CN113049763A - Experimental testing device and testing method for salt precipitation concentration of high-temperature high-pressure real formation water - Google Patents
Experimental testing device and testing method for salt precipitation concentration of high-temperature high-pressure real formation water Download PDFInfo
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- 239000008398 formation water Substances 0.000 title claims abstract description 115
- 150000003839 salts Chemical class 0.000 title claims abstract description 52
- 238000012360 testing method Methods 0.000 title claims abstract description 52
- 238000001556 precipitation Methods 0.000 title claims description 12
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 147
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 92
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 72
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 72
- 239000008367 deionised water Substances 0.000 claims abstract description 44
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 44
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 37
- 238000000034 method Methods 0.000 claims abstract description 37
- 239000011780 sodium chloride Substances 0.000 claims abstract description 37
- 229920001971 elastomer Polymers 0.000 claims abstract description 27
- 239000007789 gas Substances 0.000 claims abstract description 24
- 238000010438 heat treatment Methods 0.000 claims abstract description 18
- 239000002245 particle Substances 0.000 claims abstract description 17
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims abstract description 14
- 238000002474 experimental method Methods 0.000 claims abstract description 13
- 239000007787 solid Substances 0.000 claims abstract description 13
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000009938 salting Methods 0.000 claims abstract description 3
- 229910017053 inorganic salt Inorganic materials 0.000 claims description 53
- 238000004364 calculation method Methods 0.000 claims description 20
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 13
- 229910052799 carbon Inorganic materials 0.000 claims description 13
- 150000002500 ions Chemical class 0.000 claims description 12
- 239000012266 salt solution Substances 0.000 claims description 10
- 230000018044 dehydration Effects 0.000 claims description 7
- 238000006297 dehydration reaction Methods 0.000 claims description 7
- 238000010998 test method Methods 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 6
- 229920002545 silicone oil Polymers 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000013078 crystal Substances 0.000 claims description 5
- 239000003921 oil Substances 0.000 claims description 5
- 229910052710 silicon Inorganic materials 0.000 claims description 5
- 239000010703 silicon Substances 0.000 claims description 5
- 239000011148 porous material Substances 0.000 claims description 4
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000004458 analytical method Methods 0.000 claims description 2
- 238000005185 salting out Methods 0.000 abstract description 8
- 230000003139 buffering effect Effects 0.000 abstract description 4
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 4
- 238000011217 control strategy Methods 0.000 abstract description 3
- 229910000831 Steel Inorganic materials 0.000 abstract description 2
- 239000010959 steel Substances 0.000 abstract description 2
- 230000002265 prevention Effects 0.000 abstract 1
- 230000009919 sequestration Effects 0.000 description 12
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- 238000006467 substitution reaction Methods 0.000 description 2
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- 150000001450 anions Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
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- 230000003111 delayed effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
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- 230000002349 favourable effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
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- 238000002347 injection Methods 0.000 description 1
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- 238000004255 ion exchange chromatography Methods 0.000 description 1
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- 230000007935 neutral effect Effects 0.000 description 1
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Abstract
The invention provides a high-temperature high-pressure real formation water salting concentration experiment testing device which comprises three constant-pressure constant-speed pumps, five pressure gauges, five stop valves, deionized water, three intermediate containers, an observation container, a self-heating insulating layer, an explosion-proof steel sleeve, a temperature sensor, a solid particle feeder, a nitrogen bottle, three four-way valves, a vacuum pump, a vacuum pressure gauge, two pressure limiting valves, a gas pressure buffer, two measuring cylinders with rubber plugs, triethylene glycol, anhydrous calcium chloride, two electronic balances, a camera, an air compressor, a gas buffering storage tank, a thermostat and a constant-temperature heating system. The method can realize the testing of the concentration of the formation water salting-out salt in the process of burying the carbon dioxide in the underground saline water layer, and obtain reliable and accurate experimental results, which can provide basic data for making a control strategy for the formation water salting-out prevention in the process of burying the carbon dioxide in the underground saline water layer, thereby delaying the formation water salting-out time, reducing the damage degree of the salting-out salt and reducing the cost investment of burying the carbon dioxide.
Description
Technical Field
The invention belongs to the technical field of geological carbon dioxide sequestration, and particularly relates to a device and a method for testing the salt evolution concentration of formation water in the process of sequestration of carbon dioxide in an underground saline water layer.
Background
Carbon dioxide is one of the major gases generating the greenhouse effect, and the global warming problem caused by carbon dioxide is receiving wide attention from countries around the world. According to the latest Chinese carbon dioxide emission reduction plan: china strives for carbon emission to reach a peak value 2030 years ago, and strives for carbon neutralization 2060 years ago. As is well known, carbon dioxide capture and geological sequestration are currently one of the most direct and effective means of reducing atmospheric carbon dioxide concentration globally acknowledged. Because of the wide distribution of underground saline water layers and the great potential for carbon dioxide sequestration, underground saline water layers have been recognized as the best geological carbon dioxide sequestration site. However, during the injection of carbon dioxide into the saline water layer, the strong steam concentration effect of the dry carbon dioxide on the formation water causes the formation water in the saline water layer to generate salt separation phenomenon due to supersaturation. Along with the increase of salt crystal particles separated out from the formation water, the pore space of the underground saline water layer is gradually blocked by the salt crystal particles, so that the air suction capacity of the underground saline water layer is reduced, the carbon dioxide sequestration potential of the underground saline water layer is reduced, and the economic cost of a carbon dioxide sequestration project is increased. Therefore, before the carbon dioxide sequestration project is developed, the salt-separating concentration of the formation water in the underground saline water layer at different stages needs to be determined, so that a measure for preventing and controlling the salt-separating of the formation water is formulated, the salt-separating time of the formation water is delayed, and the damage degree of the salt-separating is reduced.
At present, the method for researching the salt separating concentration of soluble inorganic salt in water mainly comprises three types of experimental test, theoretical calculation and computer simulation. Wherein, the experimental test is the most common and accurate technical means at present; the theoretical calculation is based on the water-salt system phase equilibrium theory, and has higher calculation precision on the salt separation concentration of the less than 4-element inorganic salt ion aqueous solution; the computer simulation is to simulate the structure and behavior of molecules through an atomic-level molecular model so as to obtain the physical properties of a water-inorganic salt system, the calculation process is complex, and the calculation result depends on experimental test result verification.
For real formation water of an underground saline water layer, multiple inorganic salts exist, the composition of inorganic salt ions in the water is complex, and the problems of mutual synergy and mutual restriction exist among different inorganic salt ions. Therefore, the method for predicting the salt separation concentration of the formation water in the process of burying and storing the carbon dioxide in the underground saline water layer by adopting theoretical calculation and computer simulation has the problems of complex calculation process, high difficulty, poor reliability of prediction results and the like. Therefore, obtaining accurate real formation water salinity can only be tested experimentally. In the existing experimental test methods (solute method, solvent method and crystallization method), the water-inorganic salt solution system is saturated by changing conditions, so that the salt precipitation concentration of the water-inorganic salt solution is obtained, wherein the solute method is to increase the mass of the solute by fixing the mass of the solvent; the solvent method increases the mass of solute by fixing the mass of solvent; the crystallization method is to change the temperature and pressure conditions of a water-inorganic salt solution system by fixing the mass of solute and solvent. For simple and single water-inorganic salt solution, higher-precision experimental results can be obtained by adopting a solute method and a solvent method. Crystallization cannot be used to determine the salt evolution concentration of a saline aquifer under specific temperature and pressure conditions (formation water temperature, pressure). Therefore, the existing experimental measurement method is not suitable for testing the salt separation concentration of the formation water in the process of burying the carbon dioxide in the underground saline water layer. In view of this, it is desirable to design and establish a device and a method for testing the salt evolution concentration of high-temperature high-pressure real formation water, and combine the indoor experimental test result of the inorganic salt ion composition of the formation water in the underground saline water layer to obtain the accurate salt evolution concentration of the formation water through the indoor experimental test, thereby providing a basis for formulating a technical countermeasure for preventing and controlling the salt evolution of the formation water.
Disclosure of Invention
In view of the above problems, an object of the present invention is to provide a device and a method for testing salt evolution concentration of real formation water at high temperature and high pressure, which are used for testing the salt evolution concentration of formation water at different stages of carbon dioxide sequestration in an underground saline water layer according to the indoor experimental test result of inorganic salt ion composition of the formation water in the underground saline water layer, and establishing a salt evolution concentration chart of the formation water during carbon dioxide sequestration in the underground saline water layer.
The invention provides a device for testing a salt evolution concentration experiment of high-temperature high-pressure real formation water, which comprises a first four-way valve, wherein a valve a of the first four-way valve is communicated with a first intermediate container through a pipeline, deionized water and silicone oil which are separated by a first piston are filled in the first intermediate container, the first intermediate container is communicated with a first constant-speed constant-pressure pump through a pipeline, a first stop valve and a first pressure gauge are connected between the first constant-speed constant-pressure pump and the first intermediate container, and a valve d of the first four-way valve is communicated with a valve b of a second four-way valve through a pipeline;
a valve a of the second four-way valve is communicated with a first pressure limiting valve through a pipeline, the first pressure limiting valve is communicated with a second intermediate container through a pipeline, carbon dioxide and silicon oil which are separated through a second piston are filled in the second intermediate container, the second intermediate container is communicated with a second constant-speed constant-pressure pump through a pipeline, and a second stop valve and a second pressure gauge are connected between the second constant-speed constant-pressure pump and the second intermediate container; the valve c of the second four-way valve is used for pressure relief, and the valve d of the second four-way valve is communicated with the valve b of the third four-way valve through a pipeline;
the valve a of the third four-way valve is communicated with an observation container through a pipeline, a self-heating heat-insulating layer is wrapped outside the observation container, a round platform piston is arranged in the observation container, silicone oil is arranged below the round platform piston, a solid particle feeder is arranged on the observation container, the observation container is communicated with a third constant-speed constant-pressure pump through a pipeline, a third stop valve and a third pressure gauge are connected between the third constant-speed constant-pressure pump and the observation container, a valve d of the third four-way valve is communicated with a fourth pressure gauge through a pipeline, a valve c of the third four-way valve is communicated with a second pressure limiting valve through a pipeline, the second pressure limiting valve is communicated with a gas pressure buffer through a pipeline, the gas pressure buffer is communicated with a first rubber plug-carrying measuring cylinder arranged on a first electronic balance through a pipeline, triethylene glycol is arranged in the first rubber plug measuring cylinder, the first rubber plug measuring cylinder is communicated with a second rubber plug measuring cylinder arranged on the second electronic balance through, anhydrous calcium chloride is filled in the second measuring cylinder with the rubber plug; a camera for observing the inside of the observation container is arranged on one side of the observation container.
Preferably, the second measuring cylinder with the rubber plug is communicated with a gas buffering storage tank through a pipeline, the gas buffering storage tank is communicated with a third intermediate container through a pipeline, and a fourth stop valve, a fifth pressure gauge, an air compressor and a fifth stop valve are sequentially connected between the third intermediate container and the gas buffering storage tank.
Preferably, the valve b of the first four-way valve is communicated with a nitrogen gas cylinder through a pipeline, the valve c of the first four-way valve is communicated with a vacuum pump through a pipeline, and a vacuum pressure gauge is connected between the valve c of the first four-way valve and the vacuum pump.
Preferably, the first intermediate container, the second intermediate container and the observation container are all placed in an incubator, and a constant-temperature heating system is further installed in the incubator.
Preferably, the camera is mounted on a linear slide that slides up and down the linear slide to determine the relative position of the fluid inside the vessel for viewing.
The test method of the salt-separating concentration experiment test device utilizing the high-temperature high-pressure real formation water comprises the following steps:
step S1, connecting a salt-separating concentration experiment testing device of high-temperature high-pressure real formation water, transferring deionized water from the first intermediate container to the observation container, observing the height between the liquid level of the deionized water in the container and the top surface of the piston of the circular truncated cone through a camera, calculating the volume of the deionized water, and calculating the mass of the deionized water according to the volume and the temperature of the deionized water;
step S2, adding corresponding inorganic salt into an observation container through a solid particle feeder and stirring to fully dissolve the inorganic salt in deionized water; observing a water-inorganic salt solution system in the container through a camera, adjusting the temperature of the constant-temperature heating system and the self-heating insulating layer to the temperature of the underground saline water layer when solid particles cannot be observed, maintaining the pressure of the formation water at the pressure of the underground saline water layer by utilizing a constant-pressure pump-in mode of a third constant-speed constant-pressure pump, and standing for a preset time at constant temperature and constant pressure to obtain an experimental sample representing the real formation water of the underground saline water layer;
s3, setting the pressure of the first pressure limiting valve as the pressure of the underground salt water layer, injecting carbon dioxide in a second intermediate container into an observation container by using a second constant-speed constant-pressure pump, maintaining the pressure of the carbon dioxide-formation water system unchanged by using a constant-pressure pump withdrawing mode of a third constant-speed constant-pressure pump, stopping injecting the carbon dioxide when the total volume of the carbon dioxide-formation water system reaches 80-90% of the effective volume of the observation container, and closing an opened valve; then, the carbon dioxide-formation water system in the observation container is accelerated to reach phase state balance through stirring, so that part of formation water is evaporated into the carbon dioxide, and part of the carbon dioxide is dissolved into the formation water;
step S4, setting the pressure of a second pressure limiting valve as the pressure of the underground salt water layer, discharging and driving out carbon dioxide in the observation container at constant pressure by using a third constant-speed constant-pressure pump, dehydrating and drying the discharged carbon dioxide by using triethylene glycol in a first rubber plug-containing measuring cylinder and anhydrous calcium chloride in a second rubber plug-containing measuring cylinder, and metering the dehydration mass of the triethylene glycol to the carbon dioxide by using a first electronic balance and the dehydration mass of the anhydrous calcium chloride to the carbon dioxide by using a second electronic balance;
and S5, repeating the step S3 and the step S4 until the formation water in the observation container is observed to have crystal particles of inorganic salt through the camera, and calculating the salt precipitation concentration of the real formation water under the current pressure condition.
Preferably, the deionized water volume calculation formula is:
Vw＝Vc+π×rin 2×Hw
wherein, VwTo observe the volume of deionized water in the vessel, VcIs the pore volume r between the truncated cone piston and the observation containerinTo observe the inner radius of the vessel, HwThe height from the liquid level of the deionized water in the container to the top surface of the circular truncated cone piston is observed;
the deionized water mass calculation formula is as follows:
mw＝Vwρw
wherein m iswIs the mass of deionized water, pwThe density of the deionized water is calculated by the following formula:
ρw＝3786.31-37.2487(T+273.15)+0.196246(T+273.15)2-5.04708×10-4(T+273.15)3+6.29368×10-7(T+273.15)4-3.08480×10-10(T+273.15)5
wherein T is the temperature of the deionized water in the observation container.
Preferably, the molar concentration of the inorganic salt is determined according to the analysis result of the inorganic salt ions of the target formation water tested by the experiment, the mass of the inorganic salt required by preparing real formation water is calculated according to the molar concentration of the inorganic salt in the formation water, and then the corresponding inorganic salt is added into the observation container through the solid particle feeder;
the mass calculation formula of the inorganic salt is as follows:
wherein m issiThe mass of the i-th inorganic salt,
the i-th inorganic salt molar concentration, MN, in real formation watersiIs the i-th inorganic salt molar mass.
Preferably, the calculation formula of the salt-separating concentration of the real formation water is as follows:
wherein,
m is the salt-separating concentration of real formation water1jIs the mass of triethylene glycol to dehydrate carbon dioxide, m2jIs anhydrous calcium chloride to carbon dioxideThe quality of dewatering.
Preferably, the dried and dehydrated carbon dioxide is stored in the third intermediate container through the air compressor under the condition of pressurization again, so that the carbon dioxide can be reused, carbon dioxide resources are saved, and carbon emission is reduced.
The device and the method for testing the salt evolution concentration of the high-temperature high-pressure real formation water can accurately reflect the physical process of carbon dioxide buried in the underground saline water layer, are suitable for the real formation water of different soluble salt systems, and the precision of the test result of the experiment is not influenced by the complexity of the composition of inorganic salt in the formation water. Therefore, the method effectively realizes the formation water salt-separating concentration test in the process of burying and storing the carbon dioxide in the underground saline water layer, obtains reliable and accurate experimental test results, and provides basic data for making a control strategy for the formation water salt-separating in the process of burying and storing the carbon dioxide in the underground saline water layer. The method is favorable for delaying the salt precipitation time of the formation water in the carbon dioxide sequestration process, reducing the damage degree of the salt precipitation and reducing the carbon dioxide sequestration cost investment. Particularly, the experimental test method and the experimental test device provided by the invention have higher industrial popularization value and are also suitable for determining the salt separation concentration of formation water in the development process of an oil-gas reservoir.
Drawings
Other objects and results of the present invention will become more apparent and more readily appreciated as the same becomes better understood by reference to the following description and appended claims, taken in conjunction with the accompanying drawings. In the drawings:
fig. 1 is a schematic structural diagram of a device for testing the salt evolution concentration of high-temperature high-pressure real formation water according to an embodiment of the invention.
Wherein the reference numerals include: 1-1 part of a first constant-pressure constant-speed pump, 1-2 parts of a second constant-pressure constant-speed pump, 1-3 parts of a third constant-pressure constant-speed pump, 2-1 part of a first pressure gauge, 2-2 parts of a second pressure gauge, 2-3 parts of a third pressure gauge, 2-4 parts of a fourth pressure gauge, 2-5 parts of a fifth pressure gauge, 3-1 part of a first stop valve, 3-2 parts of a second stop valve, 3-3 parts of a third stop valve, 3-4 parts of a fourth stop valve, 3-5 parts of a fifth stop valve, 4 parts of silicone oil, 5-1 parts of a first piston, 5-2 parts of a second piston, 5-3 parts of a third piston, 6 parts of deionized water, 7-1 part of a first intermediate container, 7-2 parts of a second intermediate container, 8 parts of carbon dioxide, 9 parts of a circular table piston, 10 parts of an observation container, the device comprises a nitrogen cylinder 15, a first four-way valve 16-1, a second four-way valve 16-2, a third four-way valve 16-3, a vacuum pump 17, a vacuum pressure gauge 18, a first pressure limiting valve 19-1, a second pressure limiting valve 19-2, a gas pressure buffer 20, a first rubber plug-containing measuring cylinder 21-1, a second rubber plug-containing measuring cylinder 21-2, triethylene glycol 22, anhydrous calcium chloride 23, a first electronic balance 24-1, a second electronic balance 24-2, a linear slide rail 25, a camera 26, an air compressor 27, a gas buffer storage tank 28, a thermostat 29 and a constant temperature heating system 30.
The same reference numbers in all figures indicate similar or corresponding features or functions.
Detailed Description
Specific embodiments of the present invention will be described in detail below with reference to the accompanying drawings.
Fig. 1 shows the structure of a salt evolution concentration experimental test device for high-temperature high-pressure real formation water according to an embodiment of the invention.
As shown in fig. 1, the device for testing the salt precipitation concentration of the high-temperature high-pressure real formation water according to the embodiment of the present invention includes: the device comprises a first four-way valve 16-1, wherein a valve a of the first four-way valve 16-1 is communicated with a first intermediate container 7-1 through a pipeline, deionized water 6 and silicon oil 4 which are separated through a first piston 5-1 are filled in the first intermediate container 7-1, the first intermediate container 7-1 is communicated with a first constant-speed constant-pressure pump 1-1 through a pipeline, a first stop valve 3-1 and a first pressure gauge 2-1 are connected between the first constant-speed constant-pressure pump 1-1 and the first intermediate container 7-1, and a valve d of the first four-way valve 16-1 is communicated with a valve b of a second four-way valve 16-2 through a pipeline.
A valve a of the second four-way valve 16-2 is communicated with a first pressure limiting valve 19-1 through a pipeline, the first pressure limiting valve 19-1 is communicated with a second intermediate container 7-2 through a pipeline, carbon dioxide 8 and silicone oil 4 which are separated through a second piston 5-2 are filled in the second intermediate container 7-2, the second intermediate container 7-2 is communicated with a second constant-speed constant-pressure pump 1-2 through a pipeline, and a second stop valve 3-2 and a second pressure gauge 2-2 are connected between the second constant-speed constant-pressure pump 1-2 and the second intermediate container 7-2; the c valve of the second four-way valve 16-2 is used for pressure relief, and the d valve of the second four-way valve 16-2 is communicated with the b valve of the third four-way valve 16-3 through a pipeline.
A valve a of a third four-way valve 16-3 is communicated with an observation container 10 through a pipeline, a self-heating heat preservation layer 11 is wrapped outside the observation container 10, an explosion-proof steel sleeve 12 is sleeved outside the self-heating heat preservation layer 11, a circular table piston 9 is arranged in the observation container 10, silicon oil 4 is arranged below the circular table piston 9, a temperature sensor 13 and a solid particle feeder 14 are arranged on the observation container 10, the temperature sensor 13 is used for monitoring the temperature in the observation container 10 in real time, the observation container 10 is communicated with a third constant-speed constant-pressure pump 1-1 through a pipeline, a third stop valve 3-3 and a third pressure meter 2-3 are connected between the third constant-speed constant-pressure pump 1-1 and the observation container 10, a valve d of the third four-way valve 16-3 is communicated with a fourth pressure meter 2-4 through a pipeline, a valve c of the third four-way valve 16-3 is communicated with a second pressure limiting valve 19-, the second pressure limiting valve 19-2 is communicated with a gas pressure buffer 20 through a pipeline, the gas pressure buffer 20 is communicated with a first rubber plug-carrying measuring cylinder 21-1 arranged on a first electronic balance 24-1 through a pipeline, triethylene glycol 22 is arranged in the first rubber plug-carrying measuring cylinder 21-1, the first rubber plug-carrying measuring cylinder 21-1 is communicated with a second rubber plug-carrying measuring cylinder 21-2 arranged on a second electronic balance 24-2 through a pipeline, and anhydrous calcium chloride 23 is arranged in the second rubber plug-carrying measuring cylinder 21-2; a camera 26 for observing the inside of the observation vessel 10 is provided at one side of the observation vessel 10.
In a specific embodiment of the invention, the second graduated cylinder with a rubber plug 21-2 is communicated with a gas buffer storage tank 28 through a pipeline, the gas buffer storage tank 28 is communicated with a third intermediate container 8-3 through a pipeline, a third piston 5-3 is arranged in the third intermediate container 8-3, silicon oil 4 is arranged below the third piston 5-3, and a fourth stop valve 3-4, a fifth pressure gauge 2-5, an air compressor 27 and a fifth stop valve 3-5 are sequentially connected between the third intermediate container 8-3 and the gas buffer storage tank 28.
In another embodiment of the present invention, the valve b of the first four-way valve 16-1 is connected to the nitrogen gas tank 15 through a pipeline, the valve c of the first four-way valve 16-1 is connected to the vacuum pump 17 through a pipeline, and a vacuum pressure gauge 18 is connected between the valve c of the first four-way valve 16-1 and the vacuum pump 17.
In one example of the present invention, the first intermediate container 7-1, the second intermediate container 7-2, and the observation container 10 are all placed in an oven 29, and a constant temperature heating system 30 is further installed in the oven 29.
In another example of the present invention, the camera 26 is mounted on the linear slide 25, sliding up and down along the linear slide 25.
It should be noted that the pipeline connected between the equipments is a stainless steel pipeline with a diameter of 3 mm.
The above details describe the structure of the salt precipitation concentration experimental test device for high-temperature high-pressure real formation water provided by the present invention, and the present invention further provides a test method using the salt precipitation concentration experimental test device for high-temperature high-pressure real formation water, which specifically includes the following steps:
step S1, connecting a salt precipitation concentration experiment testing device of high-temperature high-pressure real formation water according to the graph 1, opening a valve a of a first four-way valve 16-1, transferring deionized water 6 from a first intermediate container 7-1 to an observation container 10, then closing the valve a of the first four-way valve 16-1, observing the height from the liquid level of the deionized water in the container 10 to the top surface of a circular truncated cone piston 9 through a camera 26, calculating the volume of the deionized water, and calculating the mass of the deionized water according to the volume and the temperature of the deionized water.
The deionized water volume calculation formula is:
Vw＝Vc+π×rin 2×Hw
wherein, VwTo observe the volume of deionized water in vessel 10, units mL, VcThe pore volume between the truncated cone piston 9 and the observation container 10 is expressed in unit mL, and the example value is 1.25mL, rinTo observe the inner radius of the vessel 10, in cm, the example values are 1cm, HwIn order to observe the height between the liquid level of the deionized water in the container 10 and the top surface of the circular truncated cone piston 9, the height is measured in cm.
The deionized water mass calculation formula is as follows:
mw＝Vwρw
wherein m iswIs the mass of deionized water, unit g, rhowIs the density of deionized water and has unit g/cm3The calculation formula is as follows:
ρw＝3786.31-37.2487(T+273.15)+0.196246(T+273.15)2-5.04708×10-4(T+273.15)3+6.29368×10-7(T+273.15)4-3.08480×10-10(T+273.15)5
t is the temperature of the deionized water in the observation vessel 10 in units of ℃.
Before step S1, the following steps are included: the sealing effect of each node of the whole set of experimental device is checked by nitrogen in the nitrogen bottle 15, and the nodes which do not meet the airtight requirement are reconnected. And finally, starting the constant-temperature heating system 30 and the self-heating heat-insulating layer 11, and preheating the experimental device in the constant-temperature box 29, so that the temperature difference strain of the device in the experimental process is reduced, the service life of the device is prolonged, and the preheating temperature is 50-60 ℃.
Before step S1, the method further includes the following steps: the c and d valves of the four-way valve 16-1, the b and d valves of the four-way valve 16-2 and the a and b valves of the four-way valve 16-3 are opened, the vacuum pump 17 is started to remove excess air, and then the c valve of the four-way valve 16-1 is closed.
Since the bottled carbon dioxide for laboratory use usually contains a slight amount of water vapor, it will corrode the sealing gasket of the intermediate container for containing carbon dioxide in the experiment, and will also affect the accuracy of the test results of the experiment in the present invention, causing non-negligible systematic errors. Therefore, the carbon dioxide used in the experiment of the present invention needs to be decompressed and dried with anhydrous calcium chloride before being transferred to the second intermediate container 7-2 for use. In particular, the purity of the experimental carbon dioxide was 99.99%.
Step S2, adding corresponding inorganic salt into the observation container 10 through the solid particle feeder 14 and stirring to fully dissolve the inorganic salt in the deionized water; observing a water-inorganic salt solution system in the container 10 through the camera 26, adjusting the temperature of the constant-temperature heating system 30 and the self-heating heat-insulating layer 11 to the temperature of the underground saline water layer when solid particles cannot be observed, maintaining the pressure of the formation water at the pressure of the underground saline water layer by using a constant-pressure pump-in mode of the third constant-speed constant-pressure pump 1-3, and standing for 4 hours at constant temperature and constant pressure to obtain an experimental sample representing the real formation water of the underground saline water layer.
Calculating the mass of various inorganic salts required for preparing real formation water according to the molar concentration of the inorganic salts in the formation water, wherein the molar concentration of the inorganic salts in the formation water is determined as follows:
the method comprises the steps of obtaining formation water of a target layer of carbon dioxide buried in an underground saline water layer, filtering insoluble solid impurities in the formation water by using a micro-nano filter, analyzing the type of inorganic salt ions dissolved in the formation water by using an ion chromatography and a chemical titration method, determining the molar concentration of the inorganic salt ions in the formation water, and finally determining the molar concentration of the inorganic salt in the formation water according to the ion mass composition of the inorganic salt ions in the formation water by combining a water-salt solution system charge conservation principle and an inorganic salt dissolution ionization balance principle in water.
According to the charge conservation principle of a water-salt solution system, the water-salt solution system is electrically neutral, and the charge number of each ion satisfies the following conditions:
in the formula: a ispFor p-th anion in formation water
Molar concentration of (a), unit mol/g; bqFor q type cation in formation water
Molar concentration of (3), unit mol/g.
The i-th soluble inorganic salt (B) is based on the principle of equilibrium between dissolution and ionization of inorganic salts in watermAn)iAnd the dissolution ionization in water meets the following conditions:
(BmAn)i＝mBn++nAm-。
the mass calculation formula of the inorganic salt is as follows:
wherein m issiThe mass of the i-th inorganic salt in g,
the molar concentration of the ith inorganic salt in real formation water is unit mol/g, MNsiIs the molar mass of the i-th inorganic salt in g/mol.
S3, setting the pressure of the first pressure limiting valve 19-1 as the pressure of the underground salt water layer, opening the valves a and d of the second four-way valve 16-2 and the valves a and b of the third four-way valve 16-3, injecting the carbon dioxide 8 in the second intermediate container 7-2 into the observation container 10 by using the second constant-speed constant-pressure pump 1-2, maintaining the pressure of the carbon dioxide-formation water system unchanged by using the constant-pressure pump withdrawing mode of the third constant-speed constant-pressure pump 1-3, stopping injecting the carbon dioxide when the total volume of the carbon dioxide-formation water system reaches 80-90% of the effective volume of the observation container 10, and closing the opened valves; the carbon dioxide-formation water system in the observation container 10 is accelerated to reach phase equilibrium by stirring, namely, part of the formation water is evaporated into the carbon dioxide, and part of the carbon dioxide is dissolved into the formation water.
S4, setting the pressure of the second pressure limiting valve 19-2 as the pressure of the underground salt water layer, opening the valves a and c of the third four-way valve 16-3, discharging the carbon dioxide in the observation container 10 at constant pressure by using the third constant-speed constant-pressure pump 1-3, dehydrating and drying the discharged carbon dioxide by using the triethylene glycol 22 in the first measuring cylinder 21-1 with the rubber plug and the anhydrous calcium chloride 23 in the second measuring cylinder 21-2 with the rubber plug, and measuring the dehydration mass m of the triethylene glycol 22 to the carbon dioxide by using the first electronic balance 24-11jAnd the dehydration mass m of the anhydrous calcium chloride 23 to the carbon dioxide is measured by a second electronic balance 24-22j。
And S5, repeating the step S3 and the step S4 until the formation water in the observation container is observed to have crystal particles of inorganic salt through the camera, and calculating the salt precipitation concentration of the real formation water under the current pressure condition.
The calculation formula of the salt-separating concentration of the real formation water is as follows:
wherein,
the salt-separating concentration is the real salt-separating concentration of the formation water, and the unit is mol/kg.
Preferably, the dried and dehydrated carbon dioxide is stored in the third intermediate container 7-3 by the air compressor 27 under the pressure again, which can reduce the discharge amount of carbon dioxide to the air and is beneficial to improving the recycling rate of carbon dioxide.
And changing the formation water maintaining pressure of the underground saline water layer prepared in the step S1, and repeating the steps S3-S5 to obtain the formation water salting concentration of the underground saline water layer buried carbon dioxide at different stages.
The device and the method for testing the salt evolution concentration of the high-temperature high-pressure real formation water can accurately reflect the physical process of carbon dioxide buried in the underground saline water layer, are suitable for real formation water of different systems, and the precision of the test result of the experiment is not influenced by the complexity of inorganic salt composition in the formation water. Therefore, the method can effectively realize the formation water salting-out concentration test in the process of burying and storing the carbon dioxide in the underground saline water layer, obtain reliable and accurate experimental test results, and provide basic data for making a control strategy for the formation water salting-out in the process of burying and storing the carbon dioxide in the underground saline water layer, thereby delaying the formation water salting-out time, reducing the damage degree of salting-out and reducing the cost input of carbon dioxide burying. Particularly, the experimental test method and the experimental test device provided by the invention have higher industrial popularization value, are also suitable for determining the salt separation concentration of formation water in the development process of an oil-gas reservoir, and only need to replace dry carbon dioxide gas with dry hydrocarbon gas.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (10)
1. A device for testing the salting concentration experiment of high-temperature high-pressure real formation water is characterized by comprising a first four-way valve, wherein a valve a of the first four-way valve is communicated with a first intermediate container through a pipeline, deionized water and silicone oil which are separated by a first piston are filled in the first intermediate container, the first intermediate container is communicated with a first constant-speed constant-pressure pump through a pipeline, a first stop valve and a first pressure gauge are connected between the first constant-speed constant-pressure pump and the first intermediate container, and a valve d of the first four-way valve is communicated with a valve b of a second four-way valve through a pipeline;
a valve a of the second four-way valve is communicated with a first pressure limiting valve through a pipeline, the first pressure limiting valve is communicated with a second intermediate container through a pipeline, carbon dioxide and silicon oil which are separated through a second piston are filled in the second intermediate container, the second intermediate container is communicated with a second constant-speed constant-pressure pump through a pipeline, and a second stop valve and a second pressure gauge are connected between the second constant-speed constant-pressure pump and the second intermediate container; the valve c of the second four-way valve is used for pressure relief, and the valve d of the second four-way valve is communicated with the valve b of the third four-way valve through a pipeline;
the valve a of the third four-way valve is communicated with an observation container through a pipeline, a self-heating heat-insulating layer is wrapped outside the observation container, a round platform piston is arranged in the observation container, silicone oil is arranged below the round platform piston, a solid particle feeder is arranged on the observation container, the observation container is communicated with a third constant-speed constant-pressure pump through a pipeline, a third stop valve and a third pressure gauge are connected between the third constant-speed constant-pressure pump and the observation container, a valve d of the third four-way valve is communicated with a fourth pressure gauge through a pipeline, a valve c of the third four-way valve is communicated with a second pressure limiting valve through a pipeline, the second pressure limiting valve is communicated with a gas pressure buffer through a pipeline, the gas pressure buffer is communicated with a first rubber plug-carrying measuring cylinder arranged on a first electronic balance through a pipeline, triethylene glycol is arranged in the first rubber plug measuring cylinder, the first rubber plug measuring cylinder is communicated with a second rubber plug measuring cylinder arranged on the second electronic balance through, anhydrous calcium chloride is filled in the second measuring cylinder with the rubber plug; a camera for observing the inside of the observation container is arranged on one side of the observation container.
2. The experimental testing device for salinity separating concentration of high-temperature high-pressure real formation water according to claim 1, characterized in that the second graduated cylinder with the rubber plug is communicated with a gas buffer storage tank through a pipeline, the gas buffer storage tank is communicated with a third intermediate container through a pipeline, and a fourth stop valve, a fifth pressure gauge, an air compressor and a fifth stop valve are sequentially connected between the third intermediate container and the gas buffer storage tank.
3. The experimental testing device for salinity separating concentration of high-temperature high-pressure real formation water according to claim 1, characterized in that the valve b of the first four-way valve is communicated with a nitrogen gas cylinder through a pipeline, the valve c of the first four-way valve is communicated with a vacuum pump through a pipeline, and a vacuum pressure gauge is connected between the valve c of the first four-way valve and the vacuum pump.
4. The experimental testing device for salinity separating concentration of high-temperature high-pressure real formation water as claimed in claim 1, characterized in that the first intermediate container, the second intermediate container and the observation container are all placed in a thermostat, and a constant temperature heating system is further installed in the thermostat.
5. The experimental testing device for salinity profile of high temperature high pressure real formation water according to claim 1, characterized in that the camera is mounted on the linear slide rail and slides up and down along the linear slide rail.
6. The test method by using the salt evolution concentration experimental test device of the high-temperature high-pressure real formation water according to any one of claims 1 to 5 comprises the following steps:
step S1, connecting a salt-separating concentration experiment testing device of high-temperature high-pressure real formation water, transferring deionized water from the first intermediate container to the observation container, observing the height between the liquid level of the deionized water in the container and the top surface of the piston of the circular truncated cone through a camera, calculating the volume of the deionized water, and calculating the mass of the deionized water according to the volume and the temperature of the deionized water;
step S2, adding corresponding inorganic salt into an observation container through a solid particle feeder and stirring to fully dissolve the inorganic salt in deionized water; observing a water-inorganic salt solution system in the container through a camera, adjusting the temperature of the constant-temperature heating system and the self-heating insulating layer to the temperature of the underground saline water layer when solid particles cannot be observed, maintaining the pressure of the formation water at the pressure of the underground saline water layer by utilizing a constant-pressure pump-in mode of a third constant-speed constant-pressure pump, and standing for a preset time at constant temperature and constant pressure to obtain an experimental sample representing the real formation water of the underground saline water layer;
s3, setting the pressure of the first pressure limiting valve as the pressure of the underground salt water layer, injecting carbon dioxide in a second intermediate container into an observation container by using a second constant-speed constant-pressure pump, maintaining the pressure of the carbon dioxide-formation water system unchanged by using a constant-pressure pump withdrawing mode of a third constant-speed constant-pressure pump, stopping injecting the carbon dioxide when the total volume of the carbon dioxide-formation water system reaches 80-90% of the effective volume of the observation container, and closing an opened valve; then, the carbon dioxide-formation water system in the observation container is accelerated to reach phase state balance through stirring, so that part of formation water is evaporated into the carbon dioxide, and part of the carbon dioxide is dissolved into the formation water;
step S4, setting the pressure of a second pressure limiting valve as the pressure of the underground salt water layer, discharging and driving out carbon dioxide in the observation container at constant pressure by using a third constant-speed constant-pressure pump, dehydrating and drying the discharged carbon dioxide by using triethylene glycol in a first rubber plug-containing measuring cylinder and anhydrous calcium chloride in a second rubber plug-containing measuring cylinder, and metering the dehydration mass of the triethylene glycol to the carbon dioxide by using a first electronic balance and the dehydration mass of the anhydrous calcium chloride to the carbon dioxide by using a second electronic balance;
and S5, repeating the step S3 and the step S4 until the formation water in the observation container is observed to have crystal particles of inorganic salt through the camera, and calculating the salt precipitation concentration of the real formation water under the current pressure condition.
7. The testing method of the experimental device for testing the salt evolution concentration of the high-temperature high-pressure real formation water as claimed in claim 6, wherein the volume calculation formula of the deionized water is as follows:
Vw＝Vc+π×rin 2×Hw
wherein, VwTo observe the volume of deionized water in the vessel, VcIs the pore volume r between the truncated cone piston and the observation containerinTo observe the inner radius of the vessel, HwThe height from the liquid level of the deionized water in the container to the top surface of the circular truncated cone piston is observed;
the deionized water mass calculation formula is as follows:
mw＝Vwρw
wherein m iswIs the mass of deionized water, pwThe density of the deionized water is calculated by the following formula:
ρw＝3786.31-37.2487(T+273.15)+0.196246(T+273.15)2-5.04708×10-4(T+273.15)3+6.29368×10-7(T+273.15)4-3.08480×10-10(T+273.15)5
t is the temperature of the deionized water in the observation vessel.
8. The testing method of the experimental testing device for the salinity separating concentration of the high-temperature high-pressure real formation water according to claim 7, characterized in that the molar concentration of inorganic salt is determined according to the analysis result of inorganic salt ions of target formation water in the experimental test, the mass of the inorganic salt required for preparing the real formation water is calculated according to the molar concentration of the inorganic salt in the formation water, and then the corresponding inorganic salt is added into the observation container through the solid particle feeder;
the mass calculation formula of the inorganic salt is as follows:
wherein m issiThe mass of the i-th inorganic salt,
the i-th inorganic salt molar concentration, MN, in real formation watersiIs the i-th inorganic salt molar mass.
9. The test method of the experimental test device for the salt evolution concentration of the high-temperature high-pressure real formation water as claimed in claim 8, wherein the calculation formula of the salt evolution concentration of the real formation water is as follows:
wherein,
m is the salt-separating concentration of real formation water1jIs the mass of triethylene glycol to dehydrate carbon dioxide, m2jThe dehydration quality of anhydrous calcium chloride to carbon dioxide is shown.
10. The method for testing the salinity-separating concentration experimental test device of the high-temperature high-pressure real formation water as claimed in claim 6, wherein the dried and dehydrated carbon dioxide is stored in the third intermediate container by being pressurized again through an air compressor.
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