magnetic stirrer 41 is installed at the bottom of the balancing tank 40 to stir the solution in the balancing tank 40, so as to increase the dissolution speed and the extraction efficiency.
Preferably, a preheating tank 60 is further disposed between the high-pressure pump 30 and the balancing tank 40, the high-pressure pump 30 is connected with the preheating tank 60 through a pipeline and a valve, and the preheating tank 60 is connected with the balancing tank 40 through a pipeline and a valve, so that the temperature of the solution is raised to a certain extent before the solution enters the balancing tank 40, and the extraction efficiency is also improved. The preheating structure of the preheating tank 60 can also be performed by means of a water bath jacket.
Preferably, the buffer tank 70, the compressor 80 and the condenser 90 are sequentially connected between the separation tank 50 and the solvent tank 10, the separation tank 50 is connected with the buffer tank 70 through a pipeline and a valve, the buffer tank 70 is connected with the compressor 80 through a pipeline and a valve, the compressor 80 is connected with the condenser 90 through a pipeline and a valve, and the condenser 90 is connected with the solvent tank 10 through a pipeline and a valve, so that the separated solvent is compressed and cooled from a gas state to a liquid state before entering the solvent tank 10, and the solvent is convenient for recycling.
Preferably, the vacuum pump 100 is further included, and the vacuum pump 100 is respectively connected to the balancing tank 40, the separation tank 50, the preheating tank 60, the buffer tank 70 and the condenser 90 through pipes and valves, and the balancing tank 40, the separation tank 50, the preheating tank 60, the buffer tank 70 and the condenser 90 are all vacuumized between the extraction processes, so that the solution flow is facilitated, and the extraction efficiency is improved.
Preferably, the bottom of the separation tank 50 is detachably provided with a sample collector 53 through screw thread fit, the sample collector 53 can be selected and installed according to different capacities, and according to experimental conditions, the capacity of the sample collector is changed to match the actual solute amount by connecting sample collectors with different lengths, so that blank quality can be reduced, and metering accuracy can be increased.
Meanwhile, the invention provides a method for carrying out extraction and phase balance experiments by using pressurized and easily-liquefied gas, which comprises the following steps:
determining whether to install the material cylinder 44 in the balance tank 40 according to the state of the extracted material, and installing the material cylinder 44 in the balance tank 40 when the material is in a solid state, and not installing the material cylinder 44 in the balance tank 40 when the material is in a liquid state;
starting the refrigerator 20 and the high-pressure pump 30, so that the solvent in the solvent tank 10 is refrigerated and then is conveyed into the balance tank 40 through the high-pressure pump 30, and the solute in the balance tank 40 is extracted;
the solution from which the solute is extracted enters the separator tank 50 for solvent and solute separation, the solute remains in the separator tank 50, and the solvent is again transferred to the solvent tank 10.
Therefore, the experimental device and the method can be suitable for extraction experiments of solid or liquid materials, and have simple structure and high extraction efficiency.
When the solvent enters the balance tank 40 to extract the solute, the magnetic stirrer 41 is started to stir the solution in the balance tank 40, so that the extraction efficiency is improved.
According to the above scheme, before the solvent is conveyed to the balancing tank 40, the solvent is conveyed to the preheating tank 60 for preheating, so that the temperature of the solution is raised to a certain extent before the solution enters the balancing tank 40, and the extraction efficiency can be also improved.
According to the above scheme, the solution separated from the separation tank 50 is buffered by the buffer tank 70 before entering the solvent tank 10, pressurized by the compressor 80, cooled by the condenser 90 and then conveyed into the solvent tank 10, so that the separated solvent is compressed and cooled before entering the solvent tank 10, and is changed from a gas state to a liquid state, thereby facilitating the recycling of the solvent.
According to the above scheme, before starting the refrigerator 20 and the high pressure pump 30, the vacuum pump 100 is started to vacuumize the balance tank 40, the separation tank 50, the preheating tank 60, the buffer tank 70 and the condenser 90, which is beneficial to the flow of solution and improves the extraction efficiency.
According to the above scheme, before the refrigerator 20 and the high-pressure pump 30 are started, the sample collector 53 with proper capacity is selected and installed at the bottom of the separation tank, and according to experimental conditions, the sample collectors with different lengths can be connected, so that the capacity of the sample collector can be changed to match the quantity of the actual solute, and the blank mass can be reduced to increase the metering precision.
According to the experimental device and method for extracting and balancing by using pressurized and easily-liquefied gas, the detachably-installed charging barrel 44 is designed in the balancing tank 40, and the two ends of the charging barrel 44 are provided with the filter plates, so that an extraction area is formed between the filter plates in the charging barrel, and when solid materials are extracted, the materials can be directly placed in the extraction area of the charging barrel 44, and then the charging barrel 44 is placed in the balancing tank 40 for an extraction procedure; in extracting the liquid material, the material cylinder 44 is taken out from the balance tank 40, and the material is extracted by directly using the inner space of the tank body 42 of the balance tank 40 as an extraction area.
The present invention will be described in detail with reference to a specific embodiment.
As shown in fig. 1, the experimental apparatus of the present invention includes a solvent tank 10, a refrigerator 20, a high pressure pump 30, a preheating tank 60, a balancing tank 40, a separation tank 50, a vacuum pump 100, a buffer tank 70, a compressor 80, and a condenser 90, which are connected in a loop formed by pipes in sequence; the liquid outlet at the bottom of the solvent tank 10 is connected with the liquid inlet of the refrigerator 20, and is provided with a valve A for controlling the communication state; the liquid outlet of the refrigerator 20 is connected with the liquid inlet of the high-pressure pump 30, the liquid outlet of the high-pressure pump 30 is connected with the liquid inlet on the side surface of the upper part of the preheating tank 60, and a valve B is arranged to control the communication state of the high-pressure pump 30; the liquid outlet at the bottom of the preheating tank 60 is connected with the liquid inlet at the side surface of the upper part of the balance tank 40, and a valve C is arranged to control the communication state of the liquid inlet; the liquid outlet on the side surface of the lower part of the balance tank 40 is connected with the liquid inlet on one side of the upper part of the separation tank 50, a valve D is arranged to control the communication state of the liquid outlet, the liquid inlet of the balance tank 40 is also connected with the air outlet on the other side of the upper part of the separation tank 50, and a valve N is arranged to control the communication state of the liquid inlet; the air outlet on the other side of the upper part of the separating tank 50 is connected with the air inlet on the side surface of the upper part of the buffer tank 70, and is provided with a valve E for controlling the communication state; the air outlet on the side surface of the lower part of the buffer tank 70 is connected with the air inlet of the compressor 80, and is provided with a valve F for controlling the communication state; the air outlet of the compressor 80 is connected with the air inlet at the left side of the top of the condenser 90, and is provided with a valve G for controlling the communication state; the liquid outlet on the right side of the bottom of the condenser 90 is connected with the liquid inlet on the top of the solvent tank 10, a valve H is arranged to control the communication state of the liquid outlet, the vent on the right side of the top of the condenser 90 is connected with the liquid inlet on one side of the upper part of the separation tank 50, a valve J is arranged to control the communication state of the liquid outlet, the vent on the right side of the top of the condenser 90 is also communicated with the atmosphere through a pipeline, and a valve I is arranged to control the communication state of the vent; the air outlet at one side of the upper part of the separating tank 50 is also connected with the air inlet of the vacuum pump 100, and is provided with a valve K for controlling the communication state; the air outlet of the vacuum pump 100 is connected with the air inlet of the buffer tank 70, a valve L is arranged to control the communication state of the air inlet, the air outlet of the vacuum pump 100 is communicated with the atmosphere through a pipeline, and a valve M is arranged to control the communication state of the air outlet.
As shown in fig. 2, the balancing tank specifically includes a tank body 42, a top cover 43, and a cartridge 44. The tank body 42 is provided with a water bath jacket 45, a liquid inlet pipe 46 and a liquid outlet pipe 47; the lower end of the tank body 42 of the balance tank is closed, the upper end of the tank body is open, a flange 48 matched with the top cover 43 is arranged at the opening, upper and lower grooves for accommodating sealing rings are correspondingly arranged on the flange 48 and the top cover 43, an O-shaped sealing ring 49 can be fit into the grooves, and an airtight space is formed inside the balance tank 40 by fastening bolts and nuts connected to the top cover 43 and the flange 48; a cylindrical groove is formed in the center of the bottom of the tank body 42, so that an annular boss is formed at the bottom close to the side wall of the tank body 42, and an annular sealing ring groove is formed in the boss; a magnetic stirrer 411 is arranged on the groove at the bottom of the tank body 42 and can be driven to rotate by the traction of the magnetic stirrer 41 below the bottom of the balance tank 40; the water bath jacket 45 is provided with a liquid inlet 451 and a liquid outlet 452, and hot water can be introduced to adjust the temperature in the balance tank 40; the top cover 43 of the balance tank 40 is provided with a pressure gauge P which can monitor the pressure in the tank body 42, and the lower part of the balance tank 40 is provided with a thermometer T which can monitor the temperature in the tank body 42; the material cylinder 44 can be placed in the balance tank 40, and a strip-shaped window is arranged on the outer wall of the tank body 42, so that the internal condition of the balance tank 40 can be observed through the window.
As shown in fig. 3, the cartridge 44 includes a cylinder body 441, an upper compression cap 442, and a lower compression cap 443; the upper pressing screw cap 442 is in a tubular structure and penetrates up and down, one end of the outer side of the cylinder wall is provided with threads, and the unthreaded part of the cylinder wall is symmetrically provided with liquid distribution holes 446; the lower pressing spiral cover 443 is vertically penetrated to form a cylindrical structure, one end of the outer side of the cylinder wall is provided with threads, and the bottom of the non-threaded end is provided with an annular sealing ring groove; the cylinder 441 is open up and down, and the inner sides of the upper opening and the lower opening are provided with threads which are respectively matched with the threads of the upper pressing screw cap 442 and the lower pressing screw cap 443; the screw thread end of the inner side of the upper and lower ends of the cylinder 441 is respectively provided with an annular shelf, one side of the upper and lower shelves, which is close to the screw thread, is sequentially provided with an annular sealing washer 445, a metal filter plate 444, an annular sealing washer 448 and a metal filter plate 447, which are respectively compacted by the screwed upper compaction screw cap 442 and the lower compaction screw cap 443, so that a relatively independent space is formed between the inside of the cylinder 441 and the two metal filter plates 444 and 447, and the cylinder can only communicate with the outside through fine sieve holes of the two metal filter plates.
As shown in fig. 4, the cartridge 44 may be placed on the bottom boss of the balance tank 40, an O-ring is placed between the annular seal ring groove on the lower pressing screw cap 443 of the cartridge 44 and the annular seal ring groove on the bottom boss of the balance tank 40, the cartridge 44 is lifted by the O-ring, and the upper end plane is slightly higher than the plane of the top flange 48 of the balance tank 40, so that the solvent entering from the liquid inlet pipe 46 can only reach the metal filter plate 444 through the liquid distribution hole 446 of the upper pressing screw cap 442 of the cartridge 44, pass through the filter hole into the cartridge 44, and then flow out through the metal filter plate 447 to the liquid outlet pipe 47.
As shown in fig. 5, the separation tank 50 comprises a cylinder 51 and an upper screw cap 52, and a sample receiver 53 is screw-mounted at the bottom of the cylinder 51; the sample collector 53 is in a slender tubular shape, the bottom end is closed, the upper end is open, threads are arranged on the outer side of the upper end, a plurality of sample collectors are distinguished according to different capacities, according to experimental conditions, the capacity of the sample collector is changed to match the quantity of actual solutes by connecting sample collectors with different lengths, and the blank mass can be reduced to increase the metering precision; the bottom of the cylinder body 51 is conical, a threaded opening is formed in the center of the bottom and is matched with threads of the sample receiver 53, and a sealing gasket 58 is arranged between the sample receiver 53 and the threaded opening and is used for keeping the air tightness of the connection of the sample receiver 53 and the separation tank 50; the outside of the cylinder body 51 is provided with a water bath jacket 54, and the upper part of the cylinder body 51 is provided with a liquid inlet pipe 55 and a gas outlet pipe 56; the liquid inlet pipe 55 is bent downwards at the center of the cylinder body 51 at 90 degrees after penetrating through the cylinder body and extends to the conical opening at the bottom of the cylinder body 51, so that the phenomenon that solute is stuck on the wall of the separation tank 50 during reduced pressure evaporation can be avoided in the extraction process, and the solute recovery is complete and the metering accuracy is ensured; the water bath jacket 55 is provided with a liquid inlet 541 and a liquid outlet 542, and hot water can be introduced to adjust the temperature in the separation tank 50; the inner side of the upper part of the cylinder 51 of the separating tank 50 is provided with a thread, the lower part of the thread is provided with an annular shelf, the shelf is provided with an annular sealing gasket 57, and after the upper screw cap 52 is screwed into the thread on the inner side of the cylinder 51, the sealing gasket 57 can be pressed tightly so as to keep the air tightness of the separating tank 50; the upper spiral cover 52 of the separating tank 50 is provided with a pressure gauge P which can monitor the pressure in the tank body, and the lower part of the separating tank 50 is provided with a temperature gauge T which can monitor the temperature in the tank body 51.
Further, the high-pressure pump 30 is preferably an HPLC pump, the vacuum pump 100 is preferably a claw-type dry vacuum pump, the compressor 80 is preferably a diaphragm compressor, and the flow meter is preferably a mass flow meter; the preheating tank 60, the balancing tank 40 and the separation tank 50 are preferably made of stainless steel, and the maximum withstand pressure is 20MPa; the mesh diameter of the metal filter plates 444 and 447 in the cartridge 44 is 100-200 mesh; the buffer tank 70 is filled with stainless steel ripple or annular filler, so that air flow pulsation caused by the operation of the vacuum pump is greatly reduced, the air flow stably flows through the mass flowmeter, and the metering accuracy is ensured.
During the solid material extraction and phase balance experiment, the solid material to be tested is crushed, weighed and then is put into a charging barrel 44, and an upper pressing screw cap 442 and a lower pressing screw cap 443 are screwed; placing an O-shaped sealing ring on the sealing ring groove of the boss at the bottom of the balance tank 40, and then placing the charging barrel 44 on the boss at the bottom of the balance tank 40, so that the annular sealing ring groove on the lower pressing spiral cover 443 of the charging barrel 44 is matched with the sealing ring; placing an O-shaped sealing ring 49 in a sealing ring groove of a flange 48 of the balance tank 40, covering the top cover 43, and fastening bolts and nuts connected with the top cover 43 and the flange 48 to form an airtight space inside the balance tank 40; opening a valve M, starting a vacuum pump, sequentially opening valves C, E, J, K and N, vacuumizing the preheating tank 60, the balance tank 40, the separation tank 50, the buffer tank 70 and the condenser 90, and sequentially closing the valves and the vacuum pump 100 according to the principle of opening and closing afterwards; circulating water with a certain temperature is respectively introduced into the water bath jackets of the preheating tank 60, the balancing tank 40 and the separating tank 50 to adjust the internal temperature of each tank.
The valve A of the solvent tank 10 is opened to discharge the solvent (namely, pressurized and easily-liquefied gas), the solvent is cooled to a certain temperature by the refrigerator 30, the solvent flows into the high-pressure pump 30 in a liquid state completely, the solvent is conveyed into the preheating tank 60 for a certain time by pressurization, the temperature and the pressure of the solvent are regulated to a preset temperature and pressure, the solvent is conveyed into the balance tank 40 by the liquid inlet pipe 46 through the valve C, the solvent flows in through the liquid distribution hole 446 on the upper pressing rotary cover 442, passes through the metal filter plate 444, enters an extraction area in the feed cylinder 44, contacts with materials, and then passes through the metal filter plate 447 and flows out of the balance tank 40 through the liquid outlet pipe 47.
Opening a valve D to allow the solvent carrying the solute to flow into the separation tank 50, simultaneously opening a valve E, F, G, H and starting a compressor 80, performing reduced pressure evaporation on the solvent in the separation tank 50, allowing the solvent to enter from a liquid inlet pipe 55 of the separation tank 50, evaporating at the tail end of the liquid inlet pipe 55, and collecting the solute precipitation by a sample collector 53; the solvent is gasified and then flows into the mass flowmeter G through the buffer tank 70 in a buffering and stable manner, the solvent enters the compressor 80 after being metered in mass, flows through the condenser 90 after being compressed, and returns to the solvent tank 10 after being condensed and liquefied; after the experiment was completed, the sample collector 53 was removed and weighed, and the mass of the collected solute was obtained from the difference in the front and rear masses.
When a two-phase balance experiment of liquid materials is carried out, firstly, the charging barrel 44 is taken out of the balance tank 40, then the liquid materials are filled into the tank body 42 of the balance tank 40, an O-shaped sealing ring 49 is placed in a sealing ring groove of the flange 48 of the balance tank 40, the top cover 43 is covered, and bolts and nuts which are connected with the top cover 43 and the flange 48 are fastened, so that an airtight space is formed inside the balance tank 40; opening a valve M, starting a vacuum pump, sequentially opening valves C, E, J, K and N, vacuumizing the preheating tank 60, the balance tank 40, the separation tank 50, the buffer tank 70 and the condenser 90, and sequentially closing the valves and the vacuum pump 100 according to the principle of opening and closing afterwards; circulating water with a certain temperature is respectively introduced into the water bath jackets of the preheating tank 60, the balancing tank 40 and the separating tank 50 to adjust the internal temperature of each tank.
Opening valve A of solvent tank 10 to discharge solvent (pressurized easy-to-liquefy gas), cooling the solvent to a certain temperature by refrigerator 20, making the solvent flow into high-pressure pump 30 completely in liquid state, pressurizing and conveying to preheating tank 60 for a certain time, making solvent temperature and pressure regulated to preset temperature and pressure, opening valve C to convey solvent into balancing tank 40 by liquid inlet pipe 46, observing and shooting two-phase balancing condition by long-strip window, and slowly discharging solvent out of balancing tank 40 by liquid outlet pipe 47 after experiment.
Opening a valve D to allow the solvent carrying the solute to flow into the separation tank 50, simultaneously opening a valve E, F, G, H and starting a compressor 80, performing reduced pressure evaporation on the solvent in the separation tank 50, allowing the solvent to enter from a liquid inlet pipe 55 of the separation tank 50, evaporating at the tail end of the liquid inlet pipe 55, and collecting the solute precipitation by a sample collector 53; the solvent is gasified and then steadily flows into a mass flowmeter G through a buffer tank buffer 50, the solvent enters a compressor 80 after being metered in mass, and flows through a condenser 90 after being compressed, and returns to the solvent tank 10 after being condensed and liquefied; after the experiment was completed, the sample collector 53 was removed and weighed, and the mass of the collected solute was obtained from the difference in the front and rear masses.
Either in the extraction of solid materials or in the two-phase equilibrium experiments of liquid materials, static or dynamic experiments can be used. When the static phase balance experiment is carried out, the solvent is required to be sent into the balance tank 40 by the high-pressure pump 30 to reach a preset amount, then the pumping is stopped, the magnetic stirrer 41 is started at the moment, the static phase balance experiment is carried out, after the balance time is reached, the stirring is stopped, the static phase balance experiment is kept for a period of time, the lower solvent is put into the separation tank 50 for recovery and metering, and the solubility of the solute in the solvent can be conveniently calculated according to the mass of the weighed material, the mass of the metered solvent and the mass of the collected solvent. When the dynamic phase balance experiment is performed, the solvent is required to be sent into the balance tank 40 through the high-pressure pump 30, the pumping flow of the high-pressure pump 30 is adjusted to reach a preset value, the solvent amount entering and exiting the balance tank 40 is stable, the height of the two-phase interface is kept unchanged, the solvent is recovered at the same time, the experiment is stopped after the preset time is reached, and the solubility of the solute in the solvent can be conveniently calculated according to the mass of the weighed material, the mass of the metered solvent and the collected solvent mass.
The foregoing description is only of the preferred embodiments of the invention, and all changes and modifications that come within the meaning and range of equivalency of the structures, features and principles of the invention are therefore intended to be embraced therein.
Claims (8)
1. The experimental device for carrying out extraction and phase balance by utilizing pressurized and easily-liquefied gas comprises a solvent tank, a refrigerator, a high-pressure pump, a balance tank and a separation tank which are connected in an annular mode sequentially through pipelines, wherein valves for controlling the on-off of the pipelines are arranged between the solvent tank and the refrigerator, between the high-pressure pump and the balance tank, between the balance tank and the separation tank and between the separation tank and the solvent tank, and water bath jackets are arranged on the balance tank and the separation tank; the upper end and the lower end of the charging barrel are respectively provided with an upper end filter plate and a lower end filter plate, a solid material extraction area is formed in the charging barrel in the area between the upper end filter plate and the lower end filter plate, and liquid distribution holes are formed in the side face of the upper end of the charging barrel, which is positioned above the upper end filter plate;
a preheating tank is further arranged between the high-pressure pump and the balancing tank, the high-pressure pump is connected with the preheating tank through a pipeline and a valve, and the preheating tank is connected with the balancing tank through a pipeline and a valve; the bottom of the separation tank is detachably provided with a sample collector through threaded fit.
2. The experimental device for extraction and phase equilibrium by using pressurized and easily liquefied gas according to claim 1, wherein a buffer tank, a compressor and a condenser are sequentially connected between the separation tank and the solvent tank, the separation tank is connected with the buffer tank through a pipeline and a valve, the buffer tank is connected with the compressor through a pipeline and a valve, the compressor is connected with the condenser through a pipeline and a valve, and the condenser is connected with the solvent tank through a pipeline and a valve.
3. The apparatus according to claim 2, further comprising a vacuum pump connected to the balance tank, the separation tank, the preheating tank, the buffer tank and the condenser through pipes and valves, respectively.
4. A method for carrying out extraction and phase equilibrium experiments by using pressurized and easily liquefied gas, characterized in that the experimental device according to any one of claims 1-3 is used, and specifically comprises the following steps:
determining whether to install the material cylinder in the balance tank according to the state of the extracted material, and installing the material cylinder into the balance tank when the material is solid, and not installing the material cylinder into the balance tank when the material is liquid;
starting a refrigerator and a high-pressure pump, so that the solvent in the solvent tank is refrigerated and then is conveyed into the balance tank through the high-pressure pump, and the solute in the balance tank is extracted;
the solution from which the solute is extracted enters a separation tank for solvent and solute separation, the solute remains in the separation tank, and the solvent is transported to the solution tank again.
5. The method of claim 4, wherein the solvent is preheated in a preheating tank before the solvent is fed to the balancing tank.
6. The method for extraction and phase equilibrium experiments using a pressurized, easily liquified gas of claim 5, wherein the solution separated from the separator is buffered in a buffer tank, pressurized in a compressor, cooled in a condenser and then transferred to the solvent tank before entering the solvent tank.
7. The method of claim 6, wherein the pre-heating tank, the balancing tank, the separation tank, the buffer tank and the condenser are evacuated by starting the vacuum pump before starting the refrigerator and the high pressure pump.
8. The method of claim 4, wherein the sample collector is mounted to the bottom of the separation tank prior to starting the refrigerator and the high pressure pump.
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