CN114279890A - System and method for measuring volume of liquid under high pressure - Google Patents
System and method for measuring volume of liquid under high pressure Download PDFInfo
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- CN114279890A CN114279890A CN202111604467.3A CN202111604467A CN114279890A CN 114279890 A CN114279890 A CN 114279890A CN 202111604467 A CN202111604467 A CN 202111604467A CN 114279890 A CN114279890 A CN 114279890A
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- 239000007788 liquid Substances 0.000 title claims abstract description 77
- 238000000034 method Methods 0.000 title claims abstract description 31
- 239000007789 gas Substances 0.000 claims abstract description 58
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 41
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000007787 solid Substances 0.000 claims abstract description 25
- 239000011324 bead Substances 0.000 claims abstract description 23
- 238000005259 measurement Methods 0.000 claims abstract description 18
- 238000002474 experimental method Methods 0.000 claims abstract description 17
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 16
- 238000010521 absorption reaction Methods 0.000 claims abstract description 16
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 16
- 239000010959 steel Substances 0.000 claims abstract description 16
- 239000007791 liquid phase Substances 0.000 claims description 14
- 230000002745 absorbent Effects 0.000 claims description 13
- 239000002250 absorbent Substances 0.000 claims description 13
- 238000011049 filling Methods 0.000 claims description 8
- 239000002608 ionic liquid Substances 0.000 claims description 7
- 238000012544 monitoring process Methods 0.000 claims description 7
- 229920006395 saturated elastomer Polymers 0.000 claims description 5
- 238000007789 sealing Methods 0.000 claims description 5
- 230000003068 static effect Effects 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 3
- 238000005273 aeration Methods 0.000 claims description 2
- 238000000691 measurement method Methods 0.000 abstract description 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- 229910002092 carbon dioxide Inorganic materials 0.000 description 4
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 3
- IQQRAVYLUAZUGX-UHFFFAOYSA-N 1-butyl-3-methylimidazolium Chemical compound CCCCN1C=C[N+](C)=C1 IQQRAVYLUAZUGX-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000007664 blowing Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011067 equilibration Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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Abstract
The application discloses a system and a method for measuring liquid volume under high pressure. The measuring system comprises a plurality of valves, a buffer tank, a balance kettle, a constant temperature water bath, a thermocouple, a pressure sensor, a computer, a vacuum pump, an absorption bottle, a nitrogen steel bottle and a measured gas steel bottle. The measurement method of the present invention is realized by the measurement device system. And (3) performing measurement experiments through solid beads with known volumes, and regressing secondary regression equations of the volume, the pressure of the buffer tank, the pressure and the temperature of the balance kettle before inflation and the pressure of the balance kettle after inflation. By adopting the quadratic regression method, the volume of the liquid when the gas is dissolved in the liquid under high pressure to reach balance is calculated according to the pressure of the buffer tank, the pressure of the balance kettle before and after inflation and the temperature of the experiment. The method is simple and easy to operate, cannot be influenced by the characteristics of dark and viscous liquid and the like, and has a good application prospect.
Description
Technical Field
The invention relates to the technical field of liquid volume measurement, in particular to a system and a method for measuring the volume of liquid under high pressure when gas is dissolved in the liquid under high pressure to reach balance.
Technical Field
The solubility of gas in liquid is the basic data of gas absorption, purification and separation, and is an important basis for industrial design. For the gas dissolving process adopting physical absorption, the higher the pressure is, the more favorable the gas is dissolved in liquid, for example, the low-temperature methanol method is used for removing carbon dioxide and hydrogen sulfide in the synthesis gas, the pressure range is 2MPa-10MPa, the higher the pressure is, the carbon dioxide and hydrogen sulfide are favorably dissolved and absorbed in methanol, the purification quality of the synthesis gas is improved, and the dosage of an absorbent is reduced.
The gas solubility is usually measured by a gas-liquid equilibrium kettle, and the gas-phase space volume in the equilibrium kettle is obtained by calculating the volume of liquid in the equilibrium kettle, so that the solubility of the gas in the liquid is calculated. The size of the liquid volume in the equilibrium vessel is therefore critical to calculating the gas solubility. After the gas is dissolved in the liquid under high pressure, the volume of the liquid changes, and particularly when the pressure is higher than 0.3MPa, the liquid volume for absorbing the gas is greatly different from the volume of the pure liquid, so that the liquid volume after absorbing the gas in the equilibrium kettle cannot be replaced by the pure liquid volume which is measured in advance.
There are two methods for measuring the volume of liquid in a balance kettle under high pressure. One is to open two ends of the side surface of the balance kettle, install a sapphire window with scales, and measure the liquid volume in the balance kettle by observing the scale value of the liquid level on the window. The other is that the balance kettle is internally provided with an upper buoy, and the buoy is positioned on the liquid level of the liquid. When the liquid volume changes, the scale of the buoy changes, and the liquid volume in the equilibrium kettle is determined. The disadvantage of the first method is that the liquid is dark or sticky, and it is easy to coat the window scale, making the reading difficult and potentially causing large errors in the measurement. The second method has the defect that a sealing device is needed between the buoy and the kettle cover of the balance kettle, and the sealing device not only ensures that the buoy freely moves up and down, but also ensures that the air tightness is good, thereby putting high requirements on equipment manufacture. In addition, the conventional equilibrium tank using a float is large in volume, and therefore requires a large volume of liquid. The measurement of the solubility of valuable liquids results in high costs.
In view of the above problems, we propose a new system and method for determining the volume of liquid under high pressure.
Disclosure of Invention
The invention aims to provide a system and a method for measuring the volume of liquid under high pressure, which solve the problems that the reading is difficult, the air tightness and the result accuracy cannot be simultaneously considered and the like caused by the deep and viscous color of the liquid in the existing liquid volume measurement technology.
In order to achieve the above object, in one embodiment of the present invention, a system for measuring a volume of a liquid under high pressure is provided, which is characterized by comprising a first valve, a second valve, a third valve, a fourth valve, a fifth valve, a sixth valve, a buffer tank, a balance kettle, a first constant temperature water bath, a second constant temperature water bath, a first thermocouple, a second thermocouple, a first pressure sensor, a second pressure sensor, a computer, a vacuum pump, an absorption bottle, a nitrogen steel bottle, and a steel bottle for a gas to be measured; the nitrogen steel cylinder and the measured gas steel cylinder are respectively connected with the first valve and the second valve, and the first valve and the second valve are both connected to a third valve and the on-off of the gas is controlled by the third valve; the third valve is connected with the fourth valve; one end of the buffer tank is connected with the fourth valve, the other end of the buffer tank is connected with the fifth valve, and the buffer tank is used for storing gas; the buffer tank is connected with the balance kettle, the buffer tank and the balance kettle are respectively arranged in the first constant temperature water bath and the second constant temperature water bath, the temperature of the buffer tank is controlled through the first constant temperature water bath, and the temperature of the balance kettle is controlled through the second constant temperature water bath; the first thermocouple and the second thermocouple are respectively communicated to the buffer tank and the balance kettle; the first thermocouple and the second thermocouple are respectively used for measuring the temperature in the buffer tank and the temperature in the balance kettle; the first pressure sensor and the second pressure sensor are respectively communicated to the buffer tank and the balance kettle, and are electrically connected with the computer; the first pressure sensor and the second pressure sensor are respectively used for measuring the gas pressure in the buffer tank and the balance kettle, and are connected with the computer for monitoring the pressure change on line; one end of the balance kettle is connected with the buffer tank through the fifth valve, the other end of the balance kettle is connected with the absorption bottle through the sixth valve, the balance kettle is used for measuring gas-liquid phase balance, and the absorption bottle is used for absorbing tail gas; the vacuum pump is connected with the sixth valve and used for vacuumizing the system.
Further, the lower end of the inside of the balance kettle is provided with a stirrer, the stirrer is in a static state when the balance kettle is inflated, and the stable pressure of the system is the pressure of the stirrer in the balance kettle when the stirrer is static.
Furthermore, the first thermocouple and the second thermocouple are also electrically connected with the computer and used for monitoring the change of the temperature on line.
The invention also provides a method for measuring the volume of liquid under high pressure, which adopts the system for measuring the volume of liquid under high pressure to measure the volume of liquid under high pressure, and comprises the following steps: step 1) setting the required temperature in both the first constant temperature water bath and the second constant temperature water bathDegree; step 2) pouring solid round beads with the volume of V into the balance kettle; step 3) sealing the balance kettle, and putting the balance kettle into the second constant-temperature water bath; step 4) after the temperature of the system is stabilized to be T, opening the first valve, the second valve, the third valve, the fourth valve and the fifth valve, closing the sixth valve, filling a certain amount of nitrogen, and checking the air tightness of the system; step 5) opening a sixth valve when the air tightness of the system is good, and starting a vacuum pump to vacuumize the system; closing the sixth valve, and recording the pressure in the balance kettle at the moment as P0(ii) a Step 6) closing a fifth valve between the buffer tank and the balance kettle; step 7) opening a second valve to fill the detected gas into the buffer tank, and closing the second valve and a fourth valve; keeping the temperature for a period of time after the buffer tank is inflated, and recording the pressure in the buffer tank as P1The pressure in the balance kettle is P2(ii) a Step 8) opening a fifth valve, filling the tested gas into the balance kettle, closing the fifth valve, and recording the stable pressure P in the balance kettles(ii) a Step 9) repeating step 7) and step 8); step 10) changing the volume value V of the solid beads, and repeating the steps 1) to 9); step 11) determining a regression equation by the least square method through the above operations
Parameter a in i + j + k + l ≤ 2ijkl(ii) a Wherein i, j, k, l have a value of 0, 1 or 2; and 12) replacing the solid round beads with liquid, repeating the steps 1) to 9), and calculating to obtain the volume of the liquid phase in the equilibrium kettle by measuring the temperature in the experimental process, the pressure in the buffer tank before inflation and the pressure in the equilibrium kettle before and after inflation, so as to obtain the actual volume of the liquid when the gas is dissolved in the liquid under high pressure to reach equilibrium.
Further, in steps 1) to 11), a parameter a in the regression equation is obtained by using a solid bead with a known volume to replace liquid for measurement experimentijkl。
Furthermore, the solid ball is made of a material which does not generate adsorption with the gas to be detected.
Further, when the system is vacuumized, the pressure value in the system is pumped to be larger than the saturated vapor pressure value of the absorbent used at the current temperature.
Further, if the ionic liquid is used as the absorbent, the pressure in the system should be pumped to be within 1 kPa.
Further, after the buffer tank is inflated, the buffer tank is required to be kept warm for 30-90min, and then the pressure P in the buffer tank is recorded1And the pressure P in the equilibrium vessel2。
Further, in step 11), the pressure P in the buffer tank before inflation is determined by the volume value V, the temperature T and the pressure P in the buffer tank before inflation of at least 15 different groups of solid beads1And the pressure P in the equilibrium reactor before and after inflation2And PsParameter a in the regression equationijkl。
The measuring system comprises a valve, a buffer tank, a balance kettle, a constant temperature water bath, a thermocouple, a pressure sensor, a computer, a vacuum pump, an absorption bottle, a nitrogen steel bottle and a measured gas steel bottle, wherein the buffer tank and the balance kettle are respectively arranged in the constant temperature water bath, and the pressure sensor is respectively connected with the buffer tank and the balance kettle and used for monitoring real-time pressure change in the buffer tank and the balance kettle; and the thermocouples are respectively connected with the buffer tank and the balance kettle and are used for measuring the temperature in the buffer tank and the balance kettle. The measurement method of the present invention is realized by the measurement device system. And (3) performing measurement experiments through solid beads with known volumes, and regressing secondary regression equations of the volume, the pressure of the buffer tank, the pressure and the temperature of the balance kettle before inflation and the pressure of the balance kettle after inflation. By adopting the equation, the volume of the liquid when the gas is dissolved in the liquid under high pressure to reach balance is calculated according to the pressure of the buffer tank, the pressure of the balance kettle before and after inflation and the temperature of the experiment. The method is simple and easy to operate, cannot be influenced by the characteristics of dark and viscous liquid and the like, and has a good application prospect.
Compared with the prior art, the invention has the following advantages:
(1) the problem of difficult reading due to the characteristic that the absorbent is dark in color and viscous is solved, so that the measured solubility result is more accurate;
(2) the problem that the good degree of the air tightness of the measuring device and the accuracy degree of a measuring result cannot be simultaneously considered is solved, and the organic combination of the device and the measurement is realized;
(3) the device principle is easy to understand, the operability is strong, the absorbent consumption is low, and the market prospect is good.
Drawings
The technical solution and other advantages of the present application will be presented in the following detailed description of specific embodiments of the present application with reference to the accompanying drawings.
Fig. 1 is a schematic structural diagram of a system for determining a liquid volume under high pressure according to an embodiment of the present disclosure.
The components in the figure are identified as follows:
the device comprises a first valve 1, a second valve 2, a third valve 3, a fourth valve 4, a fifth valve 5, a sixth valve 6, a buffer tank 7, a balance kettle 8, a first constant temperature water bath 9, a second constant temperature water bath 10, a first thermocouple 11, a second thermocouple 12, a first pressure sensor 13, a second pressure sensor 14, a computer 15, a vacuum pump 16, an absorption bottle 17, a nitrogen steel bottle 18 and a measured gas steel bottle 19.
Detailed Description
The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application. It is to be understood that the embodiments described are only a few embodiments of the present application and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
The present invention is directed to a system and method for determining the volume of a liquid under high pressure, which solves the above-mentioned problems and disadvantages.
In order to achieve the purpose, the invention provides the following technical scheme:
the invention provides a system for measuring the volume of liquid under high pressure, which is characterized by comprising a first valve 1, a second valve 2, a third valve 3, a fourth valve 4, a fifth valve 5, a sixth valve 6, a buffer tank 7, a balance kettle 8, a first constant temperature water bath 9, a second constant temperature water bath 10, a first thermocouple 11, a second thermocouple 12, a first pressure sensor 13, a second pressure sensor 14, a computer 15, a vacuum pump 16, an absorption bottle 17, a nitrogen steel bottle 18 and a measured gas steel bottle 19; the nitrogen cylinder 18 and the measured gas cylinder 19 are respectively connected with the first valve 1 and the second valve 2, and the first valve 1 and the second valve 2 are both connected to a third valve 3 and the third valve 3 controls the on-off of gas; the third valve 3 is connected with the fourth valve 4; one end of the buffer tank 7 is connected with the fourth valve 4, the other end of the buffer tank 7 is connected with the fifth valve 5, and the buffer tank 7 is used for storing gas; the buffer tank 7 is connected with the balance kettle 8, the buffer tank 7 and the balance kettle 8 are respectively arranged in the first constant temperature water bath 9 and the second constant temperature water bath 10, the temperature of the buffer tank 7 is controlled through the first constant temperature water bath 9, and the temperature of the balance kettle 8 is controlled through the second constant temperature water bath 10; the first thermocouple 11 and the second thermocouple 12 are respectively communicated to the buffer tank 7 and the balance kettle 8; the first thermocouple 11 and the second thermocouple 12 are respectively used for measuring the temperature in the buffer tank 7 and the balance kettle 8, and the first thermocouple 11 and the second thermocouple 12 can also be connected with the computer 15 for monitoring the change of the temperature on line; the first pressure sensor 13 and the second pressure sensor 14 are respectively communicated to the buffer tank 7 and the balance kettle 8, and the first pressure sensor 13 and the second pressure sensor 14 are both electrically connected with the computer 15; the first pressure sensor 13 and the second pressure sensor 14 are respectively used for measuring the gas pressure in the buffer tank 7 and the equilibrium kettle 8, and are connected with the computer 15 for monitoring the pressure change on line; one end of the balance kettle 8 is connected with the buffer tank 7 through the fifth valve 5, the other end of the balance kettle 8 is connected with the absorption bottle 17 through the sixth valve 6, the balance kettle 8 is used for measuring gas-liquid phase balance, and the absorption bottle 17 is used for absorbing tail gas; the vacuum pump 16 is connected with the sixth valve 6, and the vacuum pump 16 is used for vacuumizing the system.
The inside lower extreme of reation kettle 8 is equipped with the agitator that is used for stirring the inner chamber of reation kettle 8, and the agitator is in quiescent condition when reation kettle 8 aerifys, and the steady pressure of system is the pressure when the agitator is static in the reation kettle.
Before the device is used for measuring the volume of liquid under high pressure, a second-order polynomial of the pressure of a ball regression buffer tank with a known volume, the pressure and the temperature of a balance kettle before and after inflation is used for obtaining the parameters of the equation (1).
Wherein i, j, k, l have a value of 0, 1 or 2; by expanding equation (1), the expansion can be obtained:
the specific operation steps are as follows:
step 1) setting the two water baths to be required temperatures in advance and enabling the two water baths to be equal; setting the temperature in both the first and second constant- temperature water baths 9 and 10 to a desired temperature;
step 2), cleaning and wiping the balance kettle, and pouring the solid round beads with the volume of V into the balance kettle 8;
step 3), closing a cover of the balance kettle, screwing a bolt, sealing the balance kettle 8, and putting the balance kettle 8 into the second constant-temperature water bath 10;
step 4) after the temperature of the system is stabilized to be T, opening the first valve 1, the second valve 2, the third valve 3, the fourth valve 4 and the fifth valve 5, closing the sixth valve 6, filling a certain amount of nitrogen, checking the air tightness of the system, and keeping the pressure unchanged within 30min to indicate that the air tightness of the device is good;
step 5) opening a sixth valve 6 when the air tightness of the system is good, and starting a vacuum pump 16 to vacuumize the system; the sixth valve 6 is closed, and the pressure in the equilibrium reactor 8 at this time is recorded as P0；
Step 6) closing a fifth valve 5 between the buffer tank 7 and the balance kettle 8;
step 7) opening the second valve 2 to charge the gas to be detected into the buffer tank 7, and closing the second valve 2 and the fourth valve 4; keeping the temperature of the buffer tank 7 for a period of time after the buffer tank is inflated, keeping the temperature for 30-90min, and then recording the pressure in the buffer tank 7 as P1The pressure in the balance kettle 8 is P2；
Step 8) opening a fifth valve 5, filling the tested gas into the balance kettle 8, closing the fifth valve 5, and recording the stable pressure P in the balance kettle 8s；
Step 9) repeating step 7) and step 8);
step 10) changing the volume value V of the solid ball, and repeating the steps 1) to 9) until all volume values are finished;
step 11) determining a regression equation by the least square method through the above operations
Parameter a in i + j + k + l ≤ 2ijkl(ii) a Wherein i, j, k, l have a value of 0, 1 or 2;
and 12) replacing the solid round beads with liquid, repeating the steps 1) to 9), and calculating to obtain the volume of the liquid phase in the equilibrium kettle by measuring the temperature in the experimental process, the pressure in the buffer tank before inflation and the pressure in the equilibrium kettle before and after inflation, so as to obtain the actual volume of the liquid when the gas is dissolved in the liquid under high pressure to reach equilibrium.
In this embodiment, a measurement experiment is performed by using a solid bead with a known volume, and a quadratic regression equation of the volume, the pressure of the buffer tank, the pressure and the temperature of the equilibrium kettle before inflation and the pressure of the equilibrium kettle after inflation is regressed. And calculating the actual volume of the liquid when the gas is dissolved in the liquid under high pressure to reach balance according to the initial pressure of the buffer tank, the pressure of the balance kettle before and after inflation and the temperature of the experiment by adopting the regression equation.
Preferably, the deionized water in the water bath is replaced frequently to prevent corrosion, taking care of the cleaning of the apparatus.
Preferably, the device is placed in a water bath when the air tightness of the device is checked, so that the influence of fluctuation of the ambient temperature is avoided; the water bath is covered and insulated, and the temperature fluctuation of the system is reduced.
Preferably, the solid beads are made of a material that does not adsorb the gas to be measured. If the solid beads adsorb the gas to be detected, the pressure of the equilibrium kettle is difficult to stabilize.
Preferably, when the system is evacuated, the pressure in the system is drawn to a value greater than the saturated vapor pressure of the absorbent used at the current temperature. When the ionic liquid is used as the absorbent, the pressure in the system is pumped to within 1kPa (absolute pressure), preferably 0 to 0.5kPa, to minimize the nitrogen content in the system. When another liquid is used as the absorbent, it is necessary to adjust the pressure in consideration of the saturated vapor pressure of the absorbent at the current temperature in combination with the saturated vapor pressure of the absorbent at the current temperature.
Preferably, the agitator is at rest when the balance tank is aerated and the steady pressure is the pressure at which the balance tank agitator is at rest.
Preferably, after the experiment is finished, the gas is discharged into the absorption bottle to prevent the environment from being polluted. Blowing with nitrogen for 20 min and opening the balance kettle; and cleaning the balance kettle to prevent corrosion.
Preferably, the volume value V, the temperature T, the pressure P in the buffer tank before aeration are determined by at least 15, preferably more than 20, different solid beads1And the pressure P in the equilibrium reactor before and after inflation2And PsParameter a in regression equation (1)ijklTo improve accuracy.
Compared with the prior art, the invention has the following advantages:
(1) the problem of difficult reading caused by the characteristic that the absorbed liquid is dark in color and viscous is solved, so that the measured solubility result is more accurate;
(2) the problem that the good degree of the air tightness of the measuring device and the accuracy degree of a measuring result cannot be simultaneously considered is solved, and the organic combination of the device and the measurement is realized;
(3) the device principle is easy to understand, the operability is strong, the absorbent consumption is low, and the market prospect is good.
The method for measuring the volume of liquid under high pressure provided by the invention adopts the system for measuring the volume of liquid under high pressure to measure the volume of liquid under high pressure, and the specific embodiment of the method for measuring the volume of liquid under high pressure is as follows.
Example 1: introducing CO2Equation fitting of gases
Adding solid beads with the volume of 30mL into the balance kettle, adjusting the system to 303.15K through a constant-temperature water bath, filling a certain amount of nitrogen into the system, and checking the airtightness of the device. After confirming that the device was well air-tight, the system was evacuated to 0.3kPa (abs.). Charging part of CO into the system2Gas, after the fifth valve 5 is closed, CO with certain pressure is filled into the buffer tank2. After 70min, the pressure in the buffer tank at this time was recorded as 212.78kPa, the pressure in the equilibrium kettle was recorded as 129.67kPa, the fifth valve 5 was rapidly opened and then closed, and the steady pressure in the equilibrium kettle was recorded as 200.24 kPa.
According to the above experimental procedures, a series of experimental data were obtained by changing the volume of the solid beads, the system temperature, the initial pressure of the buffer tank and the equilibrium tank, and the results are shown in table 1.
TABLE 1 measurement results of the respective experiments
Fitting the experimental results into equation (1) to obtain a fitting parameter a1～a15. The mean relative deviation of the equation fit was 0.15% and the maximum relative deviation was 0.30%.
TABLE 2 values of fitting parameters
Example 2: introducing CO2Liquid phase volume solution after gas
The temperature of the system is adjusted to 303.15K through a thermostatic water bath, and 52.65g of 1-butyl-3-methylimidazolium-based ionic liquid is added into the balance kettle. And (3) filling a certain amount of nitrogen into the system to check the air tightness of the device, wherein the pressure in the system does not change when exceeding 30min, which indicates that the air tightness of the device is good. The system was evacuated to 0.5kPa (abs.) and subjected to solubility determination experiments. When the gas-liquid phase balance in the balance kettle is achieved, CO with certain pressure is filled into the buffer tank2After 60min, the pressure in the buffer tank was recorded at 319.37kPa, the pressure in the autoclave was recorded at 117.26kPa, the fifth valve 5 was opened and then rapidly closed, and the steady pressure in the autoclave was recorded at 295.27 kPa. Substituting the above result into equation (1), and calculating to obtain that the volume of the liquid phase in the equilibrium kettle is 39.32mL when the gas-liquid phase equilibrium is reached.
According to the steps, the ionic liquid can absorb CO under different equilibrium pressures through the system temperature, the initial pressure of the buffer tank and the equilibrium kettle before inflation and the stable pressure of the equilibrium kettle after inflation2The latter volume. The results are shown in Table 3.
TABLE 3 measurement results and calculated liquid volume values of the respective experiments
| T/K | P1/kPa | P2/kPa | Ps/kPa | V/mL |
| 303.15 | 319.37 | 117.26 | 295.27 | 39.32 |
| 303.15 | 467.52 | 269.71 | 443.03 | 40.16 |
| 303.15 | 579.02 | 382.76 | 554.53 | 40.78 |
| 303.15 | 743.08 | 546.59 | 718.96 | 41.68 |
| 303.15 | 884.35 | 685.37 | 860.83 | 42.43 |
| 303.15 | 1025.65 | 822.16 | 1002.97 | 43.18 |
| 303.15 | 1145.95 | 937.08 | 1124.13 | 43.80 |
| 303.15 | 1305.51 | 1087.43 | 1285.04 | 44.61 |
Example 3: introduction of H2Equation fitting of S gas
A30 mL volume of solid beads was added to the equilibration tank and the system was adjusted to 303.15K by a constant temperature water bath. The system was charged with a certain amount of nitrogen gas to check the airtightness of the apparatus. After confirming that the device was well air-tight, the system was evacuated to 0.4kPa (abs.). Charging the system with fraction H2S gas, after the fifth valve 5 is closed, H with certain pressure is filled into the buffer tank2And (4) keeping the temperature of the S gas for 65min, recording the pressure in the buffer tank to be 251.63kPa, recording the pressure in the equilibrium kettle to be 142.09kPa, quickly opening the fifth valve 5, then closing the fifth valve, and recording the stable pressure in the equilibrium kettle to be 234.38 kPa.
According to the above experimental procedures, a series of experimental data was obtained by changing the volume of the solid beads, the system temperature, the initial pressure of the buffer tank and the equilibrium tank, and the results are shown in table 4.
TABLE 4 measurement results of the respective experiments
Fitting the experimental results into equation (1) to obtain a fitting parameter a1～a15. The mean relative deviation of the equation fit was 0.15% and the maximum relative deviation was 0.25%.
TABLE 5 values of fitting parameters
Example 4: introduction of H2Liquid phase volume solution after S gas
44.69g of 1-butyl-3-methylimidazolium-based ionic liquid is added into the balance kettle and is adjusted to 323.15K through a constant-temperature water bath adjusting system. A predetermined amount of nitrogen gas was charged into the system to conduct the airtightness test of the apparatus. After confirming that the airtightness of the apparatus was good, the system was evacuated to 0.3kPa (absolute pressure) to conduct a solubility measurement experiment. When the gas-liquid phase balance in the balance kettle is achieved, H with certain pressure is filled into the buffer tank2And (5) after 60min, recording the pressure in the buffer tank at the moment to be 448.22kPa, the pressure in the balance kettle to be 102.83kPa, opening the fifth valve 5, then rapidly closing, and recording the stable pressure in the balance kettle to be 419.03 kPa. Substituting the above result into equation (1), and calculating to obtain that the volume of the liquid phase in the equilibrium kettle is 33.76mL when the gas-liquid phase equilibrium is reached.
According to the steps, the absorption H of the ionic liquid under different equilibrium pressures can be calculated through the system temperature, the initial pressure of the buffer tank and the equilibrium kettle before inflation and the stable pressure of the equilibrium kettle after inflation2Volume after S. The results are shown in Table 6.
TABLE 6 measurement results and calculated liquid volume values of the respective experiments
| T/K | P1/kPa | P2/kPa | Ps/kPa | V/mL |
| 323.15 | 448.22 | 102.83 | 419.03 | 33.76 |
| 323.15 | 554.21 | 204.22 | 523.01 | 34.28 |
| 323.15 | 666.37 | 312.58 | 633.08 | 34.83 |
| 323.15 | 776.59 | 420.17 | 741.29 | 35.37 |
| 323.15 | 878.20 | 520.36 | 841.11 | 35.87 |
| 323.15 | 980.02 | 621.75 | 941.21 | 36.36 |
| 323.15 | 1081.57 | 723.89 | 1041.16 | 36.86 |
| 323.15 | 1189.17 | 833.26 | 1147.19 | 37.39 |
In the foregoing embodiments, the descriptions of the respective embodiments have respective emphasis, and for parts that are not described in detail in a certain embodiment, reference may be made to related descriptions of other embodiments.
The above embodiments of the present application are described in detail, and specific examples are applied in the present application to explain the principles and implementations of the present application, and the description of the above embodiments is only used to help understand the technical solutions and core ideas of the present application; those of ordinary skill in the art will understand that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; such modifications or substitutions do not depart from the spirit and scope of the present disclosure as defined by the appended claims.
Claims (10)
1. A system for measuring the volume of liquid under high pressure is characterized by comprising a first valve, a second valve, a third valve, a fourth valve, a fifth valve, a sixth valve, a buffer tank, a balance kettle, a first constant-temperature water bath, a second constant-temperature water bath, a first thermocouple, a second thermocouple, a first pressure sensor, a second pressure sensor, a computer, a vacuum pump, an absorption bottle, a nitrogen steel bottle and a measured gas steel bottle;
the nitrogen steel cylinder and the measured gas steel cylinder are respectively connected with the first valve and the second valve, and the first valve and the second valve are both connected to a third valve and the on-off of the gas is controlled by the third valve; the third valve is connected with the fourth valve; one end of the buffer tank is connected with the fourth valve, the other end of the buffer tank is connected with the fifth valve, and the buffer tank is used for storing gas; the buffer tank is connected with the balance kettle, the buffer tank and the balance kettle are respectively arranged in the first constant temperature water bath and the second constant temperature water bath, the temperature of the buffer tank is controlled through the first constant temperature water bath, and the temperature of the balance kettle is controlled through the second constant temperature water bath; the first thermocouple and the second thermocouple are respectively communicated to the buffer tank and the balance kettle; the first thermocouple and the second thermocouple are respectively used for measuring the temperature in the buffer tank and the temperature in the balance kettle; the first pressure sensor and the second pressure sensor are respectively communicated to the buffer tank and the balance kettle, and are electrically connected with the computer; the first pressure sensor and the second pressure sensor are respectively used for measuring the gas pressure in the buffer tank and the balance kettle, and are connected with the computer for monitoring the pressure change on line; one end of the balance kettle is connected with the buffer tank through the fifth valve, the other end of the balance kettle is connected with the absorption bottle through the sixth valve, the balance kettle is used for measuring gas-liquid phase balance, and the absorption bottle is used for absorbing tail gas; the vacuum pump is connected with the sixth valve and used for vacuumizing the system.
2. The system for determining the volume of liquid under high pressure according to claim 1, wherein the lower end of the inside of the equilibrium still is provided with a stirrer, the stirrer is in a static state when the equilibrium still is inflated, and the stable pressure of the system is the pressure of the stirrer in the equilibrium still when the stirrer is in a static state.
3. A system for determining the volume of liquid under high pressure as in claim 1, wherein the first thermocouple and the second thermocouple are further electrically connected to the computer for on-line monitoring of temperature changes.
4. A method for determining the volume of a liquid under high pressure, using a system for determining the volume of a liquid under high pressure according to any one of claims 1 to 3, comprising the steps of:
step 1) setting the temperature in the first constant-temperature water bath and the second constant-temperature water bath to be required;
step 2) pouring solid round beads with the volume of V into the balance kettle;
step 3) sealing the balance kettle, and putting the balance kettle into the second constant-temperature water bath;
step 4) after the temperature of the system is stabilized to be T, opening the first valve, the second valve, the third valve, the fourth valve and the fifth valve, closing the sixth valve, filling a certain amount of nitrogen, and checking the air tightness of the system;
step 5) opening a sixth valve when the air tightness of the system is good, and starting a vacuum pump to vacuumize the system; closing the sixth valve, and recording the pressure in the balance kettle at the moment as P0；
Step 6) closing a fifth valve between the buffer tank and the balance kettle;
step 7) opening a second valve to fill the gas to be detected into the buffer tank, closing the second valve anda fourth valve; keeping the temperature for a period of time after the buffer tank is inflated, and recording the pressure in the buffer tank as P1The pressure in the balance kettle is P2；
Step 8) opening a fifth valve, filling the tested gas into the balance kettle, closing the fifth valve, and recording the stable pressure Ps in the balance kettle;
step 9) repeating step 7) and step 8);
step 10) changing the volume value V of the solid beads, and repeating the steps 1) to 9);
step 11) determining a regression equation by the least square method through the above operations
Parameter a inijkl(ii) a Wherein i, j, k, l have a value of 0, 1 or 2;
and 12) replacing the solid round beads with liquid, repeating the steps 1) to 9), and calculating to obtain the volume of the liquid phase in the equilibrium kettle by measuring the temperature in the experimental process, the pressure in the buffer tank before inflation and the pressure in the equilibrium kettle before and after inflation, so as to obtain the actual volume of the liquid when the gas is dissolved in the liquid under high pressure to reach equilibrium.
5. A method for determining the volume of a liquid under high pressure according to claim 4, wherein the parameters a in the regression equation are obtained from the measurement experiments using solid beads of known volume instead of liquid in steps 1) to 11)ijkl。
6. The method of claim 4, wherein the solid beads are of a material that does not adsorb to the gas being measured.
7. A method of determining the volume of liquid under high pressure according to claim 4, wherein the system is evacuated to a pressure greater than the saturated vapor pressure of the absorbent used at the current temperature.
8. A method for determining the volume of liquid at elevated pressure according to claim 7, wherein the pressure in the system is pumped to within 1kPa if the ionic liquid is used as the absorbent.
9. A method for determining the volume of a liquid under high pressure as claimed in claim 4, wherein the buffer tank is inflated, kept at a temperature for 30-90min and then the pressure P in the buffer tank is recorded1And the pressure P in the equilibrium vessel2。
10. A method for determining the volume of a liquid under high pressure according to claim 4, characterized in that in step 11) the pressure P in the buffer tank before aeration is determined by the volume value V, the temperature T, of at least 15 different groups of solid beads1And the pressure P in the equilibrium reactor before and after inflation2And PsParameter a in the regression equationijkl。
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