CN114279890B - System and method for measuring liquid volume under high pressure - Google Patents
System and method for measuring liquid volume under high pressure Download PDFInfo
- Publication number
- CN114279890B CN114279890B CN202111604467.3A CN202111604467A CN114279890B CN 114279890 B CN114279890 B CN 114279890B CN 202111604467 A CN202111604467 A CN 202111604467A CN 114279890 B CN114279890 B CN 114279890B
- Authority
- CN
- China
- Prior art keywords
- valve
- pressure
- buffer tank
- balance
- balance kettle
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000007788 liquid Substances 0.000 title claims abstract description 71
- 238000000034 method Methods 0.000 title claims abstract description 31
- 239000007789 gas Substances 0.000 claims abstract description 59
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 39
- 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 21
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 18
- 239000010959 steel Substances 0.000 claims abstract description 18
- 238000010521 absorption reaction Methods 0.000 claims abstract description 17
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 16
- 238000005273 aeration Methods 0.000 claims abstract 3
- 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
- 230000003068 static effect Effects 0.000 claims description 8
- 239000002608 ionic liquid Substances 0.000 claims description 7
- 238000012544 monitoring process Methods 0.000 claims description 6
- 238000011049 filling Methods 0.000 claims description 5
- 229920006395 saturated elastomer Polymers 0.000 claims description 5
- 238000007789 sealing Methods 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 3
- 238000005259 measurement Methods 0.000 abstract description 14
- 238000002474 experimental method Methods 0.000 abstract description 13
- 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
- 238000004090 dissolution Methods 0.000 description 3
- -1 1-butyl-3-methylimidazole iron Chemical compound 0.000 description 2
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 238000004140 cleaning Methods 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
- 230000002349 favourable effect Effects 0.000 description 2
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 230000009286 beneficial effect Effects 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
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000011067 equilibration Methods 0.000 description 1
- 238000007689 inspection Methods 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
- 238000010926 purge Methods 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
Landscapes
- Measuring Fluid Pressure (AREA)
Abstract
The application discloses a system and a method for measuring the volume of liquid 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 measuring method of the present application is realized by the measuring device system. And (3) carrying out measurement experiments through solid beads with known volumes, and returning to a quadratic regression equation of the volumes, the buffer tank pressure, the pressure before the balance tank is inflated, the temperature and the pressure after the balance tank is inflated. By adopting the secondary 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 the aeration and the temperature of the buffer tank. The application has simple and easy operation, is not affected by the characteristics of deep and viscous liquid color and the like, and has 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 under high pressure is dissolved in the liquid 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 dissolution process adopting physical absorption, the higher the pressure is, the more favorable the dissolution of the gas in the liquid, for example, the carbon dioxide and hydrogen sulfide in the synthesis gas are removed by a low-temperature methanol method, the pressure range is 2MPa-10MPa, the higher the pressure is, the dissolution and absorption of the carbon dioxide and the hydrogen sulfide in the methanol are favorable, the purification quality of the synthesis gas is improved, and the consumption of an absorbent is reduced.
The gas solubility is measured by a gas-liquid balance kettle, and the volume of a gas phase space in the balance kettle is obtained by calculating the volume of liquid in the balance kettle, so that the solubility of the gas in the liquid is calculated. The size of the liquid volume in the equilibration tank is therefore critical for calculating the solubility of the gas. 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 volume of the liquid absorbing the gas is greatly different from the volume of the pure liquid, so that the volume of the pure liquid which is measured in advance cannot be used for replacing the volume of the liquid after the gas is absorbed in the balance kettle.
There are two existing methods for measuring the volume of liquid in a balance kettle under high pressure. One is to open at two ends of the side of the balance kettle, to install a sapphire window with graduation, and to measure the liquid volume in the balance kettle by observing the graduation value of the liquid level on the window. The other is to install a float in the balance kettle, and the float is above the liquid level. When the liquid volume changes, the scale of the buoy changes, so that the liquid volume in the balance kettle is determined. The first method has the disadvantage that the window graduations are easily coated when the liquid is dark or viscous, making reading difficult and possibly causing large errors in the measurement results. The second method has the defects that a sealing device is needed between the buoy and the kettle cover of the balance kettle, the sealing device ensures that the buoy can freely move up and down, and the air tightness is good, so that high requirements are put on equipment manufacture. In addition, the balance tank usually adopts a buoy, so that the volume of liquid required is large. The solubility measurement of valuable liquids results in higher costs.
In view of the above problems, we propose a new system and method for measuring the volume of liquid at high pressure.
Disclosure of Invention
The invention aims to provide a system and a method for measuring the liquid volume under high pressure, which solve the problems that the reading is difficult, the air tightness and the result accuracy cannot be simultaneously considered due to the deep and thick liquid color in the existing liquid volume measuring technology.
In order to achieve the above objective, an embodiment of the present invention provides a system for measuring a volume of a liquid under high pressure, 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 tank, a first thermostatic water bath, a second thermostatic 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 gas steel bottle, and a measured gas steel bottle; the nitrogen steel cylinder and the detected 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 are controlled to be opened and closed 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 into the buffer tank and the balance kettle; the first thermocouple and the second thermocouple are respectively used for measuring the temperatures in the buffer tank and the balance kettle; the first pressure sensor and the second pressure sensor are respectively communicated into 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 on-line monitoring of pressure change; 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 is 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 when the stirrer in the balance kettle is static.
Further, the first thermocouple and the second thermocouple are electrically connected with the computer and used for monitoring temperature change 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 specifically comprises the following steps: step 1) setting the required temperature in the first constant-temperature water bath and the second constant-temperature water bath; step 2) pouring solid round beads with the volume of V into the balance kettle; step 3) sealing the balance kettle, and placing the balance kettle into the second constant-temperature water bath; step 4) after the temperature of the system is stabilized to be T, opening a first valve, a second valve, a third valve, a fourth valve and a fifth valve, closing a sixth valve, filling a certain amount of nitrogen, and checking the air tightness of the system; step 5), when the air tightness of the system is good, a sixth valve is opened, and a vacuum pump is started to vacuumize the system; closing a sixth valve, and recording the pressure in the balance kettle as P 0 at the moment; step 6) closing a fifth valve between the buffer tank and the balance kettle; step 7), a second valve is opened to fill the tested gas into the buffer tank, and the second valve and the fourth valve are closed; keeping the temperature for a period of time after the buffer tank is inflated, recording the pressure in the buffer tank as P 1, and recording the pressure in the balance kettle as P 2; step 8), a fifth valve is opened, the measured gas is filled into the balance kettle, the fifth valve is closed, and the stable pressure P s in the balance kettle is recorded; step 9) repeating step 7) and step 8); step 10) changing the volume value V of the solid round beads, and repeating the steps 1) to 9); step 11) determining a regression equation by the least squares method by the above operationParameters a ijkl in i+j+k+l.ltoreq.2; wherein i, j, k, l has a value of 0,1, or 2; step 12) changing the solid ball into liquid, repeating the steps 1) to 9), and calculating the volume of the liquid phase in the balance kettle by measuring the temperature in the experimental process, the pressure in the buffer tank before inflation and the pressure in the balance 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 balance.
Further, step 1) to step 11) are performed by using a known volume of solid beads instead of liquid to perform a measurement experiment to obtain the parameter a ijkl in the regression equation.
Further, the solid beads are made of a material which does not have an adsorption effect with the gas to be detected.
Further, when the system is vacuumized, the pressure value in the system is higher than the saturated vapor pressure value of the absorbent used at the current temperature.
Further, if the ionic liquid is used as an 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 kept at a temperature for 30-90min, and then the pressure P 1 in the buffer tank and the pressure P 2 in the balance kettle are recorded.
Further, in step 11), parameters a ijkl in the regression equation are passed through the volume value V, the temperature T, the pressure P 1 in the buffer tank before inflation, and the pressures P 2 and P s in the balance tank before and after inflation of at least 15 sets of different solid beads.
The invention relates to a measuring system, which 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; the thermocouple is connected with the buffer tank and the balance kettle respectively and is used for measuring the temperature in the buffer tank and the balance kettle. The measuring method of the present invention is realized by the measuring device system. And (3) carrying out measurement experiments through solid beads with known volumes, and returning to a quadratic regression equation of the volumes, the buffer tank pressure, the pressure before the balance tank is inflated, the temperature and the pressure after the balance tank is inflated. By adopting the equation, the volume of the liquid when the gas is dissolved in the liquid to reach balance under high pressure is calculated according to the pressure of the buffer tank, the pressure of the balance kettle before and after the inflation and the temperature of the buffer tank. The invention has simple and easy operation, is not affected by the characteristics of deep and viscous liquid color and the like, and has good application prospect.
Compared with the prior art, the invention has the following advantages:
(1) The problem of difficult reading caused by the characteristic of deep and sticky color of the absorbent 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 accurate degree of the 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 consumption of the absorbent is less, and the device has good market prospect.
Drawings
The technical scheme and other beneficial effects of the present application are presented by the detailed description of the specific embodiments of the present application with reference to the accompanying drawings.
Fig. 1 is a schematic structural diagram of a system for measuring a liquid volume under high pressure according to an embodiment of the present application.
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 tested 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 accompanying drawings in the embodiments of the present application. It will be apparent that the described embodiments are only some, but not all, embodiments of the application. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to fall within the scope of the application.
The present invention is directed to a new system and method for measuring the volume of a liquid under high pressure, which solve the above-mentioned drawbacks and disadvantages of the prior art.
In order to achieve the above purpose, the present invention provides the following technical solutions:
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 thermostatic water bath 9, a second thermostatic 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 steel cylinder 18 and the detected gas steel 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 the third valve 3 and the third valve 3 controls the gas on-off; 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 be connected with the computer 15 for online monitoring of temperature change; 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 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 balance kettle 8, and are connected with the computer 15 for on-line monitoring of pressure changes; 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 to the sixth valve 6, and the vacuum pump 16 is used for evacuating the system.
The inner lower end of the balance kettle 8 is provided with a stirrer for stirring the inner cavity of the balance kettle 8, the stirrer is in a static state when the balance kettle 8 is inflated, and the stable pressure of the system is the pressure when the stirrer in the balance kettle is static.
Before the device is used for measuring the volume of liquid under high pressure, the parameters of the equation (1) are obtained by using a quadratic polynomial of the pressure of a round bead regression buffer tank with a known volume, the pressure and the temperature of a balance kettle before and after inflation.
Wherein i, j, k, l has a value of 0, 1, or 2; expanding equation (1) gives its expansion:
The specific operation steps are as follows:
step 1), two water baths are set to be at required temperatures in advance and are equal to each other; which is set to the required temperature in both the first thermostatic waterbath 9 and the second thermostatic waterbath 10;
step 2), cleaning and wiping the balance kettle, and pouring solid round beads with the volume of V into the balance kettle 8;
step 3) closing a cover of the balance kettle, screwing bolts, sealing the balance kettle 8, and placing the balance kettle 8 into the second constant-temperature water bath 10;
Step 4) after the system temperature is stabilized as T, opening a first valve 1, a second valve 2, a third valve 3, a fourth valve 4 and a fifth valve 5, closing a sixth valve 6, filling a certain amount of nitrogen, checking the air tightness of the system, and keeping the pressure unchanged within 30min to show that the air tightness of the device is good;
step 5), when the air tightness of the system is good, opening a sixth valve 6, and starting a vacuum pump 16 to vacuumize the system; closing the sixth valve 6, and recording the pressure in the balance kettle 8 at the moment as P 0;
Step 6) closing a fifth valve 5 between the buffer tank 7 and the balance kettle 8;
Step 7), opening a second valve 2 to charge the tested gas into the buffer tank 7, and closing the second valve 2 and a fourth valve 4; keeping the temperature for a period of time after the buffer tank 7 is inflated, keeping the temperature for 30-90min, and then recording the pressure in the buffer tank 7 as P 1 and the pressure in the balance kettle 8 as P 2;
Step 8), a fifth valve 5 is opened, the measured gas is filled into the balance kettle 8, the fifth valve 5 is closed, and the stable pressure P s in the balance kettle 8 is recorded;
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 the volume values are finished;
Step 11) determining a regression equation by the least squares method by the above operation Parameters a ijkl in i+j+k+l.ltoreq.2; wherein i, j, k, l has a value of 0, 1, or 2;
Step 12) changing the solid ball into liquid, repeating the steps 1) to 9), and calculating the volume of the liquid phase in the balance kettle by measuring the temperature in the experimental process, the pressure in the buffer tank before inflation and the pressure in the balance 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 balance.
In the embodiment, a measurement experiment is carried out through solid beads with known volumes, and a quadratic regression equation of the regression volume, the buffer tank pressure, the pressure before the balance tank is inflated, the temperature and the pressure after the balance tank is inflated is adopted. And by adopting the regression equation, the actual volume of the liquid when the gas is dissolved in the liquid under high pressure to reach balance is calculated according to the initial pressure of the buffer tank, the pressure of the balance kettle before and after the inflation and the temperature of the buffer tank.
Preferably, care is taken to clean the device, and deionized water in the water bath is often replaced to prevent corrosion.
Preferably, the device is placed in a water bath when the air tightness of the device is checked, so that the influence of the fluctuation of the ambient temperature is avoided; the water bath is covered for heat preservation, 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 ball adsorbs the tested gas, the pressure of the balance kettle is difficult to stabilize.
Preferably, when the system is evacuated, the pressure in the system is pumped to a value greater than the saturated vapor pressure of the absorbent used at the current temperature. When the ionic liquid is used as an absorbent, the pressure in the system is pumped to be within 1kPa (absolute pressure), preferably 0-0.5kPa, so that the nitrogen content in the system is reduced as much as possible. When another liquid is used as the absorbent, it is necessary to adjust the pressure by taking into consideration the saturated vapor pressure of the absorbent at the present temperature and combining the saturated vapor pressure of the absorbent at the present temperature.
Preferably, the stirrer is in a static state when the balance kettle is inflated, and the stable pressure is the pressure when the balance kettle stirrer is static.
Preferably, after the experiment is completed, the gas is discharged into an absorption bottle to prevent environmental pollution. After purging with nitrogen for 20 minutes, opening the balance kettle; cleaning the balance kettle and preventing corrosion.
Preferably, the accuracy is improved by regressing the parameters a ijkl in equation (1) by at least 15, preferably more than 20, sets of different solid beads in volume V, temperature T, pressure P 1 in the buffer tank before inflation, and pressures P 2 and P s in the balance tank before and after inflation.
Compared with the prior art, the invention has the following advantages:
(1) The problem of difficult reading caused by the characteristic of deep and sticky absorption liquid 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 accurate degree of the 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 consumption of the absorbent is less, and the device has good market prospect.
The method for measuring the volume of the liquid under the high pressure provided by the invention adopts the system for measuring the volume of the liquid under the high pressure, and the specific embodiment of the method for measuring the volume of the liquid under the high pressure is as follows.
Example 1: equation fitting of CO 2 gas
Solid beads with the volume of 30mL are added into the balance kettle, the temperature is adjusted to 303.15K through a constant-temperature water bath, a certain amount of nitrogen is filled into the system, and the air tightness of the device is checked. After the device was determined to be well airtight, the system was evacuated to 0.3kPa (absolute). Part of CO 2 gas is filled into the system, and after the fifth valve 5 is closed, CO 2 with a certain pressure is filled into the buffer tank. After 70min, the pressure in the buffer tank was taken down to 212.78kPa, the pressure in the balance tank was 129.67kPa, the fifth valve 5 was opened rapidly and then closed, and the steady pressure in the balance tank was taken down to 200.24kPa.
According to the above experimental procedure, a series of experimental data were obtained by varying the volume of the solid beads, the temperature of the system, the initial pressure of the buffer tank and the balance tank, and the results are shown in table 1.
Table 1 results of the experiments of each group
And substituting the experimental result into the equation (1) for fitting to obtain a fitting parameter a 1～a15. The average relative deviation of the equation fit was 0.15% and the maximum relative deviation was 0.30%.
Table 2 fitting parameter values
Example 2: solution of liquid phase volume after introducing CO 2 gas
The temperature of the system was adjusted to 303.15K by a thermostatic water bath, and 52.65g of 1-butyl-3-methylimidazole iron-based ionic liquid was added to 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 is not changed after exceeding 30min, which indicates that the air tightness of the device is good. The system was evacuated to 0.5kPa (absolute pressure) and a solubility measurement experiment was performed. When the gas-liquid phase balance is achieved in the balance kettle, CO 2 with a certain pressure is filled into the buffer tank, after 60min, the pressure in the buffer tank is recorded to be 319.37kPa, the pressure in the balance kettle is 117.26kPa, the fifth valve 5 is opened, the valve is quickly closed, and the stable pressure in the balance kettle is recorded to be 295.27kPa. Substituting the result into the equation (1), and calculating to obtain the volume of the liquid phase in the balance kettle which is 39.32mL when the gas-liquid phase balance is achieved.
According to the steps, the volume of the ionic liquid after absorbing CO 2 under different balance pressures can be calculated through the system temperature, the initial pressure of the buffer tank and the balance kettle before inflation and the stable pressure of the balance kettle after inflation. The results are shown in Table 3.
Table 3 measurement results and calculated liquid volume values of each set of 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: equation fitting for H 2 S gas feed
Solid beads were added to the equilibrater kettle in a volume of 30mL and the system was adjusted to 303.15K by a thermostatic water bath. A certain amount of nitrogen gas was filled into the system to check the air tightness of the device. After the device was determined to be well airtight, the system was evacuated to 0.4kPa (absolute). Part of H 2 S gas is filled into the system, after the fifth valve 5 is closed, H 2 S gas with certain pressure is filled into the buffer tank, after heat preservation is carried out for 65min, the pressure in the buffer tank is recorded as 251.63kPa, the pressure in the balance tank is 142.09kPa, the fifth valve 5 is opened rapidly and then closed, and the stable pressure in the balance tank is recorded as 234.38kPa.
Following the above experimental procedure, a series of experimental data were obtained by varying the volume of the solid beads, the temperature of the system, the initial pressure of the buffer tank and the balance tank, and the results are shown in table 4.
Table 4 measurement results of each set of experiments
And substituting the experimental result into the equation (1) for fitting to obtain a fitting parameter a 1～a15. The average relative deviation of the equation fit was 0.15% and the maximum relative deviation was 0.25%.
Table 5 fitting parameter values
Example 4: solution of liquid phase volume after introducing H 2 S gas
44.69G of 1-butyl-3-methylimidazole iron-based ionic liquid was added to the equilibrated kettle, and the system was adjusted to 323.15K by a thermostatic water bath. And (5) filling a certain amount of nitrogen into the system, and performing device air tightness inspection. After the air tightness of the device was confirmed to be good, the system was evacuated to 0.3kPa (absolute pressure), and a solubility measurement experiment was performed. When the balance of gas and liquid phases is achieved in the balance kettle, H 2 S gas with certain pressure is filled into the buffer tank, after 60min, the pressure in the buffer tank is recorded to be 448.22kPa, the pressure in the balance kettle is 102.83kPa, the fifth valve 5 is opened, and then the stable pressure 419.03kPa in the balance kettle is recorded. Substituting the result into the equation (1), and calculating to obtain the volume of the liquid phase in the balance kettle which is 33.76mL when the gas-liquid phase balance is achieved.
According to the steps, the volume of the ionic liquid after absorbing H 2 S under different balance pressures can be calculated through the system temperature, the initial pressure of the buffer tank and the balance kettle before inflation and the stable pressure of the balance kettle after inflation. The results are shown in Table 6.
Table 6 measurement results and calculated liquid volume values of each set of 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 embodiments are emphasized, and for parts of one embodiment that are not described in detail, reference may be made to related descriptions of other embodiments.
The foregoing has described in detail embodiments of the present application, and specific examples have been employed herein to illustrate the principles and embodiments of the present application, the above description of the embodiments being only for the purpose of aiding in the understanding of the technical solution and core idea of the present application; those of ordinary skill in the art will appreciate that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the application.
Claims (10)
1. The system for measuring the liquid volume 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 detected 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 are controlled to be opened and closed 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 into the buffer tank and the balance kettle; the first thermocouple and the second thermocouple are respectively used for measuring the temperatures in the buffer tank and the balance kettle; the first pressure sensor and the second pressure sensor are respectively communicated into 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 on-line monitoring of pressure change; 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 is used for vacuumizing the system.
2. The system for measuring the volume of liquid under high pressure according to claim 1, wherein the stirrer is arranged at the lower end of the inside of the balance kettle, the stirrer is in a static state when the balance kettle is inflated, and the stable pressure of the system is the pressure when the stirrer in the balance kettle is static.
3. The system of 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, characterized in that a system for determining the volume of a liquid under high pressure according to any one of claims 1 to 3 is used for determining the volume of a liquid under high pressure, comprising the steps of:
step 1) setting the required temperature in the first constant-temperature water bath and the second constant-temperature water bath;
step 2) pouring solid round beads with the volume of V into the balance kettle;
step 3) sealing the balance kettle, and placing the balance kettle into the second constant-temperature water bath;
step 4) after the temperature of the system is stabilized to be T, opening a first valve, a second valve, a third valve, a fourth valve and a fifth valve, closing a sixth valve, filling a certain amount of nitrogen, and checking the air tightness of the system;
Step 5), when the air tightness of the system is good, a sixth valve is opened, and a vacuum pump is started to vacuumize the system; closing a sixth valve, and recording the pressure in the balance kettle as P 0 at the moment;
Step 6) closing a fifth valve between the buffer tank and the balance kettle;
Step 7), a second valve is opened to fill the tested gas into the buffer tank, and the second valve and the fourth valve are closed; keeping the temperature for a period of time after the buffer tank is inflated, recording the pressure in the buffer tank as P 1, and recording the pressure in the balance kettle as P 2;
step 8), a fifth valve is opened, the measured gas is filled into the balance kettle, the fifth valve is closed, and the stable pressure Ps in the balance kettle is recorded;
Step 9) repeating step 7) and step 8);
Step 10) changing the volume value V of the solid round beads, and repeating the steps 1) to 9);
Step 11) determining a regression equation by the least squares method by the above operation Parameters a ijkl in (a); wherein i, j, k, l has a value of 0, 1, or 2;
Step 12) changing the solid ball into liquid, repeating the steps 1) to 9), and calculating the volume of the liquid phase in the balance kettle by measuring the temperature in the experimental process, the pressure in the buffer tank before inflation and the pressure in the balance 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 balance.
5. The method according to claim 4, wherein the step 1) to the step 11) are performed by using solid beads of known volume instead of the liquid to obtain the parameter a ijkl in the regression equation.
6. The method according to claim 4, wherein the solid beads are made of a material that does not adsorb the gas to be measured.
7. The method of measuring the volume of a liquid at a high pressure according to claim 4, wherein the system is evacuated until the pressure in the system is higher than the saturated vapor pressure of the absorbent used at the present temperature.
8. A method according to claim 7, wherein if the ionic liquid is used as the absorbent, the pressure in the system is pumped to within 1 kPa.
9. The method according to claim 4, wherein after the buffer tank is inflated, the buffer tank is kept warm for 30-90min, and the pressure P 1 in the buffer tank and the pressure P 2 in the balance tank are recorded.
10. The method according to claim 4, wherein in the step 11), the parameters a ijkl in the regression equation are obtained by at least 15 different sets of solid beads of volume value V, temperature T, pressure P 1 in the buffer tank before aeration, and pressures P 2 and P s in the balancing tanks before and after aeration.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111604467.3A CN114279890B (en) | 2021-12-24 | 2021-12-24 | System and method for measuring liquid volume under high pressure |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111604467.3A CN114279890B (en) | 2021-12-24 | 2021-12-24 | System and method for measuring liquid volume under high pressure |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114279890A CN114279890A (en) | 2022-04-05 |
| CN114279890B true CN114279890B (en) | 2024-06-07 |
Family
ID=80875478
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111604467.3A Active CN114279890B (en) | 2021-12-24 | 2021-12-24 | System and method for measuring liquid volume under high pressure |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114279890B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117782878B (en) * | 2024-02-26 | 2024-04-26 | 太原理工大学 | Constant pressure device and method for measuring dissolution parameters of gas in liquid in real time |
| CN117871591A (en) * | 2024-03-13 | 2024-04-12 | 中海石油气电集团有限责任公司 | Fluid phase balance measuring device and method suitable for different volatility characteristics |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5342580A (en) * | 1990-04-17 | 1994-08-30 | Alan Brenner | Apparatus and method for measuring the amount of gas adsorbed on or desorbed from a solid and reactions of a gas with a solid |
| KR100658642B1 (en) * | 2005-07-19 | 2006-12-21 | 정경환 | Measuring method of gas storage capacity onto high pressure and the apparatus for measuring the gas storage capacity |
| CN101819170A (en) * | 2010-05-13 | 2010-09-01 | 大连理工大学 | Non-integrated variable volume high-pressure phase balance measuring device |
| CN105806738A (en) * | 2016-03-11 | 2016-07-27 | 西安交通大学 | Variable-volume pressure fixing device and method for measuring solubility of gas in liquid |
| CN206074384U (en) * | 2016-07-21 | 2017-04-05 | 浙江工业大学 | A kind of experimental provision for determining vapor liquid equilibrium data |
| JP2017125773A (en) * | 2016-01-14 | 2017-07-20 | 株式会社デンソー | Device and method for airtight leakage inspection |
| CN112881230A (en) * | 2021-03-23 | 2021-06-01 | 中国石油大学(华东) | Shale gas vibration desorption test evaluation device and method |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103038507B (en) * | 2010-02-23 | 2016-04-06 | 阿尔特弥斯智能动力有限公司 | The valve timing of fluid-working machine |
-
2021
- 2021-12-24 CN CN202111604467.3A patent/CN114279890B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5342580A (en) * | 1990-04-17 | 1994-08-30 | Alan Brenner | Apparatus and method for measuring the amount of gas adsorbed on or desorbed from a solid and reactions of a gas with a solid |
| KR100658642B1 (en) * | 2005-07-19 | 2006-12-21 | 정경환 | Measuring method of gas storage capacity onto high pressure and the apparatus for measuring the gas storage capacity |
| CN101819170A (en) * | 2010-05-13 | 2010-09-01 | 大连理工大学 | Non-integrated variable volume high-pressure phase balance measuring device |
| JP2017125773A (en) * | 2016-01-14 | 2017-07-20 | 株式会社デンソー | Device and method for airtight leakage inspection |
| CN105806738A (en) * | 2016-03-11 | 2016-07-27 | 西安交通大学 | Variable-volume pressure fixing device and method for measuring solubility of gas in liquid |
| CN206074384U (en) * | 2016-07-21 | 2017-04-05 | 浙江工业大学 | A kind of experimental provision for determining vapor liquid equilibrium data |
| CN112881230A (en) * | 2021-03-23 | 2021-06-01 | 中国石油大学(华东) | Shale gas vibration desorption test evaluation device and method |
Non-Patent Citations (1)
| Title |
|---|
| 常温高压下气体在液体中溶解度测定装置的研制;吕秀阳, 吴兆立;高校化学工程学报;19920630(第02期);全文 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114279890A (en) | 2022-04-05 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN114279890B (en) | System and method for measuring liquid volume under high pressure | |
| CN112432889B (en) | Method for measuring rock porosity by liquid saturation method and correction method | |
| US11312625B2 (en) | Hydrogen sulfide mixture, method for producing same, and filling container | |
| Holldorff et al. | Vapor pressures of n-butane, dimethyl ether, methyl chloride, methanol and the vapor-liquid equilibrium of dimethyl ether-methanol:: Experimental apparatus, results and data reduction | |
| CN103528909A (en) | Determination apparatus for gas solubility and usage method | |
| WO2017181392A1 (en) | Method for measuring diffusion coefficient of carbon dioxide in crude oil | |
| CN202372338U (en) | Breathing valve calibrating table | |
| CN113092310A (en) | Transformer oil gas content testing device and method for measuring density by U-shaped oscillation tube | |
| CN107677699A (en) | It is a kind of under high conditions in mirror surface dew point method detection gas micro-water content method | |
| CN104215547B (en) | A kind of test method utilizing succusion detection new running transformer oil air content | |
| EP4257956A1 (en) | Method and apparatus for calibrating optical dissolved oxygen sensor | |
| CN111595408B (en) | Equipment for measuring liquid level in constant-temperature closed container, film coating device and method for measuring liquid level | |
| CN113740202B (en) | Volumetric adsorption measurement method and device | |
| CN113884645A (en) | Device is prepared to methane henry constant standard in experimental water | |
| CN109211726B (en) | On-line resonant densimeter calibrating device | |
| CN203490145U (en) | Gas solubility measuring device | |
| CN113866373A (en) | Method and cavity for measuring Henry constant of methane in water | |
| BR112019008362B1 (en) | APPARATUS AND METHODS FOR MONITORING THE QUALITY OF GAS IN A PROCESS STREAM IN A SUBSEA LOCATION | |
| CN102519686B (en) | Sterilization intensity detector is combined the detection method of sealing with Bottle neck for wine bottle | |
| CN107340214B (en) | System for detecting adsorption capacity of molecular sieve under high pressure condition and detection method thereof | |
| CN113670702A (en) | Gas mixing system and gas mixing method for SF6 decomposed gas | |
| CN112782340A (en) | Method for measuring hydrogen content in chlorine | |
| KR20180010473A (en) | measurment method of pressing water without pressure container for pressure inspection of non-water jacket type for pressure container | |
| CN219104842U (en) | Liquefied gas moisture testing arrangement | |
| KR100210652B1 (en) | Method and apparatus for measuring specific surface area in porous material sample |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant |