CN113155886A - Visual experiment device and measurement method for determining VLE - Google Patents
Visual experiment device and measurement method for determining VLE Download PDFInfo
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- CN113155886A CN113155886A CN202110349207.XA CN202110349207A CN113155886A CN 113155886 A CN113155886 A CN 113155886A CN 202110349207 A CN202110349207 A CN 202110349207A CN 113155886 A CN113155886 A CN 113155886A
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- 230000000007 visual effect Effects 0.000 title claims abstract description 96
- 238000002474 experimental method Methods 0.000 title claims abstract description 39
- 238000000691 measurement method Methods 0.000 title claims description 4
- 238000006243 chemical reaction Methods 0.000 claims abstract description 89
- 238000005070 sampling Methods 0.000 claims abstract description 64
- 239000003507 refrigerant Substances 0.000 claims abstract description 57
- 239000007791 liquid phase Substances 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 22
- 239000005388 borosilicate glass Substances 0.000 claims abstract description 10
- 239000011521 glass Substances 0.000 claims abstract description 3
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 44
- 229910052697 platinum Inorganic materials 0.000 claims description 22
- 239000010687 lubricating oil Substances 0.000 claims description 19
- 239000000203 mixture Substances 0.000 claims description 11
- 238000003760 magnetic stirring Methods 0.000 claims description 7
- 239000012071 phase Substances 0.000 claims description 6
- 238000007789 sealing Methods 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000010726 refrigerant oil Substances 0.000 claims description 3
- 238000012360 testing method Methods 0.000 claims description 2
- 230000003068 static effect Effects 0.000 abstract description 9
- 239000007789 gas Substances 0.000 description 22
- 239000007788 liquid Substances 0.000 description 4
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 238000012800 visualization Methods 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 2
- 238000011010 flushing procedure Methods 0.000 description 2
- 239000000314 lubricant Substances 0.000 description 2
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 238000009530 blood pressure measurement Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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Abstract
The invention discloses a visual experimental device for determining VLE (very low-temperature orientation), which comprises a visual reaction kettle, a visual high-precision thermostatic bath, a sample tank, a vacuum pump, a temperature measuring system, a pressure measuring system and a vapor-liquid phase sampling system, wherein the visual reaction kettle is respectively connected with the sample tank and a gas chromatograph through pipelines; the front side of the visual high-precision thermostatic bath adopts a high borosilicate glass window, and the layering condition of the reaction kettle in the experiment is directly observed through the glass window; the temperature measuring system and the pressure measuring system are respectively connected with the visual reaction kettle and the visual high-precision thermostatic bath, and the vacuum pump is connected with the visual reaction kettle; the vapor-liquid phase sampling system. The invention also discloses a solubility measuring method and a mixed refrigerant vapor-liquid phase equilibrium data measuring method. The sampling system is additionally arranged on a static method for solubility, so that the sampling system is applied to two conditions, and the precision of vapor-liquid phase equilibrium experimental data is effectively improved.
Description
Technical Field
The invention relates to the field of refrigerant vapor-liquid phase balance, in particular to an experimental device and a measuring method capable of measuring solubility of refrigerant and lubricating oil and vapor-liquid phase balance data of a refrigerant mixture.
Background
The Montreal protocol-Bulgarian amendment, signed by International society, further limits the use of HFCs refrigerants due to environmental warming and ozone depletion issues. Therefore, it is urgent to develop a new environment-friendly refrigerant.
Solubility data of new refrigerants and lubricating oils is a major concern in the development of new refrigerants. If the solubility is too high, the viscosity is reduced, and the lubricating performance of the lubricating oil is affected; and during system operation, the system COP decreases as gaseous refrigerant is absorbed by the lubricating oil. If the miscibility of the refrigerant and the lubricant is poor, the oil return will be poor.
However, in order to meet the environmental protection requirements, the novel refrigerant always has the problems of flammability, poor system efficiency and the like, and the mixed refrigerant can make up for the deficiencies. The solubility and the vapor-liquid phase equilibrium data of the refrigerant mixture belong to the vapor-liquid two-phase data, and the vapor-liquid phase equilibrium data is the basis for developing the research on the refrigerant mixture and has important significance.
The solubility is measured mainly by a static method and a cyclic method. Compared with the static method, the circulation method has limited pressure bearing because the pressure bearing device not only comprises the reaction kettle but also comprises the circulation pipeline; more accessories such as gear pumps and the like are needed; and the insulation of the pipes exposed to the air needs to be taken into account during the circulation. The static law does not have the pressure bearing problem, and for systems that do not require sampling of gas phase components, the liquid phase composition can be predicted from the pvt data. However, the static method cannot analyze the vapor-liquid equilibrium data of the mixed refrigerant. However, if a sampling device is added to the static method, two sets of data can be measured simultaneously.
Disclosure of Invention
The invention aims to improve the defects of the prior art, and provides a visual experimental device and a measurement method for determining VLE (very large volume index), wherein a sampling system is additionally arranged on a static method for solubility, so that the device is applied to two conditions, and the accuracy of vapor-liquid phase balance experimental data is effectively improved.
In order to realize the purpose, the technical scheme of the invention is as follows: a visual experimental device for determining VLE comprises a visual reaction kettle, a visual high-precision thermostatic bath, a sample tank, a vacuum pump, a temperature measuring system, a pressure measuring system and a vapor-liquid phase sampling system;
the front and the back of the visual reaction kettle are respectively provided with a high borosilicate glass window and are respectively connected with the sample tank and the gas chromatograph through pipelines;
the front side of the visual high-precision thermostatic bath adopts a high borosilicate glass window, and the layering condition of the reaction kettle in the experiment is directly observed through the glass window;
the temperature measuring system and the pressure measuring system are respectively connected with the visual reaction kettle and the visual high-precision thermostatic bath, and the vacuum pump is connected with the visual reaction kettle;
the vapor-liquid phase sampling system comprises a small sampling chamber, an expansion chamber and a gas chromatograph;
when a solubility experiment is carried out, the left side and the right side of the first sampling small chamber and the second sampling small chamber are both closed, a refrigerant and lubricating oil are filled into the reaction kettle, the stirring device is started, and when the fluctuation of temperature and pressure is within an uncertainty range, the temperature and the pressure are recorded;
when carrying out refrigerant mixture balance experiment, the side switch is opened to first sampling cell and second sampling cell left side, fills the reation kettle with the refrigerant mixture in, opens agitating unit, when the fluctuation of temperature and pressure is in the uncertainty scope, records temperature, pressure.
Valves are arranged between the sample tank and the visual reaction kettle, between the vacuum pump and the pipeline, between the sampling small chamber and the expansion chamber, and between the expansion chamber and the gas chromatograph;
the control cabinet of the high-precision thermostatic bath comprises a circulating pump, a heating system, a refrigerating system and a temperature control system, and the temperature requirement is met;
the temperature measuring system comprises an upper computer, a data acquisition card, a first platinum resistor and a second platinum resistor; the first platinum resistor is arranged in the thermostatic bath and used for detecting the fluctuation of temperature; the second platinum resistor is arranged in the visual reaction kettle and used for detecting whether the reaction temperature reaches balance or not;
the pressure measuring system comprises a first pressure transmitter and a second pressure transmitter, wherein the first pressure transmitter is connected with the gas distribution pipeline and used for detecting the pressure of the pipeline; and the second pressure transmitter is connected with the visual reaction kettle and is used for measuring pressure data and pressure fluctuation of the visual reaction kettle.
The first sampling small chamber and the second sampling small chamber are positioned at the top and the bottom of the visual reaction kettle and have the same structure.
The first sampling small chamber is bilaterally symmetrical, the first electromagnet on the left side is arranged on the first sliding rail and is reset by the first spring in an unpowered state, and the left side of the small chamber is communicated with the visual reaction kettle; the second electromagnet on the right side is arranged on the second sliding rail and is reset by the second spring in an unpowered state, and the right side of the small chamber is communicated with the expansion chamber.
The second technical scheme of the invention is a method for measuring the solubility of a visual experimental device for determining VLE, which comprises the following steps:
1) before the experiment is started, the sampling small chamber is closed, a valve and a vacuum pump for vacuumizing are opened, the visual reaction kettle is vacuumized and pressure is maintained for 24 hours, and high-purity CO is used2Calibrating the volume of the visual reaction kettle;
2) when the experiment is started, keeping the two sampling small chambers closed, injecting lubricating oil by using an injector, and sealing the visual reaction kettle; opening a valve and a vacuum pump for vacuumizing, and vacuumizing the visual reaction kettle; closing the valves, opening all the valves on the gas distribution pipeline, and filling the refrigerant;
3) in the experimental process, setting the temperature of a thermostatic bath, starting magnetic stirring, observing the balance phenomenon of the visual reaction kettle, and recording the pressure and the temperature;
4) adjusting the temperature of the constant temperature bath, and continuing the next group of experiments;
keeping the sealing of the reaction kettle, vacuumizing the pipeline again, injecting the refrigerant again, and performing solubility experiments of different components;
5) the solubility of the refrigerant in the lubricating oil can be calculated from the formulas (1), (2):
in the formula: m is3Is the total mass of refrigerant flushed in, veIs the molar volume of the refrigerant gas phase at equilibrium, M is the relative molecular mass of the refrigerant, VrIs the volume of the visual reaction kettle, V2Is the volume of lubricating oil dissolved, v1Is the molar volume of the refrigerant liquid phase in equilibrium, m1Is the mass of refrigerant dissolved, m2Is the quality of the lubricating oil that is flushed in.
The third technical scheme of the invention is a method for measuring vapor-liquid phase equilibrium data of a mixed refrigerant of a visual experimental device for determining VLE, which comprises the following steps:
1) before the experiment begins, opening a left channel of a sampling small chamber, closing two right channels for sampling, opening a valve and a vacuum pump for vacuumizing, vacuumizing the visual reaction kettle and maintaining the pressure for 24 hours;
2) when the experiment is started, the left channel and the right channel of the two sampling small chambers, and a valve and a vacuum pump for vacuumizing are opened, and the visual reaction kettle and the whole system pipeline are vacuumized; closing the valve and the two right channels for sampling, opening the gas distribution valve, and filling the system with mixed refrigerant;
3) in the experimental process, setting the temperature of a thermostatic bath, opening a magnetic stirring rod, observing the balance phenomenon of the visual reaction kettle, and recording the pressure and the temperature;
4) at the moment, the left channels of the two sampling small chambers are closed, the right channels and the valves are opened, so that the refrigerant is fully expanded in the expansion chamber, and then the refrigerant is introduced into a gas chromatograph for analysis;
5) and adjusting the temperature of the constant temperature bath, distributing gas again, and continuing the next group of experiments.
Advantageous effects
When the solubility is measured by a static method, the method also stores and analyzes the data of the vapor-liquid phase balance of the mixed refrigerant. The sampling system is additionally arranged on a static method for solubility, so that the sampling system is applied to two conditions, and the precision of vapor-liquid phase equilibrium experimental data is effectively improved.
Drawings
FIG. 1 is a VLE system diagram;
FIG. 2 is a detailed view of a visual reaction vessel;
FIG. 3 is a detail view of a first sampling cell;
figure 4 is a detailed view of the second sampling cell.
Reference numerals: 1 sample tank, 2 first valve, 3 third valve, 4 vacuum pump, 5 first pressure transmitter, 6 upper computer, 7 data acquisition card, 8 first bolt, 9 second valve, 10 second differential pressure transmitter, 11 flange, 12 second bolt, 13 fourth valve, 14 first expansion chamber, 15 sixth valve, 16 gas chromatograph, 17 visual reaction kettle wall, 18 reaction kettle high borosilicate glass window, 19 first platinum resistor, 20 constant temperature bath high borosilicate glass window, 21 high precision constant temperature bath, 22 fifth valve, 23 second expansion chamber, 24 seventh valve, 25 second platinum resistor, 26 visual reaction kettle, 27 blade, 28 magnetic stirring rod, 29 first sampling cell, 30 second sampling cell, 31 first wall, 32 first channel, 33 first electromagnet, 34 first coil, 35 first spring, 36 first slide rail, 37 first slide block, 38 second slide rail, 39 second slide, 40 second spring, 41 second coil, 43 second channel, 44 second wall, 45 third wall, 46 third channel, 47 third electromagnet, 48 third coil, 49 third spring, 50 third slide, 51 third slide, 52 fourth slide, 53 fourth slide, 54 fourth spring, 55 fourth coil, 56 fourth channel, 57 fourth wall.
Detailed Description
The invention is further described below with reference to the accompanying drawings.
As shown in fig. 1 to 4, the visual experimental apparatus for determining VLE provided by the present invention comprises a visual reaction kettle 26, a visual high-precision thermostatic bath 21, a sample tank 1, a vacuum pump 4, a temperature measuring system, a pressure measuring system, and a vapor-liquid phase sampling system. The wall surface 17 of the visual reaction kettle 26 is made of stainless steel, and the front and the back are made of reaction kettle high borosilicate glass windows 18 which are respectively connected with the sample tank 1 and the gas chromatograph 15 through pipelines. Visual high accuracy thermostatic bath 21, the front side adopts thermostatic bath borosilicate glass window 20, and the layering condition of reation kettle 26 in the experiment is directly observed to accessible thermostatic bath borosilicate glass window 20. The temperature measuring system and the pressure measuring system are respectively connected with the visual reaction kettle 26 and the high-precision thermostatic bath 21. The vacuum pump 4 is connected with the visual reaction kettle 26. The vapor-liquid phase sampling system comprises a first sampling small chamber 29, a second sampling small chamber 30, a first expansion chamber 14, a second expansion chamber 23 and a gas chromatograph 16.
The working principle is as follows: when performing the solubility experiment, the first sampling cell and the second sampling cell are both closed on the left and right sides. Filling the refrigerant and the lubricating oil into the reaction kettle, starting the stirring device, and recording the temperature and the pressure when the fluctuation of the temperature and the pressure is in an uncertainty range. When the refrigerant mixture balance experiment is carried out, the left side of the first sampling chamber and the left side of the second sampling chamber are opened and closed. The refrigerant mixture is filled into the reaction kettle, the stirring device is started, and when the fluctuation of the temperature and the pressure is in an uncertain range, the temperature and the pressure are recorded.
Valves are arranged between the sample tank 1 and the visualization reaction kettle 26, between the vacuum pump 4 and the pipeline, between the first sampling small chamber 29 and the second sampling small chamber 30 and the expansion chamber, and between the first expansion chamber 14 and the second expansion chamber 23 and the gas chromatograph 16.
The high-precision thermostatic bath 26 comprises a circulating pump, a heating system, a refrigerating system and a temperature control system in a control cabinet, and meets the temperature requirement.
The temperature measuring system comprises an upper computer 6, a data acquisition card 7, a first platinum resistor 19 and a second platinum resistor 25. The first platinum resistor 19 is placed in the high-precision thermostatic bath 21 and used for detecting temperature fluctuation; the second platinum resistor 25 is arranged in the visual reaction kettle 26 and used for detecting whether the reaction temperature reaches equilibrium or not.
The pressure measurement system comprises a first pressure transmitter 5 and a second pressure transmitter 10. The first pressure transmitter 5 is connected with the gas distribution pipeline and used for detecting the pressure of the pipeline; second pressure transmitter 10 is coupled to visual reactor 26 for measuring pressure data and pressure fluctuations of visual reactor 26.
The first sampling small chamber 29 and the second sampling small chamber 30 are respectively located at the top and the bottom of the visualization reaction kettle 26, and have the same structure. The first sampling small chamber 29 is bilaterally symmetrical, the first electromagnet 33 on the left side is fixed on the sliding block 37, is placed on the first sliding rail 36 and is reset by the first spring 35 in an unpowered state, the left side of the small chamber is communicated with the visual reaction kettle 26 at the moment, and the first electromagnet closes the channel 32 on the first wall surface 31 in the powered state; the second electromagnet 42 on the right is fixed to the slide 39, is placed on the second slide 38, is returned by the first spring 40 in the non-energized state, in which the right side of the small chamber is in communication with the first expansion chamber 14, and in the energized state closes the passage 43 in the second wall 44. The second sampling small chamber 30 is bilaterally symmetrical, a third electromagnet 47 on the left side is fixed on a sliding block 51, is placed on a third sliding rail 50 and is reset by a third spring 49 in an unpowered state, the left side of the small chamber is communicated with the visual reaction kettle 26 at the moment, and the third electromagnet closes a channel 46 on the third wall surface 45 in the powered state; a fourth electromagnet 56 on the right side is fixed to the slider 53, is placed on the fourth slide rail 52, is reset by a fourth spring 54 in the non-energized state, at this time, the right side of the small chamber is communicated with the second expansion chamber 23, and closes a passage 57 on a fourth wall surface 58 in the energized state;
the solubility test procedure was carried out as follows:
1) before the experiment starts, firstly, the coil 34 on the first electromagnet 33 is electrified, and the channel 32 on the first wall surface 31 is closed; energizing the coil 41 on the second electromagnet 42 to close the passage 43 on the second wall 44; energizing the coil 48 on the third electromagnet 47 to close the channel 46 on the third wall 45; the coil 55 on the fourth electromagnet 56 is energized to close the passage 57 in the fourth wall 58. And opening the vacuum pump 4, the first valve 2 and the second valve 9 to vacuumize the visual reaction kettle 26, vacuumizing the system, closing the vacuum pump 4, the first valve 2 and the second valve 9 when the pressure of the pressure transmitter is not higher than 0.1Pa, standing for 24h, and inspecting the air tightness of the visual reaction kettle 26.
Next, the volume of the visualization reactor 26 was calibrated with CO2 having a purity of 99.99%, keeping the left and right channels 32, 43 of the first sampling cell 29 and the left and right channels 46, 57 of the second sampling cell 30 closed.
2) At the beginning of the experiment, the left and right channels of the first sample cell 29 and the second sample cell 30 in the first holding step are closed. A certain mass of the lubricating oil was weighed using an analytical balance and then injected into the reaction vessel 26 through the syringe, and the total mass of the syringe at this time was weighed. The visual reaction kettle 26 is sealed with the first bolt 8 and the second bolt 12 through the flange plate 11 and is connected with a gas distribution pipeline. And opening the vacuum pump 4, the first valve 2 and the second valve 9 again to vacuumize the visual reaction kettle 26, vacuumizing the system, and closing the vacuum pump, the first valve 2 and the second valve 9 when the pressure of the pressure transmitter is not higher than 0.1 Pa. And (3) reducing the temperature of the thermostatic bath 21, opening the second valve 9 and the third valve 3, flushing refrigerant into the visual reaction kettle 26 until the second pressure transmitter 10 displays that the pressure in the visual reaction kettle 26 reaches the value required by the experiment, and closing the second valve 9 and the third valve 3. The sample tank is removed 1 and the refrigerant injection mass is weighed.
3) During the experiment, the temperature of the high-precision thermostatic bath 21 was set, and the magnetic stirring rod 28 was turned on. When the second pressure transmitter 10, the first platinum resistor 19 and the second platinum resistor 25 all tend to be stable, the numerical value changes of the first pressure transmitter, the second platinum resistor and the second platinum resistor are within the uncertainty range of pressure and temperature; and the phenomenon of layering or flocculent precipitation does not exist in the high-precision thermostatic bath 21 and the visual reaction kettle 26, and the temperature and pressure values at the moment are read.
4) The temperature of the high-precision thermostatic bath 21 is adjusted, and the next set of experiments is continued. When this set of experiments was completed, no re-injection of lubricating oil was required. And keeping the second valve 9 closed, opening the first valve 2, vacuumizing the distribution pipeline, and closing the vacuum pump 4 and the first valve 2 when the pressure of the pressure transmitter is not higher than 0.1 Pa. And reducing the temperature of the high-precision thermostatic bath 21, opening the third valve 3 and the second valve 9, distributing gas to the visual reaction kettle 26 again until the second pressure transmitter 10 displays that the pressure in the visual reaction kettle 26 reaches the value required by the experiment, and closing the second valve 9 and the third valve 3. The sample tank 1 was removed and the refrigerant injection mass was weighed. And finally, repeating the step four.
5) The solubility of the refrigerant in the lubricating oil can be calculated from the formulas (1), (2):
in the formula: m is3Is the total mass of refrigerant flushed in, veIs the molar volume of the gas phase of the refrigerant in an equilibrium state, M is the relative molecular mass of the refrigerant, Vr is the volume of the visual reaction kettle, V2Is the volume of lubricating oil dissolved, v1Is the molar volume of the refrigerant liquid phase at equilibrium, m1 is the mass of the refrigerant dissolved, and m2 is the mass of the lubricant flushed in.
The specific implementation method of the refrigerant mixture vapor-liquid phase equilibrium test is as follows:
1) before the experiment is started, the vacuum pump 4, the first valve 2 and the second valve 9 are firstly opened, the visual reaction kettle 26 is vacuumized, the vacuum pump 4, the first valve 2 and the second valve 9 are closed when the pressure 5 of the pressure transmitter is not higher than 0.1Pa, the operation is kept still for 24h, and the air tightness of the visual reaction kettle 26 is inspected.
2) When the experiment is started, the visual reaction kettle 26 is sealed with the first bolt 8 and the first bolt 8 through the flange plate 11 and is connected with the gas distribution pipeline. Keeping the first electromagnet 33 reset by the spring 35, opening the passage 32 in the first wall 31; keeping the second electromagnet 42 reset by the spring 40, opening the passage 43 in the second wall 44; keeping the third electromagnet 47 reset by the spring 49, opening the passage 46 on the third wall 45; keeping the fourth electromagnet 56 reset by the spring 54 opens the passage 57 in the fourth wall 58. Opening the vacuum pump 4, the first valve 2, the second valve 9, the third valve 3, the fourth valve 13, the fifth valve 22, the sixth valve 15 and the seventh valve 24 again to vacuumize the visual reaction kettle 26 and the whole system pipeline, closing the vacuum pump 4, the first valve 2, the second valve 9, the third valve 3, the fourth valve 13, the fifth valve 22, the sixth valve 15 and the seventh valve 24 when the pressure of the pressure transmitter 5 is not higher than 0.1Pa, electrifying a coil 48 on a third electromagnet 47, and closing a channel 46 on the third wall surface 45; the coil 55 on the fourth electromagnet 56 is energized to close the passage 57 in the fourth wall 58. And (3) reducing the temperature of the high-precision thermostatic bath 21, opening the second valve 2 and the third valve 3, flushing the mixed refrigerant into the visual reaction kettle 26 until the second pressure transmitter 10 displays that the pressure in the visual reaction kettle 26 reaches the value required by the experiment, observing that gas-liquid two phases exist in the visual reaction kettle 26 at the moment, and closing the second valve 9 and the third valve 3.
3) During the experiment, the temperature of the high-precision thermostatic bath 26 was set, and the magnetic stirring rod 28 was turned on. When the second pressure transmitter 10, the first platinum resistor 19 and the second platinum resistor 25 all tend to be stable, the numerical value changes of the first pressure transmitter, the second platinum resistor and the second platinum resistor are within the uncertainty range of pressure and temperature; and the existence of liquid phase in the reaction kettle 26 is observed through the high-precision thermostatic bath 21 and the visual reaction kettle, and the temperature and pressure values at the moment are read.
4) At this time, the coil 34 of the first electromagnet 33 is electrified to close the channel 32 on the first wall surface 31; energizing the coil 41 on the second electromagnet 42 to close the passage 43 on the second wall 44; keeping the third electromagnet 47 reset by the spring 49, opening the passage 46 on the third wall 45; keeping the fourth electromagnet 56 reset by the spring 54 opens the passage 57 in the fourth wall 58. The fourth valve 13 and the fifth valve 22 are opened to fully expand the vapor-liquid refrigerant into the first expansion chamber 14 and the second expansion chamber 23. The fourth valve 13 and the fifth valve 22 are closed, the sixth valve 15 and the seventh valve 24 are opened, and the gases in the first expansion chamber 14 and the second expansion chamber 23 are respectively introduced into the gas chromatograph 16 for component analysis.
5) And (5) adjusting the temperature of the constant temperature bath to 21, distributing gas again, and continuing the next group of experiments.
Claims (6)
1. A visual experimental device for determining VLE is characterized by comprising a visual reaction kettle, a visual high-precision thermostatic bath, a sample tank, a vacuum pump, a temperature measuring system, a pressure measuring system and a vapor-liquid phase sampling system;
the front and the back of the visual reaction kettle are respectively provided with a high borosilicate glass window and are respectively connected with the sample tank and the gas chromatograph through pipelines;
the front side of the visual high-precision thermostatic bath adopts a high borosilicate glass window, and the layering condition of the reaction kettle in the experiment is directly observed through the glass window;
the temperature measuring system and the pressure measuring system are respectively connected with the visual reaction kettle and the visual high-precision thermostatic bath, and the vacuum pump is connected with the visual reaction kettle;
the vapor-liquid phase sampling system comprises a small sampling chamber, an expansion chamber and a gas chromatograph;
when a solubility experiment is carried out, the left side and the right side of the first sampling small chamber and the second sampling small chamber are both closed, a refrigerant and lubricating oil are filled into the reaction kettle, the stirring device is started, and when the fluctuation of temperature and pressure is within an uncertainty range, the temperature and the pressure are recorded;
when carrying out refrigerant mixture balance experiment, the side switch is opened to first sampling cell and second sampling cell left side, fills the reation kettle with the refrigerant mixture in, opens agitating unit, when the fluctuation of temperature and pressure is in the uncertainty scope, records temperature, pressure.
2. The visual experimental apparatus for determining VLE of claim 1, wherein valves are installed between said sample tank and said visual reaction kettle, between said vacuum pump and said pipeline, between said sampling chamber and said expansion chamber, and between said expansion chamber and said gas chromatograph;
the control cabinet of the high-precision thermostatic bath comprises a circulating pump, a heating system, a refrigerating system and a temperature control system, and the temperature requirement is met;
the temperature measuring system comprises an upper computer, a data acquisition card, a first platinum resistor and a second platinum resistor; the first platinum resistor is arranged in the thermostatic bath and used for detecting the fluctuation of temperature; the second platinum resistor is arranged in the visual reaction kettle and used for detecting whether the reaction temperature reaches balance or not;
the pressure measuring system comprises a first pressure transmitter and a second pressure transmitter, wherein the first pressure transmitter is connected with the gas distribution pipeline and used for detecting the pressure of the pipeline; and the second pressure transmitter is connected with the visual reaction kettle and is used for measuring pressure data and pressure fluctuation of the visual reaction kettle.
3. The visual testing apparatus of claim 1, wherein the first and second sampling chambers are located at the top and bottom of the visual reaction vessel and have the same structure.
4. The visual experimental apparatus for determining VLE of claim 1, wherein said first sampling chamber is symmetric to the left and right, the first electromagnet on the left side is placed on the first slide rail and is reset by the first spring under the non-energized state, and the left side of the chamber is connected to the visual reaction vessel; the second electromagnet on the right side is arranged on the second sliding rail and is reset by the second spring in an unpowered state, and the right side of the small chamber is communicated with the expansion chamber.
5. The visual experiment apparatus solubility measurement method for determining VLE of claim 1, comprising the steps of:
1) before the experiment begins, the sampling small chamber is closed, a valve and a vacuum pump for vacuumizing are opened, the visual reaction kettle is vacuumized and pressure is maintained for 24 hours, andwith high purity CO2Calibrating the volume of the visual reaction kettle;
2) when the experiment is started, keeping the two sampling small chambers closed, injecting lubricating oil by using an injector, and sealing the visual reaction kettle; opening a valve and a vacuum pump for vacuumizing, and vacuumizing the visual reaction kettle; closing the valves, opening all the valves on the gas distribution pipeline, and filling the refrigerant;
3) in the experimental process, setting the temperature of a thermostatic bath, starting magnetic stirring, observing the balance phenomenon of the visual reaction kettle, and recording the pressure and the temperature;
4) adjusting the temperature of the constant temperature bath, and continuing the next group of experiments;
keeping the sealing of the reaction kettle, vacuumizing the pipeline again, injecting the refrigerant again, and performing solubility experiments of different components;
5) the solubility of the refrigerant in the lubricating oil can be calculated from the formulas (1), (2):
in the formula: m is3Is the total mass of refrigerant flushed in, veIs the molar volume of the refrigerant gas phase at equilibrium, M is the relative molecular mass of the refrigerant, VrIs the volume of the visual reaction kettle, V2Is the volume of lubricating oil dissolved, v1Is the molar volume of the refrigerant liquid phase in equilibrium, m1Is the mass of refrigerant dissolved, m2Is the quality of the lubricating oil that is flushed in.
6. The method of claim 1, comprising the steps of:
1) before the experiment begins, opening a left channel of a sampling small chamber, closing two right channels for sampling, opening a valve and a vacuum pump for vacuumizing, vacuumizing the visual reaction kettle and maintaining the pressure for 24 hours;
2) when the experiment is started, the left channel and the right channel of the two sampling small chambers, and a valve and a vacuum pump for vacuumizing are opened, and the visual reaction kettle and the whole system pipeline are vacuumized; closing the valve and the two right channels for sampling, opening the gas distribution valve, and filling the system with mixed refrigerant;
3) in the experimental process, setting the temperature of a thermostatic bath, opening a magnetic stirring rod, observing the balance phenomenon of the visual reaction kettle, and recording the pressure and the temperature;
4) at the moment, the left channels of the two sampling small chambers are closed, the right channels and the valves are opened, so that the refrigerant is fully expanded in the expansion chamber, and then the refrigerant is introduced into a gas chromatograph for analysis;
5) and adjusting the temperature of the constant temperature bath, distributing gas again, and continuing the next group of experiments.
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