CN108169078B - FeCO3High CO content at medium and low temperature2Device and method for testing solubility in aqueous solution - Google Patents

FeCO3High CO content at medium and low temperature2Device and method for testing solubility in aqueous solution Download PDF

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CN108169078B
CN108169078B CN201810011984.1A CN201810011984A CN108169078B CN 108169078 B CN108169078 B CN 108169078B CN 201810011984 A CN201810011984 A CN 201810011984A CN 108169078 B CN108169078 B CN 108169078B
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feco
pipeline
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solubility
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CN108169078A (en
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邓宽海
林元华
刘婉颖
刘冰
潘潇扬
韦奇
曾德智
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Southwest Petroleum University
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Abstract

The invention provides FeCO3High CO content at medium and low temperature2The device and the method for testing the solubility in the water solution mainly comprise the following steps: the device comprises a vacuum pump, a first valve, a first precision valve, a second valve, a pressure gauge, a thermometer, a second precision valve, a pipette, a third valve, a fourth valve, a liquid taking pipe, a fifth valve, a top cover, a gas collecting bottle, a reaction cylinder, a micro CT probe, a magnetic stirring rod, a magnetic stirrer, a constant temperature box, a glass window, a first pipeline, a second pipeline, a third pipeline and the like. The invention utilizes the suction of a vacuum pump and CO2The injection of the test solution can well realize the anaerobic condition in the whole test process, avoid the influence of oxygen on the test result of the solubility of the ferrous carbonate, and monitor FeCO in real time3The method for comprehensively determining FeCO in solution by combining the deposition and dissolution kinetic processes and the multiple sampling method with the spectrophotometry and the complexometric titration3Solubility. The invention is suitable for the technical field of acid gas reservoir and carbon dioxide flooding development.

Description

FeCO3High CO content at medium and low temperature2Device and method for testing solubility in aqueous solution
Technical Field
The invention relates to the technical field of acid gas reservoir and carbon dioxide thickened oil flooding development, in particular to FeCO3High CO content at medium and low temperature2Device for testing solubility in aqueous solution anda method.
Background
In the presence of CO2Acid gas reservoir and use of CO2In reservoir exploration and development of reservoir oil displacement, CO2The corrosion problem is always an important problem facing the exploration and development of petroleum and natural gas. Thus investigating the presence of carbon steel in CO2Corrosion behavior (including corrosion rate, corrosion characteristics, corrosion morphology, etc.) and the failure modes induced by it are highly desirable in the environment.
In recent years, research means such as XRD, XPS and SEM have proved that carbon steel is in CO2The corrosion product in the environment is mainly FeCO3And a small amount of iron oxide, and it has been shown in prior studies that as corrosion proceeds, Fe is present in solution2+Increase continuously when Fe is in solution2+And CO3 2-Over FeCO3When the solubility of (2) is high, FeCO3The crystal will nucleate and grow on the surface of the sample to form FeCO3Film and FeCO3The membrane has good protection effect on the carbon steel pipeline in a sulfur-free system, and the protection effect of the membrane and FeCO3The film characteristics (including the growth and formation process of the film, structure, form, thickness, density, bonding strength between the product film and the substrate, i.e. adhesive force, elastic modulus, hardness, etc.) are closely related. Influencing CO2Corrosion product FeCO3The main and important factors of the film properties include temperature, CO2Partial pressure and acidity/PH of the etching medium, etc.
With respect to the pH of the corrosive medium, Dugstad et al have found that the pH of the solution affects FeCO3Solubility of FeCO at low pH3The film tends to dissolve and is in 2<PH<5, the solubility of the film increases with increasing acidity, resulting in an increasing corrosion rate, while at high pH values it is more favorable for FeCO3Deposition of the film, and therefore, as the corrosion proceeds, the cathodic reaction consumes H in the solution+Resulting in an increase in pH, FeCO3The solubility decreases, the corrosion product film forms and the growth rate thereof may increase, and the corrosion rate is continuously decreased. In summary, the acidity and pH of the solution primarily control the etch rate by affecting the solubility of the film.
With respect to temperature, the studies of Wang Xiao Bo and Xileining, etc. show that at low temperature, a film FeCO is formed due to the corrosion product3Very high solubility, i.e. FeCO3The solubility has a negative temperature relationship, the surface component of the sample is mainly Fe after the sample is corroded, and only a small amount of FeCO is generated on the surface of the sample3Corrosion products; while with increasing temperature, on the one hand the Fe accelerates2+On the other hand, reduces FeCO3The combined action of the two results in FeCO near the surface of the sample3Easily exhibit a supersaturated state, thereby accelerating FeCO3The deposition on the surface of the sample and the forming rate of the film layer are increased, the thickness of the film layer is also increased continuously, the progress of the corrosion process is inhibited, and the corrosion rate is reduced. At temperatures greater than 150 deg.C, the film FeCO forms as a result of corrosion products in solution3A kinetic balance of deposition and dissolution is exhibited and the film thickness tends to be stable. Thus, FeCO3Solubility to CO of2The corrosion behavior (especially corrosion rate and corrosion product film properties) has a significant impact.
For CO2Partial pressure of CO2After increasing the partial pressure, first, CO2Increased solubility, increased acidity of the solution, increased hydrogen depolarization and increased FeCO3Solubility, promote corrosion, and secondly, FeCO3With CO2And H2O reaction to form soluble Fe (HCO)3)2Thereby increasing FeCO3And thirdly, as the corrosion rate increases, Fe is more easily formed in the vicinity of the metal surface2+Supersaturated solution layer to promote FeCO3And the formation of protective corrosion product films to inhibit corrosion; apparently, the corrosion behavior is the result of the coordination of the three components, but the practical analysis shows that the corrosion behavior is mainly affected by FeCO3And controlling the solubility.
As can be seen, the corrosion product film FeCO3The solubility of (A) can directly reflect CO2Severity of corrosion, especially in the medium-low temperature stage: (<80 deg.C) or early in corrosion, temperature, CO2The partial pressure and pH are important but the nature is openOver-influencing FeCO3Solubility indirectly affects its corrosion behavior, and thus FeCO is obtained3At different temperatures, CO2Solubility at component force and pH vs. CO2The research of corrosion mechanism is very necessary, so the invention aims to provide FeCO in the medium-low temperature and early corrosion stage3The concentration of (3) can be determined by the concentration test method of (2)2Corrosion of metals in the environment. In addition, it should be noted that, first, CO2Dissolved in water to form H2CO3Resulting in a pH drop of the aqueous solution with a minimum pH of about 3.0, and secondly, no CO2Or low CO content2Water-soluble neutral FeCO3Higher CO in deposition-dissolution kinetics and solubility2Content namely CO2Partial pressure will significantly accelerate FeCO3The deposition-dissolution kinetics of (a) and its solubility. Thus, CO2Partial pressure pair FeCO3The influence of solubility is to some extent equivalent to pH, so that it influences FeCO3The main factors of solubility are temperature and CO2Partial pressure. At present, no testing device and method capable of accurately obtaining medium-low temperature high CO exist2Partial pressure (equivalent to high CO content in aqueous solution)2) The solubility of ferrous carbonate in aqueous solution. Therefore, the present invention provides a FeCO3High CO content at medium and low temperature2The device and the method for testing the solubility in the water solution can promote the CO of the carbon steel2Corrosion study to further clarify CO of carbon steels2Corrosion mechanism, and may be CO2Prediction and protection from corrosion provides a better basis.
Disclosure of Invention
The invention aims to provide FeCO3High CO content at medium and low temperature2Device and method for testing solubility in aqueous solution to solve the problem that ferrous carbonate contains high content of CO at medium and low temperature2The technical problem that the solubility in the aqueous solution is difficult to accurately obtain is solved, the complexity of a testing device is simplified while the aim is fulfilled, and the cost of equipment is reduced.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention proposesFeCO of3High CO content at medium and low temperature2The testing device for the solubility in the water solution mainly comprises: the device comprises a vacuum pump, a first valve, a first precision valve, a second valve, a pressure gauge, a thermometer, a second precision valve, a pipette, a third valve, a fourth valve, a liquid taking pipe, a fifth valve, a top cover, a gas collecting bottle, a reaction cylinder, a micro CT probe, a magnetic stirring rod, a magnetic stirrer, a constant temperature box, a side cover, a side bolt, a glass window, a top bolt, a first pipeline, a second pipeline, a third pipeline and a fourth pipeline. Wherein, the vacuum pump is used for pumping the whole test system and forming a certain negative pressure, and the third pipeline and the first precision valve are used for injecting specified CO into the reaction cylinder, the first pipeline, the second pipeline and the fourth pipeline2Partial pressure, suction from vacuum pump and CO2The air of the whole test system can be well exhausted by the injection of the test system; the first pipeline is used for communicating the pipette, the fourth pipeline and the vacuum pump, and the second pipeline is used for communicating the liquid taking pipe and the reaction barrel; the first valve, the second valve, the third valve, the fourth valve and the fifth valve are used for controlling the trend of fluid in all pipelines, and the second precision valve and the liquid taking pipe are used for accurately taking samples from the reaction cylinder; the reaction cylinder for dissolving the ferrous carbonate consists of a top cover, a top bolt, a side cover, a side bolt, a glass window, a thermometer, a pressure gauge and a sealing ring; the magnetic stirrer and the stirring rod are used for stirring the solution to accelerate the full dissolution of the ferrous carbonate; the micro CT probe on the glass window is used for monitoring the deposition and dissolution kinetic process of the ferrous carbonate; a thermostat heated by water bath is used for controlling the temperature of the reaction cylinder; the gas collecting bottle is used for collecting gas discharged in the deoxygenation process of the pipette; the temperature gauge and the pressure gauge are respectively used for displaying the temperature and the CO in the process of testing the solubility of the ferrous carbonate2Partial pressure.
After the pipette is deaerated, the reaction cylinder is sucked by a vacuum pump to form negative pressure, and CO passing through the second pipeline2The liquid in the pipette is injected into the reaction cylinder under negative pressure by pressure.
After the ferrous carbonate is dissolved and deposited to reach dynamic equilibrium each time, the liquid taking pipe, the second precision valve and the second pipeline of the invention pass through the reaction cylinderCO2The ferrous carbonate solution in the reaction cylinder is taken out under the action of pressure.
Compared with the prior art, the invention has the following advantages:
(1) the invention can realize the high CO content of ferrous carbonate at medium and low temperature2The solubility in the aqueous solution is tested, the anaerobic condition in the whole testing process can be well realized, the influence of oxygen on the solubility testing result of the ferrous carbonate is avoided, and the accurate solubility testing result is obtained;
(2) the invention can well monitor the deposition and dissolution kinetic processes of the ferrous carbonate in the solution in real time, and provides very important basis for the accurate test of the solubility of the ferrous carbonate.
Drawings
FIG. 1 is a schematic view of the structure of the apparatus of the present invention.
Detailed Description
As shown in the attached drawings, the device provided by the invention mainly comprises: the device comprises a vacuum pump 1, a first valve 2, a first precision valve 3, a second valve 4, a pressure gauge 5, a thermometer 6, a second precision valve 7, a pipette 8, a third valve 9, a fourth valve 10, a liquid taking pipe 11, a fifth valve 12, a top cover 13, a gas collecting bottle 14, a reaction cylinder 15, a micro-CT probe 16, a stirring rod 17, a magnetic stirrer 18, a thermostat 19, a side cover 20, a side bolt 21, a glass window 22, a top bolt 23, a first pipeline 24, a second pipeline 25, a third pipeline 26 and a fourth pipeline 27. Wherein the vacuum pump 1 is used for pumping the whole test system and forming a certain negative pressure, the third pipeline 26 and the first precision valve 3 are used for injecting specified CO into the reaction cylinder 15, the first pipeline 24, the second pipeline 25 and the fourth pipeline 272Gas, suction of vacuum pump 1 and CO2The air of the whole test system can be well exhausted by the injection of the test system; the first pipeline 24 is used for communicating the pipette 8, the fourth pipeline 27 and the vacuum pump 1, and the second pipeline 25 is used for communicating the liquid taking pipe 11 and the reaction cylinder 15; the first valve 2, the second valve 4, the third valve 9, the fourth valve 10 and the fifth valve 12 are used for controlling the flow direction of fluid in all pipelines, and the second precision valve 7 and the liquid taking pipe 11 are used for accurately sampling from the reaction cylinder 15; the reaction cylinder 15 for dissolving ferrous carbonate consists of a top cover 13 and a top partThe temperature gauge comprises a bolt 23, a side cover 20, a side bolt 21, a glass window 22, a thermometer 6, a pressure gauge 5 and a sealing ring; the magnetic stirrer 18 and the stirring rod 17 are used for stirring the solution to accelerate the full dissolution of the ferrous carbonate; the micro CT probe 16 on the glass window 22 is used to monitor the deposition and dissolution kinetics of ferrous carbonate; a thermostat 19 heated by water bath is used for controlling the temperature of the reaction cylinder 15; the gas collection bottle 14 is used for collecting gas discharged in the process of deoxygenating the pipette 8; a thermometer 6 and a pressure gauge 5 are used for displaying the temperature and CO in the ferrous carbonate solubility test process2Partial pressure.
The glass window 22 is fixed on the reaction cylinder 15 through the side cover 20, the side bolt 21 and the sealing ring;
after the oxygen is removed, the pipette 8 pumps the reaction cylinder 15 by using the vacuum pump 1 to form negative pressure, and then CO in the second pipeline 25 is discharged2The liquid in the pipette 8 is injected into the reaction cylinder 15 in a negative pressure state by pressure.
After the ferrous carbonate dissolution and deposition reach the dynamic equilibrium each time, the liquid taking pipe 11, the second precision valve 7 and the second pipeline 25 of the invention pass through CO in the reaction cylinder 152The ferrous carbonate solution in the reaction cylinder 15 is taken out under the action of pressure.
In order to make the objects, technical solutions and advantages of the present invention more clear, the following description of the embodiments of the present invention with reference to fig. 1 shows the following detailed steps:
the method comprises the following steps: the whole test system is subjected to pressure test, and the test pressure is higher than FeCO3CO required for solubility test2Partial pressure, ensuring CO in the test process2The partial pressure is kept constant all the time;
step two: adding excessive high-purity ferrous carbonate powder into a reaction cylinder 15 which is sequentially cleaned by petroleum ether, acetone and methanol, firmly sealing the reaction cylinder 15 by a top cover 13, a top bolt 23 and a sealing ring, and simultaneously injecting required test solution, such as deionized water, artificial seawater and the like, into a pipette 8;
step three: the second valve 4, the second precision valve 7 and the fifth valve 12 are closed, the first valve 2 and the first precision valve 3 are opened, and firstlyThe whole test system is pumped by the vacuum pump 1 to form a negative pressure and maintained for 10 minutes, then the first valve 2 is closed, and CO with a certain pressure is injected into the test system through the third pipeline 262Releasing the negative pressure, and completely deoxidizing after repeating the process for three times;
step four: closing the first valve 2, the first precision valve 3 and the fifth valve 12, opening the second valve 4, the third valve 9 and the fourth valve 10 and introducing low-pressure CO into the pipette 82Driving off dissolved oxygen in the solution for 30 minutes;
step five: closing the second valve 4, the second precision valve 7, the third valve 9, the fourth valve 10 and the fifth valve 12, opening the first valve 2 and the first precision valve 3, sucking the reaction cylinder 15 by the vacuum pump 1 and forming negative pressure, closing the first valve 2 and the first precision valve 3, opening the second valve 4 and the fifth valve 12, and simultaneously injecting CO into the pipette 82Gas, which ensures that the test solution in the pipette 8 smoothly enters the reaction cylinder 15 in a vacuum state through the first pipeline 24;
step six: starting the magnetic stirrer 18 and the stirring rod 17, opening the first precision valve 3, closing all other valves, and injecting CO required by the experiment into the reaction cylinder 152Partial pressure;
step seven: when CO is present2When the partial pressure reaches a preset value, closing all valves, increasing and controlling the temperature of the reaction cylinder by adopting a constant temperature box 19, unloading the pressure increased due to the temperature increase by adopting a first precision valve 3 when the temperature reaches the preset value, opening a micro CT probe 16, and monitoring the deposition and dissolution kinetic processes of the ferrous carbonate;
step eight: after three days, the magnetic stirrer 18 was stopped and the micro CT probe 16 was observed until FeCO suspended in the solution3Until the particles are completely deposited, generally 24 hours are needed, then a first sampling is started by adopting a second pipeline 25, a second precision valve 7 and a liquid taking pipe 11, and 1-2 ml of FeCO is taken3Diluting the solution, and then performing spectrophotometry (more suitable for FeCO)3Test for lower solubility) and complex titration (more suitable for FeCO)3Test for higher solubility) to comprehensively determine FeCO of the sampling solution3Solubility;
step nine: after the first sampling is finished, the magnetic stirrer 17 is restarted, the second, third, fourth and Nth sampling is carried out by adopting the method used in the step seven after every other day, and the FeCO of the solution sampled every time is comprehensively determined by adopting a spectrophotometry and a complexometric titration method3Solubility until FeCO in reaction cylinder 153At experimental temperature and CO2Reach the dynamic equilibrium of deposition and dissolution under partial pressure, namely FeCO of the solution sampled for the last two times3Until the solubility is equal.

Claims (2)

1. FeCO3High CO content at medium and low temperature2The testing arrangement of solubility in aqueous solution, its characterized in that, the device mainly includes: the device comprises a vacuum pump (1), a first valve (2), a first precision valve (3), a second valve (4), a second precision valve (7), a pipette (8), a third valve (9), a fourth valve (10), a liquid taking pipe (11), a fifth valve (12), a gas collecting bottle (14), a reaction cylinder (15), a micro CT probe (16), a stirring rod (17), a magnetic stirrer (18), a constant temperature box (19), a first pipeline (24), a second pipeline (25), a third pipeline (26) and a fourth pipeline (27); wherein, the vacuum pump (1) is used for pumping the whole test system and forming a certain negative pressure, the third pipeline (26) and the first precision valve (3) are used for injecting specified CO into the reaction cylinder (15), the first pipeline (24), the second pipeline (25) and the fourth pipeline (27)2A gas; the first pipeline (24) is used for communicating the pipette (8), the fourth pipeline (27) and the vacuum pump (1), and the second pipeline (25) is used for communicating the liquid taking pipe (11) and the reaction cylinder (15); the first valve (2), the second valve (4), the third valve (9), the fourth valve (10) and the fifth valve (12) are used for controlling the flow direction of fluid in all pipelines, and the second precision valve (7) and the liquid taking pipe (11) are used for accurately sampling from the reaction cylinder (15); for dissolving FeCO3The reaction cylinder (15) consists of a top cover (13), a top bolt (23), a side cover (20), a side bolt (21), a glass window (22), a thermometer (6), a pressure gauge (5) and a sealing ring, wherein the top cover (13) is fixed on the reaction cylinder (15) through the top bolt (23) and the sealing ring, and the glass window (22) is fixed on the reaction cylinder (15) through the side cover (20), the side bolt (21) and the sealing ring; magnetic stirrer (18) and stirring rod(17) For stirring solution and accelerating FeCO3Fully dissolving; a micro CT probe (16) on a glass window (22) is used to monitor FeCO3Deposition and dissolution kinetics of; the constant temperature box (19) is used for controlling the temperature of the reaction cylinder (15); the gas collection bottle (14) is used for collecting gas discharged in the process of deoxygenation of the pipette (8); the thermometer (6) and the pressure gauge (5) are used for displaying FeCO3Temperature and CO during solubility test2Partial pressure.
2. FeCO3High CO content at medium and low temperature2Method for measuring solubility in aqueous solution by using FeCO according to claim 13High CO content at medium and low temperature2The testing arrangement of solubility in aqueous solution, its characterized in that: the method comprises the following steps: the whole test system is subjected to pressure test, and CO in the test process is ensured2The partial pressure is kept constant all the time; step two: adding excessive high-purity FeCO into a reaction cylinder (15) which is washed by petroleum ether, acetone and methanol in sequence3Powder, a top cover (13), a top bolt (23) and a sealing ring are used for firmly closing the reaction cylinder (15), and meanwhile, required test solution is injected into the pipette (8); step three: closing the second valve (4), the second precision valve (7) and the fifth valve (12), opening the first valve (2) and the first precision valve (3), firstly pumping the test system by using a vacuum pump (1) to form negative pressure and maintaining the negative pressure for 10 minutes, then closing the first valve (2), and injecting CO with certain pressure into the test system through a third pipeline (26)2Releasing the negative pressure, and completely deoxidizing after repeating the process for three times; step four: closing the first valve (2), the first precision valve (3) and the fifth valve (12), opening the second valve (4), the third valve (9) and the fourth valve (10) and introducing low-pressure CO into the pipette (8)2Driving off dissolved oxygen in the aqueous solution for 30 minutes; step five: closing the second valve (4), the second precision valve (7), the third valve (9), the fourth valve (10) and the fifth valve (12), opening the first valve (2) and the first precision valve (3), sucking the reaction cylinder (15) by the vacuum pump (1) and forming negative pressure, closing the first valve (2) and the first precision valve (3) and opening the second valve (4) and the fifth valve (12), and simultaneously injecting CO into the pipette 82Gas, doesThe test solution in the pipette (8) is smoothly fed into the reaction cylinder (15) in a vacuum state through the first pipeline (24); step six: starting the magnetic stirrer (18) and the stirring rod (17), opening the first precision valve (3), closing all other valves, and injecting CO required by the experiment into the reaction cylinder (15)2Partial pressure; step seven: when CO is present2When the partial pressure reaches a preset value, closing all valves, increasing the temperature of the reaction cylinder, unloading the pressure increased due to the temperature increase by adopting a first precise valve (3) when the temperature reaches the preset value, opening a micro CT probe (16) and monitoring the deposition and dissolution kinetic processes of the ferrous carbonate; step eight: after three days, the magnetic stirrer (18) was stopped and the micro CT probe (16) was observed until FeCO suspended in the solution3Until the particles are completely deposited, sampling for the first time by adopting a second pipeline (25), a second precision valve (7) and a liquid taking pipe (11), and taking 1-2 ml of FeCO3After the solution is diluted, the FeCO of the sampling solution is comprehensively determined by adopting a spectrophotometry method and a complexometric titration method3Solubility; step nine: after the first sampling is finished, the magnetic stirrer (18) is restarted, the second, third, fourth and Nth sampling is carried out by adopting the method used in the step eight after every other day, and the FeCO of the solution sampled every time is comprehensively determined by adopting a spectrophotometry method and a complexometric titration method3Solubility until FeCO in the reaction cylinder (15)3At experimental temperature and CO2Reach the dynamic equilibrium of deposition and dissolution under partial pressure, namely FeCO of the solution sampled for the last two times3Until the solubility is equal.
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