CN107290249B - Observation of supercritical CO2Method of gas diffusion phenomenon - Google Patents
Observation of supercritical CO2Method of gas diffusion phenomenon Download PDFInfo
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Abstract
Observation of supercritical CO2-a method of gas diffusion phenomenon comprising the steps of: 1) introducing CO2And experimental gas A is respectively filled into the gas active areas of the two evacuated high-temperature high-pressure gas piston containers, and supercritical CO is added2Placing a coloring agent into a gas diffusion area of the visual reaction kettle; 2) vacuumizing a gas diffusion area of the visual reaction kettle and heating to an experimental temperature which is not lower than CO2A critical temperature; 3) piston-compressing CO in high-temperature high-pressure gas container2Injecting the mixture into a gas diffusion area of a visual reaction kettle for dyeing, wherein the experimental pressure is not lower than CO2Critical pressure, recording CO in the reactor2The state of (1); 4) to be treated with CO2After dyeing uniformly, injecting the experimental gas A in the high-temperature high-pressure gas piston container into a gas diffusion area of the visual reaction kettle, and observing and/or recording supercritical CO in the reaction kettle2The state of the test gas a. The method can visually evaluate the supercritical CO2-gas diffusion phenomena.
Description
Technical Field
The invention relates to the field of oil and gas field development, in particular to a method for observing supercritical CO under the conditions of high temperature and high pressure2-visualization of the gas diffusion phenomenon.
Background
Diffusion is a phenomenon in which a component having a concentration gradient in a system is transferred from a high concentration region to a low concentration region. The diffusion phenomenon is spread in various fields of chemical industry, building material industry, food industry and the like, and the diffusion process is complex and comprises a plurality of diffusion mechanisms. The research on the diffusion phenomenon is beneficial to deepening the understanding of the mass transfer process, and has important theoretical and industrial significance.
CO at normal temperature and pressure2Diffusion speed between other gases is fast, but under high temperature and high pressure, due to supercritical CO2The diffusion rate may be greatly reduced due to the property difference between the supercritical CO and other gases2The difference of gas diffusion properties is widely applied to the fields of petroleum and natural gas, environmental protection, chemical industry and the like, particularly the properties that the carbon dioxide is low in diffusion coefficient in natural gas and is not easy to mix are utilized for improving the recovery ratio of the gas reservoir and sealing and storing the carbon dioxide in the gas reservoir, and the gas reservoir recovery effect is obvious.
At present, because the calculation of the molecular diffusion phenomenon has no unified theoretical method, an experimental test means is generally adopted for research. There are two main experimental research methods: the method comprises the steps of sampling fluid at different time and different diffusion distances by a direct method, analyzing the samples to obtain gas concentration data, and evaluating the diffusion phenomenon by combining with a corresponding mathematical model; the other is indirect method, which is determined by testing the change of system pressure, fluid density and the like caused by inter-phase mass transfer and adopting a corresponding mathematical model. In recent years, with the development of modern testing techniques, indirect methods have become the primary means of testing molecular diffusion. A representative example is Riazi M R (A new method for experimental measurement of differential coeefficients in Reservoir fluids [ J]，SPEJ，1996， 14(5)：235-250)、GuoP(Molecular Diffusion Coefficients of the Multi-component Gas-Crude OilSystems under High Temperature and Pressure[J]，Industrial&Engineering chemistry Research, 2009, 48: 9023-]，Journalof Canadian Petroleum Technology，1989，28(2)：63-90)、Wen Y(Estimation ofdiffusion coefficients in bitumen solvent mixtures using low field NMR and X-ray cat scanning[C]The 5th International Conference oil Petroleum phase Behavior and Fouling, Banff, Alberta, Canada, June 13-17th, 2004), etc. by using laser and X-ray scanning technique to test The Diffusion between black oil and Liquid light hydrocarbon components by Measuring The saturation curve, and patent document CN104390886A discloses a Method for rapidly determining The Gas-Liquid Diffusion Coefficient by using nuclear magnetic resonance imaging technique, Yang D (Dynamic Interactive testing Method for Measuring The Gas Diffusion Coefficient and Interactive Mass Transfer Cooefficient in a Liquid [ J ] J]，Industrial&Engineering chemistry Research, 2006, 45: 4999-5008), and the like by using a dynamic interfacial tension test method2Diffusion in saline, etc. However, the above method has the following disadvantages: 1) evaluation of supercritical CO2Less gas diffusion phenomena; 2) the direct method needs continuous sampling, gas concentration is tested, and a system is disturbed in the sampling process, so that molecular diffusion cannot be completely and truly embodied; 3) the experimental process is not intuitive enough. At present, the method for visually observing supercritical CO under the conditions of high temperature and high pressure is lacked2-a gas diffusion phenomenon.
Realizing visual observation requires distinguishing supercritical CO2With other gases, primarily by supercritical CO2The dyeing method of (1). George et al (solubility study of disperse dyes in supercritical carbon dioxide fluid [ J)]Dyeing & printing, 2005, 31(10):21-24), abalone-duckweed, etc. (test of solubility of supercritical carbon dioxide dye [ J)]The research on dyeing & printing, 2003, 29(3):29-32) discussed the use of different commercial disperse dyes in supercritical CO2The medium solubility of the commercial disperse dye is easy to dissolve in supercritical CO due to weak molecular polarity and small molecular weight2And forms a phase therewith, which distinguishes supercritical CO2And lays a foundation with other gases.
Disclosure of Invention
The invention aims to establish the observation of supercritical CO under the conditions of high temperature and high pressure2A gas diffusion phenomenon method, which utilizes the weak polarity, small molecular weight and easy solubility in supercritical CO of disperse dye molecules2Forming an equal characteristic to supercritical CO2Dyeing, to distinguish supercritical CO2Lays a foundation with other gases, and further realizes supercritical CO2Visualization and visual evaluation of the gas diffusion phenomenon.
In order to achieve the above object, the present invention provides a method for observing supercritical CO2-a method of gas diffusion phenomena, comprising the steps of:
1) introducing CO2The experimental gas A is respectively filled into gas active areas of two high-temperature high-pressure gas piston containers which are vacuumized, the gas active area is one of two independent areas of the high-temperature high-pressure gas piston container divided by a piston, and the other area is a pressure control area;
supercritical CO2Placing a coloring agent into a gas diffusion area of the visual reaction kettle; the gas diffusion area is one of two independent areas divided by a piston of the visual reaction kettle, and the other area is a pressure control area;
2) vacuumizing a gas diffusion area of the visual reaction kettle and heating to an experimental temperature which is not lower than CO2A critical temperature;
3) piston-compressing CO in high-temperature high-pressure gas container2Injecting the mixture into a gas diffusion area of a visual reaction kettle for dyeing, keeping the pressure in the reaction kettle constant as an experimental pressure in the injection process, wherein the experimental pressure is not lower than CO2Critical pressure, recording CO in the reactor2The state of (1);
4) to be treated with CO2After dyeing uniformly, injecting the experimental gas A in the high-temperature high-pressure gas piston container into a gas diffusion area of a visual reaction kettle, keeping the pressure in the reaction kettle constant as the experimental pressure in the injection process, and recording the supercritical CO in the reaction kettle2The state of the test gas a.
According to the method provided by the invention, the device used in the method comprises: visual reation kettle, oven, high-pressure plunger pump, high temperature high pressure gas piston container, vacuum pump, high-pressure manometer, pipe valve spare, light source and high definition camera device. The high-temperature high-pressure gas piston container is divided into two independent areas by the piston: a gas active zone and a pressure control zone; the visual reaction kettle is divided into two independent areas by a piston: a gas diffusion zone and a pressure control zone. The oven provides a constant high-temperature environment for the visual reaction kettle, the high-temperature high-pressure gas container and the pipe valve. And the two sets of high-pressure plunger pumps respectively provide gas injection power and control the system pressure of the visual reaction kettle. And the vacuum pump removes air in the visual reaction kettle, the two sets of high-temperature high-pressure gas piston containers and the pipe valve member before filling the experimental medium. The high-pressure gauge is used for measuring the gas injection pressure and the system pressure of the visual reaction kettle.
The visual reaction kettle is a high-temperature high-pressure visual reaction kettle, the material can be transparent high-temperature and high-pressure resistant material, the bearable maximum temperature is 150 ℃, and the maximum pressure is 70 MPa.
According to the method provided by the invention, the temperature and the pressure of the experiment can meet the requirement that CO is enabled to be generated2It is in the critical state. Preferably, the experimental temperature is CO2Critical temperature of 150 ℃ and experimental pressure of CO2The critical pressure is 70 MPa.
According to the method provided by the invention, the recording is preferably a photograph. The gas phenomenon in the visual reation kettle is shot to adoption high definition camera device in the experimentation. Specifically, the rear part of the visual reaction kettle adopts a light source for transmission, and the front part adopts a high-definition camera device for shooting the gas state in the reaction kettle.
According to the method provided by the invention, the experimental gas A is preferably selected from inert gases and/or organic hydrocarbon gases. The test gas a is further preferably methane and/or ethane.
According to the method provided by the invention, in step 3), CO is preferably fed at a constant speed2And injecting the mixture into a gas diffusion area of the visual reaction kettle.
According to the method provided by the invention, in the step 4), the experimental gas A is preferably injected into the gas diffusion area of the visual reaction kettle at a constant speed.
According to the method provided by the invention, in the step 4), preferably, the supercritical CO in the gas diffusion area of the visual reaction kettle is continuously shot at certain time intervals2The state of the test gas A and the time until supercritical CO is recorded2The experimental gas a is mixed homogeneously.
According to the method provided by the invention, in the step 3) and the step 4), preferably, a high-pressure plunger pump is used for keeping the pressure in the gas diffusion area of the visual reaction kettle constant to be the experimental pressure.
According to the method provided by the invention, preferably, the supercritical CO2The coloring agent is selected from anthraquinone dye or azo dye, and the concentration of the coloring agent is preferably 0.02 g/L-0.2 g/L. The supercritical CO2The coloring agent is preferably disperse scarlet S-BWFL with chemical name of 2,2' - [ [ 3-acetamido-4- [ (4-nitrophenyl) azo ]]Phenyl radical]Imino radical]Diethyl diacetate, molecular structure shown below:
compared with the prior art, the invention has the beneficial effects that: the invention utilizes the advantages of weak molecular polarity, small molecular weight and easy dissolution in supercritical CO of the disperse dye2Formation of one phase, for supercritical CO2Dyeing, to distinguish supercritical CO2Lays a foundation with other gases and can visually evaluate the supercritical CO2Gas diffusion phenomena, enabling the observation of supercritical CO under conditions of high temperature and high pressure2Visualization and visual evaluation of the gas diffusion phenomenon, enabling the diffusion between molecules to be realistically represented.
Drawings
FIG. 1 shows a schematic diagram of an experimental setup and a flow chart of the method of the invention.
The numbers in the above figures are illustrated as follows:
the device comprises the following components of 1-a visual reaction kettle, 2-an oven, 3-1-a high-pressure plunger pump, 3-2-a high-pressure plunger pump, 4-1-a high-temperature and high-pressure gas piston container, 4-2-a high-temperature and high-pressure gas piston container, 5-a vacuum pump, 6-a high-pressure gauge, 7-1-a pipe valve, 7-2-a pipe valve, 7-3-a pipe valve, 8-a light source and 9-a high-definition camera.
Detailed Description
Preferred embodiments of the present invention will be described in more detail below with reference to the accompanying drawings. While the preferred embodiments of the present invention are shown in the drawings, it should be understood that the present invention may be embodied in various forms and should not be limited to the embodiments set forth herein.
Example 1
This example is to observe supercritical CO2In CH4The diffusion phenomenon in (1). An experimental set-up as shown in figure 1 was used. Supercritical CO used2The coloring agent is disperse scarlet S-BWFL.
The specific experimental steps are as follows:
1) introducing CO2And CH4Respectively filling the gas active areas into the gas active areas of two high-temperature and high-pressure gas piston containers 4-1 and 4-2 which are vacuumized, wherein the gas active area is one of two independent areas divided by the piston of the high-temperature and high-pressure gas piston containers 4-1 and 4-2, and the other area is a pressure control area;
placing the disperse scarlet S-BWFL into a gas diffusion area of a visual reaction kettle 1; the gas diffusion area is one of two independent areas of the visual reaction kettle divided by the piston 1, and the other area is a pressure control area;
2) vacuumizing a gas diffusion area of the visual reaction kettle 1 by using a vacuum pump 5, heating to 85 ℃ by using an oven 2, and starting an experiment after the temperature of a system is stable;
3) the CO in the high-temperature high-pressure gas piston container 4-1 is compressed by a high-pressure plunger pump 3-22Injecting the mixture into a gas diffusion area of a visual reaction kettle 1 for dyeing, driving the lower part of a piston of the visual reaction kettle 1 by using a high-pressure plunger pump 3-1 in the injection process, measuring the gas injection pressure by using a high-pressure gauge 6, keeping the pressure in the reaction kettle constant at 10MPa, stopping injecting gas after injecting 25ml, and recording CO in the reaction kettle2The state of (1);
4) to be treated with CO2After dyeing uniformly, the CH in the high-temperature high-pressure gas piston container 4-2 is treated4Injecting the gas into a gas diffusion area of the visual reaction kettle 1, driving the lower part of a piston of the visual reaction kettle 1 by using a high-pressure plunger pump 3-1 in the injection process, measuring the gas injection pressure by using a high-pressure gauge 6, keeping the pressure in the reaction kettle constant at 10MPa, stopping injecting gas after injecting 75ml, closing an injection valve of the visual reaction kettle 1, transmitting the rear part of the visual reaction kettle 1 by using a light source 8, and shooting supercritical CO in the reaction kettle by using a high-definition camera device 9 at the front part of the visual reaction kettle 12-CH4The initial state of (a); continuously shooting supercritical CO in the reaction kettle according to a certain time interval2-CH4Until the color of the gas in the reaction vessel was uniform, and the equilibrium time was recorded to be 77 hours.
Examples 2 to 4
An experiment was conducted in accordance with the method in example 1 except that the experimental pressures were 15MPa, 20MPa, and 25MPa, respectively.
The experimental pressures and recorded equilibration times for examples 1-4 are shown in table 1.
TABLE 1
| Numbering | Experimental pressure (MPa) | Equilibration time (h) |
| Example 1 | 10 | 77 |
| Example 2 | 15 | 118 |
| Example 3 | 20 | 190 |
| Example 4 | 25 | 213 |
The above experimental results show that the method of the invention can realize the observation of supercritical CO under the conditions of high temperature and high pressure2-gas diffusion. It can also be seen that the higher the pressure, the supercritical CO2In CH4The slower the diffusion speed in (1).
Having described embodiments of the present invention, the foregoing description is intended to be exemplary, not exhaustive, and not limited to the embodiments disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments.
Claims (9)
1. Observation of supercritical CO2-a method of gas diffusion phenomenon, characterized in that it comprises the following steps:
1) introducing CO2The experimental gas A is respectively filled into gas active areas of two high-temperature high-pressure gas piston containers which are vacuumized, the gas active area is one of two independent areas of the high-temperature high-pressure gas piston container divided by a piston, and the other area is a pressure control area;
supercritical CO2Placing a coloring agent into a gas diffusion area of the visual reaction kettle; the gas diffusion area is one of two independent areas divided by a piston of the visual reaction kettle, and the other area is a pressure control area;
2) vacuumizing a gas diffusion area of the visual reaction kettle and heating to an experimental temperature which is not lower than CO2A critical temperature;
3) piston-compressing CO in high-temperature high-pressure gas container2Injecting the mixture into a gas diffusion area of a visual reaction kettle for dyeing, keeping the pressure in the reaction kettle constant as an experimental pressure in the injection process, wherein the experimental pressure is not lower than CO2Critical pressure, observing and/or recording CO in the reactor2The state of (1);
4) to be treated with CO2After dyeing uniformly, injecting the experimental gas A in the high-temperature high-pressure gas piston container into a gas diffusion area of a visual reaction kettle, keeping the pressure in the reaction kettle constant as the experimental pressure in the injection process, and observing and/or recording supercritical CO in the reaction kettle2-the state of the test gas a;
wherein the experimental gas A is selected from inert gas and/or organic hydrocarbon gas.
2. Observing supercritical CO according to claim 12-a gas diffusion phenomenon, wherein said recording is a shot.
3. Observing supercritical CO according to claim 12-a gas diffusion phenomenon, wherein said test gas a is selected from methane and/or ethane.
4. Observation of supercritical CO according to any of claims 1-32A gas diffusion phenomenon method, wherein, in step 3), CO is supplied at a constant rate2And injecting the mixture into a gas diffusion area of the visual reaction kettle.
5. Observation of supercritical CO according to any of claims 1-32-a gas diffusion phenomenon, wherein, in step 4), the test gas a is injected at a constant rate into the gas diffusion zone of the visual reaction vessel.
6. Observation of supercritical CO according to any of claims 1-32A method for gas diffusion phenomenon, wherein, in the step 4), supercritical CO in a gas diffusion area of a visual reaction kettle is continuously shot according to certain time intervals2Condition of the test gas AAnd recording the time until supercritical CO2The experimental gas a is mixed homogeneously.
7. Observation of supercritical CO according to any of claims 1-32-a gas diffusion phenomenon, wherein in step 3) and step 4), the pressure in the gas diffusion zone of the visual reaction vessel is kept constant at the experimental pressure by means of a high-pressure plunger pump.
8. Observing supercritical CO according to claim 12-method of gas diffusion phenomenon, wherein said supercritical CO2The coloring agent is selected from anthraquinone dye or azo dye, and the concentration of the coloring agent is preferably 0.02 g/L-0.2 g/L.
9. Observing supercritical CO according to claim 82-method of gas diffusion phenomenon, wherein said supercritical CO2The coloring agent is disperse scarlet S-BWFL.
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| CN108181431B (en) * | 2017-12-28 | 2023-09-29 | 中国华能集团公司 | Related CO 2 Solubility experiment system and method |
| CN109163880B (en) * | 2018-09-18 | 2020-02-07 | 天津大学 | Method for simulating formation and air leakage process of carbon dioxide saturated solution |
| CN113049763B (en) * | 2021-03-08 | 2022-02-11 | 西南石油大学 | Experimental testing device and testing method for salt precipitation concentration of high-temperature high-pressure real formation water |
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