CN111595763A - Simulation experiment method for influence of different magnesium ion concentrations on carbonate rock corrosion - Google Patents
Simulation experiment method for influence of different magnesium ion concentrations on carbonate rock corrosion Download PDFInfo
- Publication number
- CN111595763A CN111595763A CN202010337473.6A CN202010337473A CN111595763A CN 111595763 A CN111595763 A CN 111595763A CN 202010337473 A CN202010337473 A CN 202010337473A CN 111595763 A CN111595763 A CN 111595763A
- Authority
- CN
- China
- Prior art keywords
- rock
- polished section
- reaction
- sample
- morphology
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000011435 rock Substances 0.000 title claims abstract description 57
- 229910001425 magnesium ion Inorganic materials 0.000 title claims abstract description 35
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 title claims abstract description 34
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 238000005260 corrosion Methods 0.000 title claims abstract description 28
- 230000007797 corrosion Effects 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 20
- 238000004088 simulation Methods 0.000 title claims abstract description 19
- 229910052500 inorganic mineral Inorganic materials 0.000 claims abstract description 47
- 239000011707 mineral Substances 0.000 claims abstract description 47
- 238000006243 chemical reaction Methods 0.000 claims abstract description 45
- 230000003628 erosive effect Effects 0.000 claims abstract description 43
- 150000002500 ions Chemical class 0.000 claims abstract description 42
- 239000000203 mixture Substances 0.000 claims abstract description 29
- 239000012530 fluid Substances 0.000 claims abstract description 28
- 238000012360 testing method Methods 0.000 claims abstract description 14
- 230000008859 change Effects 0.000 claims abstract description 11
- 238000004140 cleaning Methods 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000005303 weighing Methods 0.000 claims abstract description 8
- 239000011777 magnesium Substances 0.000 claims description 32
- 239000000243 solution Substances 0.000 claims description 29
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 16
- 238000004458 analytical method Methods 0.000 claims description 14
- 238000002441 X-ray diffraction Methods 0.000 claims description 10
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 8
- 239000007832 Na2SO4 Substances 0.000 claims description 8
- 239000011780 sodium chloride Substances 0.000 claims description 8
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 8
- 238000005530 etching Methods 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 7
- 238000002591 computed tomography Methods 0.000 claims description 6
- 239000008398 formation water Substances 0.000 claims description 6
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 6
- 229910001424 calcium ion Inorganic materials 0.000 claims description 5
- 238000004364 calculation method Methods 0.000 claims description 5
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 claims description 5
- 230000035699 permeability Effects 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 5
- 239000001110 calcium chloride Substances 0.000 claims description 4
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 238000005562 fading Methods 0.000 claims description 4
- 238000011160 research Methods 0.000 claims description 4
- 238000010183 spectrum analysis Methods 0.000 claims description 4
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 230000005540 biological transmission Effects 0.000 claims description 3
- 229910001748 carbonate mineral Inorganic materials 0.000 claims description 3
- 238000011835 investigation Methods 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 230000001502 supplementing effect Effects 0.000 claims description 3
- 238000012876 topography Methods 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 239000013078 crystal Substances 0.000 claims description 2
- 238000007654 immersion Methods 0.000 claims description 2
- 125000000896 monocarboxylic acid group Chemical group 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 238000010998 test method Methods 0.000 claims description 2
- 229910021532 Calcite Inorganic materials 0.000 description 26
- 238000002474 experimental method Methods 0.000 description 14
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 13
- 230000000694 effects Effects 0.000 description 8
- 238000004090 dissolution Methods 0.000 description 7
- 230000002401 inhibitory effect Effects 0.000 description 6
- 230000005764 inhibitory process Effects 0.000 description 6
- 239000003112 inhibitor Substances 0.000 description 4
- 230000007246 mechanism Effects 0.000 description 4
- 235000019738 Limestone Nutrition 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 239000006028 limestone Substances 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000010459 dolomite Substances 0.000 description 2
- 229910000514 dolomite Inorganic materials 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000011859 microparticle Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000002829 reductive effect Effects 0.000 description 2
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 238000000089 atomic force micrograph Methods 0.000 description 1
- 239000012267 brine Substances 0.000 description 1
- 239000007853 buffer solution Substances 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000000100 multiple collector inductively coupled plasma mass spectrometry Methods 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 238000000059 patterning Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000007619 statistical method Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 230000009897 systematic effect Effects 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 238000000733 zeta-potential measurement Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N17/00—Investigating resistance of materials to the weather, to corrosion, or to light
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
- G01N15/088—Investigating volume, surface area, size or distribution of pores; Porosimetry
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Immunology (AREA)
- Biochemistry (AREA)
- Pathology (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- Dispersion Chemistry (AREA)
- Environmental & Geological Engineering (AREA)
- Ecology (AREA)
- Biodiversity & Conservation Biology (AREA)
- Environmental Sciences (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
Abstract
The invention discloses a simulation experiment method for influence of different magnesium ion concentrations on carbonate rock corrosion, which comprises the following steps of: 1) testing physical parameters, mineral compositions and micro-morphology of a plurality of parallel sample polished sections; 2) configuring a series of different Mg2+An eroding fluid of ionic concentration; 3) cleaning, drying and weighing the sample polished section; 4) respectively putting each corrosion fluid into a closed system, and respectively immersing the corrosion fluid into a sample polished section to carry out water-rock reaction; 5) after the reaction is finished, cleaning, drying and weighing the sample polished section; then, the physical parameters, mineral composition and micro-morphology of the sample polished section are tested again to compare the change before and after the reaction; 6) calculating the erosion amount and the erosion rate before and after the reaction, and combining the physical parameters, mineral composition and micro-morphology change of the sample polished section before and after the reactionTo determine Mg2+Influence of ion concentration on carbonate rock erosion.
Description
Technical Field
The invention belongs to the field of petroleum exploration, and particularly relates to a simulation experiment method for influences of different magnesium ion concentrations on carbonate rock corrosion.
Background
Carbonate rock has always been the key field of oil and gas exploration at home and abroad, and in recent years, the oil and gas exploration of carbonate rock in China has made an important progress, and a northeast China gas field, a Tarim Tahe-Tanan oil field, a mid-oil gas field in a tower and the like are discovered successively. The carbonate rock has important significance in the aspects of reservoir finding evaluation and target area prediction of a reservoir stratum and has important guiding significance in the aspect of a global climate warming carbon dioxide isolation storage strategy. The research on the carbonate rock buried corrosion mechanism, control factors and favorable conditions is helpful for comprehensively and deeply understanding the scientific problem of the deep sea phase carbonate rock scale reservoir development mechanism.
With respect to Mg2+The effect of ions on carbonate erosion, a series of studies were performed by a number of scholars (Berner, 1967; Weyl, 1967;
1978; buhmann and Dreybrodt, 1987; compton and Brown, 1994; gutjahr et al, 1996; alkattan et al, 2002; arvidson et al, 2006; xu and Higgins, 2011). For example Weyl (1967) and Berner (1967) note that Mg is present at medium-basic pH values2+The presence of ions has a significant inhibitory effect on calcite erosion. Similarly, Compton and Brown (1994) have Mg in them2+Mg was determined in alkaline solutions with ions up to 80mM (pH. apprxeq.8.0-9.0)2+The existence of the ions has inhibition effect on the corrosion rate, and the experimental result shows that the Mg in the solution2+The presence of ions exhibits a strong inhibitory effect on the dissolution of calcite and attributes this inhibitory effect to Mg on the calcite surface2+And Ca2+Competitive absorption.
(1978) It was found experimentally that under mildly alkaline conditions (T ═ 25 ℃; Ca2+Up to 10-5m) with MgCl present in the solution2The concentration is increased, so that the corrosion rate of calcite is obviously reduced, and Mg2+The inhibition of ions is enhanced with the increase of the saturation degree of calcite in the solution, and the reason for the phenomenon is attributed to the surface adsorption of calciteAqueous phase of magnesium ion (Mg)2+< 50mM) according to Langmuir adsorption isotherm. When the concentration of the inhibitor solution components is outside a certain range, the Langmuir-Volmer model predicts that the erosion rate will be independent of the inhibitor concentration. Gledhill and Morse (2006) experiments found Mg2+The ion's inhibition of the rate of erosion of calcite is not significant and the reason for this is attributed to Mg in solution2+The ion concentration exceeds the inhibition height. Gutjahr et al (1996) showed Mg2+The ion has no influence on the rate of dissolution of calcite (Mg)2+Ion ≤ 3x10-4M and omegacalcite0.5). Ruiz-Agudo et al (2009; 2010) noted lower Mg in neutral solution2+Ion concentration (C)Mg2+< 50mM) inhibits calcite dissolution while Mg2+The ion concentration of more than 50mM promotes the erosion of calcite. Gledhill and Morse (2004) investigated the erosion experiments of calcite in brine environment and found that Ca in solution followed the experiment2+Or Mg2+Increase in ion concentration, SO4 2-The inhibition effect on calcite is more obvious. From the above, the influence of magnesium ions on the erosion rate of calcite is controversial, but it is clear that: within a certain inhibitor concentration range, Mg2+The ions act to inhibit the rate of dissolution of calcite, and when the solution has a higher inhibitor concentration, the effect of the magnesium ions on the rate of erosion of calcite is not as pronounced, possibly suggesting that the inhibition is maximized. Arvidson et al (2006) found that Mg in carbonate buffer solutions under conditions far from equilibrium2+Ions (< 5X 10)-5m) has a certain inhibiting effect on the erosion of calcite, but no change in the micro-morphology of the erosion pit is observed by AFM. When Mg2+Ion addition to 0.8X10-3m, a unique etch pit profile was observed in AFM and VSI experiments. Arvidson et al (2006) attribute to Mg that the reduction in calcite erosion rate would result2+Step pinning effect and slow dehydration caused by ion adsorption; variations in etch pit topography may be due to selective patterning pinning and excessive node build-up along obtuse patterned edges. Sabbides and Koutsoukos (199)5) Described therein in Mg2+＝4x10-5M and omegacalciteAt 0.004-0.02, the rate of calcite dissolution is significantly reduced, by about three times. Xu and Higgins (2011) have described that Mg dissolves under near equilibrium conditions2+Ions (< 10)-4m) shows a weak inhibiting effect on the erosion of calcite, in Mg2+Ion concentration of 10-3m is when solution omegacalciteLess than 0.2, Mg2+The ions have little influence on the dissolution of calcite, while ΩcalciteMagnesium ions suddenly play a certain inhibiting role in calcite dissolution when the magnesium ions are more than 0.2.
From this it can be seen that Mg2+The influence of ion concentration on the erosion rate of carbonate rock is also greatly divergent, thus developing Mg2+Experiments on the effect of ion concentration on the erosion rate of carbonate rock are of great necessity.
Disclosure of Invention
Based on the background technology, the invention provides a simulation experiment method for the influence of different magnesium ion concentrations on carbonate rock corrosion. The experiment simulates different Mg under specific temperature, pressure and ionic strength2+Influence of ion concentration on carbonate rock erosion.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a simulation experiment method for influence of different magnesium ion concentrations on carbonate rock corrosion, which comprises the following steps:
1) testing physical parameters, mineral compositions and micro-morphology of a plurality of parallel sample polished sections;
2) formation water configuration of simulated research area a series of different Mg2+An eroding fluid of ionic concentration;
3) cleaning, drying and weighing the sample polished section;
4) respectively placing each corrosion fluid into a closed system, respectively immersing a sample polished section in the closed system, and setting the temperature and the pressure to carry out water-rock reaction;
in the reaction process, the regression rate and the microscopic morphology of the carbonate corrosion step are observed at certain time intervals, and the component analysis is carried out on the reaction solution;
5) after the reaction is finished, cleaning, drying and weighing the sample polished section; then, the physical parameters, mineral composition and micro-morphology of the sample polished section are tested again to compare the change before and after the reaction;
6) calculating the erosion amount and the erosion rate before and after the reaction, and determining Mg by combining the physical parameters, mineral composition and micro-morphology change of the sample polished section before and after the reaction2+Influence of ion concentration on carbonate rock erosion.
According to the invention, Mg can be determined by comparing the micro-morphologies of the minerals before and after the reaction according to the experimental method2+The influence of the presence of ions on carbonate corrosion can be further analyzed by analyzing the chemical composition (Mg) of hydro-hydrocarbons in the reservoir2+Ion concentration) a potential good reservoir zone can be delineated. The invention also can know the corrosion mechanism and microscopic characterization through the change of the mineral micro-morphology and the internal structure.
In a preferred embodiment of the invention, when there is inclusion data for carbonate minerals in the formation of the investigation region, the composition of the simulated inclusions is configured differently for Mg2+An eroding fluid of ionic concentration.
In a preferred embodiment of the invention, the formation water or inclusion in the simulated research area is provided with NaCl, CaCl with corresponding concentration2、MgCl2、Na2SO4And 0.15M CH3The COOH mixed solution is used as an erosion fluid;
wherein, Mg is added according to preset different concentrations2+Adjustment of ion concentration MgCl2While correspondingly adjusting CaCl2To ensure that the ionic strength of the etching fluid is constant.
In a preferred embodiment of the present invention, when the temperature and the pressure are set, the temperature and the pressure are set according to a ground temperature gradient and a pressure gradient as follows: 40 ℃/10MPa, 80 ℃/30MPa, 120 ℃/40MPa or 160 ℃/50 MPa; to investigate Mg under specific temperature and pressure conditions2+Influence of ion concentration on carbonate rock erosion.
Setting the pressure to be 10MPa, 20MPa, 40MPa and 60MPa respectively, and simulating the pressure range from the earth surface to the depth of 6Km of the rock, wherein the pressure gradient of the buried depth is 10 MPa/Km; different depths correspond to different pressures and temperatures.
For example, in the embodiment of the invention, a series of different Mg is arranged under each temperature and pressure condition2+Parallel test of ion concentration to further investigate Mg under different temperature and pressure conditions2+The effect of ion concentration on carbonate rock erosion; the total parallel test quantity is the quantity of different Mg under the condition of temperature and pressure2+Number of ion concentrations.
In a preferred embodiment of the present invention, the process for testing the physical parameters, mineral composition and micro-morphology of the sample polished section comprises:
observing the apparent micro-morphology of the rock polished section and marking a specific area;
determining mineral composition and semi-quantitative chemical components in the rock polished section;
phase identification and quantitative calculation of each mineral component content are carried out on the rock polished section, and the crystallinity, the order degree and the unit cell parameter information of the minerals are calculated;
measuring the surface potential of the rock polished section;
measuring the physical parameters of the porosity and permeability of the rock polished section;
preferably, observing the rock sample light-sheet apparent micro-morphology by using a scanning electron microscope and marking a specific area; observing the rock sample light-sheet apparent micro-morphology by using a Scanning Electron Microscope (SEM) and marking a specific area; determining mineral composition and semi-quantitative chemical composition in a rock sample polished section by using energy spectrum analysis (EDS); performing phase identification and quantitative calculation of each mineral component content by X-ray diffraction (XRD), and calculating information such as crystallinity, order degree and unit cell parameters of the minerals according to diffraction peak data of XRD; measuring the surface potential of the rock sample polished section by using a solid surface Zeta potential analyzer; the rock sample slide was subjected to electron computed tomography (CT scan) to obtain physical parameters including porosity and permeability before and after its reaction.
Because XRD has certain deviation on the content of each mineral component, in a preferred scheme of the invention, the content of each mineral component can be calculated by analyzing main quantity elements and mutually corrected with the content of each mineral component quantitatively calculated by X-ray diffraction (XRD) so as to accurately quantify; for CaO, MgO and SiO in the analysis of main elements2Analysis, when only calcite and dolomite are seen on the rock sample polished section under a polarizing microscope, SiO is not analyzed when the main element analysis is carried out2. The mineral contents calculated by XRD and principal element analysis can be calibrated to each other for accurate quantification.
Preferably, the process of testing the physical parameters, mineral composition and micro-morphology of the sample polished section further comprises: observing the internal atomic arrangement structure of the sample light sheet; more preferably, the internal atomic arrangement structure of the sample light sheet is observed using a transmission electron microscope.
The physical parameters, mineral composition and micro-morphology change of the sample polished section before and after the reaction are compared, and the corrosion mechanism and the microscopic representation are known through the change of the micro-morphology and the internal structure of the mineral.
In a preferred embodiment of the present invention, during the reaction, the fading rate and the microscopic morphology of the erosion step of the carbonate are observed at certain time intervals, and the step of analyzing the composition of the reaction solution comprises:
taking out rock polished sections at certain time intervals, directly observing the fading rate and the microscopic morphology of the carbonate corrosion step at a specific calibration position by using an atomic force microscope, and adopting a contact mode; simultaneously extracting a certain amount of reaction solution, immediately supplementing a corresponding amount of original corrosion fluid into the system, and performing ICP-MS analysis on the extracted reaction solution and the original corrosion fluid to analyze Ca2+、Mg2+And testing the ion content and the pH value.
For example, in the example of the present invention, the reaction time is set to 24 hours, 10mL of the reaction solution is taken every 4 hours, and then 10mL of the original reaction solution (i.e., the original etching fluid) is injected into the system, in order to ensure a fixed water-rock ratio, even if the same 10mL of the original reaction solution is injected into the system, the concentration of each component in the system is temporarily diluted, which is a systematic error and does not affect the experimental result.
In a preferred embodiment of the present invention, the size of the sample light sheet is 2.5cm x1.5cm x (300-. The samples used are selected in areas with uniform mineral composition and distribution as much as possible, and one sample is cut into parallel sample light pieces (such as 20 pieces in the embodiment of the invention) as much as possible, so that unnecessary interference on the aspect of corrosion rate measurement caused by different mineral compositions and non-uniform mineral distribution is avoided. Before the experiment in the step 1), phase identification is carried out on the sample used in the experiment by using XRD, if the composition and distribution of minerals in the sample polished section are relatively uniform, only one sample polished section can be used for replacing the initial mineral composition and the content of each component of the sample polished section used under different conditions.
The present invention has strict requirements on the thickness of the sample, and the thickness is maintained to be less than 1mm as much as possible, and the thickness is preferably 300-500 μm. Because the film is too thin and fragile, and the film is too thick, the requirement of a high-precision instrument for a sample, such as surface Zeta potential measurement, is met, and the thickness of the sample is required to be less than 1 mm.
In a preferred embodiment of the present invention, during the immersion of the sample polished section, the sample polished section is suspended and immersed in an erosion fluid to increase the reaction area.
In a preferred embodiment of the present invention, the cleaning of the sample polished section is performed in an ultrasonic cleaning apparatus using deionized water to remove impurities and mineral microparticles attached to the surface.
The closed system is adopted instead of the open-flow system, the concentration of the components in the fluid is simulated to be increased along with the continuous water-rock reaction in the nature, and the open-flow system reacts with the rock by the constant fluid components, so that the water-rock ratio is increased invisibly, and the condition that the content difference of the components measured by ICP-MS in equal time intervals is small is avoided. In addition, the use of closed systems also makes it possible to reduce the control variables, for example to avoid CO in the air2The components and the solution generate acid equilibrium, thereby influencing the pH value and the reaction of the solutionSolubility product, both of which have been found in earlier literature investigations of the present application to have important responses to the erosion of carbonate minerals. Finally, the closed system can ensure that the Ca and Mg ions in the solution can reach the detection limit, and if the open system is adopted, the concentration of the Ca and Mg in the solution is too low, the analysis error is large, and the closed system can be completely avoided.
The types of carbonate rocks of the invention include, for example, dolomite, limestone, dolomitic limestone, oolitic limestone and the like.
The experiment simulates different Mg under specific temperature, pressure and ionic strength2+Influence of ion concentration on carbonate rock erosion. Meanwhile, the influence of the change of the Ca/Mg ratio on the carbonate corrosion is indirectly proved through the experimental method; and further provides experimental basis for judging whether the deep part of a certain region is likely to develop a good-quality reservoir.
Detailed Description
In order to more clearly illustrate the invention, the invention is further described below in connection with preferred embodiments. It is to be understood by persons skilled in the art that the following detailed description is illustrative and not restrictive, and is not to be taken as limiting the scope of the invention.
The following examples are provided herein to illustrate the simulation test method:
experimental materials: polishing carbonate rock sample films (20 copies in a formula) of Ordovician in a Tarim basin, wherein the specification is 2.5 cmx1.5cmx0.5 mm, and the two surfaces are polished; adopting acetic acid + synthetic formation water mixed solution as corrosion fluid; adopts reagent grade pure NaCl and CaCl2、Na2SO4、MgCl2As a salt standard substance; deionized water is used as the main solvent for the etching fluid.
Experimental equipment: micro-area X-ray diffraction (XRD), Scanning Electron Microscope (SEM) equipped with energy spectrum analysis (EDS), ICP-MS, high temperature high pressure reaction kettle, Transmission Electron Microscope (TEM), Atomic Force Microscope (AFM), core CT scanner, MC-ICP-MS, solid surface Zeta potential analyzer.
The experimental process comprises the following steps:
1) before a simulation experiment, the apparent micro-morphology of the mineral is observed by using SEM, a specific area is marked, the composition and semi-quantitative chemical components of the mineral in the rock are determined by using energy spectrum analysis (EDS), phase identification and quantitative calculation of the content of each mineral component are carried out by using X-ray powder crystal diffraction, meanwhile, the diffraction spectrum of the mineral (which can be used for determining the information such as the crystallinity, the order degree, unit cell parameters and the like of the mineral) can be given by using XRD analysis, and if the conditions allow the internal atomic arrangement structure of the mineral to be observed by using (TEM), and CT scanning is carried out on a sample.
2) Statistical analysis is carried out on the analysis result of the formation water of the Tarim basin by looking up related documents, and the following different Mg are configured2+An eroding fluid of ionic concentration.
Wherein, Mg is added according to preset different concentrations2+Adjustment of ion concentration MgCl2While correspondingly adjusting CaCl2To ensure that the ionic strength of the etching fluid is constant.
0.5M NaCl、0.11M CaCl2、0.02M Na2SO4And 0.15M CH3COOH；
0.5M NaCl、0.1M CaCl2、0.01M MgCl2、0.02M Na2SO4And 0.15M CH3COOH；
0.5M NaCl、0.071M CaCl2、0.03M MgCl2、0.02M Na2SO4And 0.15M CH3COOH；
0.5M NaCl、0.051M CaCl2、0.05M MgCl2、0.02M Na2SO4And 0.15M CH3COOH；
0.5M NaCl、0.01M CaCl2、0.1M MgCl2、0.02M Na2SO4And 0.15M CH3COOH。
3) And cleaning the sample polished section by using an ultrasonic cleaning instrument, drying and weighing the sample polished section, and putting the sample polished section into a reactor of a closed reaction system. The ultrasonic cleaning instrument is used for cleaning to remove impurities and mineral microparticles attached to the surface. And placing the sample into a container, and hanging the sample as much as possible to increase the reaction area.
4) In this experiment, a closed system was used, about 2L of an etching fluid was introduced into a reactor, and the reaction temperature (T ═ 40 ℃, 80 ℃, 120 ℃ and 160 ℃) was set according to the geothermal gradient, and the corresponding pressure was set to (P ═ 10MPa, 30MPa, 40MPa, 50 MPa). Simulating the pressure range from the earth surface to the depth of 6Km of the rock, wherein the pressure gradient of the buried depth is 10 MPa/Km; different depths correspond to different pressures and temperatures. The above series of different Mg are arranged under each temperature and pressure condition2+Ion concentration parallel test, the total parallel test quantity is Mg with different quantity x under temperature and pressure conditions2+The number of ion concentrations was 20 in total.
Analyzing the components of the reacted solution at 4-hour intervals, extracting 10mL of the reacted solution each time, immediately supplementing 10mL of the reaction original solution into the system, and performing ICP-MS analysis on the extracted reacted solution and the extracted original solution to mainly analyze Ca2 +、Mg2+And testing the ion content and the pH value. One parallel reaction was sampled 6 times, and 20 parallel reactions were performed for a total of 120 samples, plus the original etching fluid, and a total of 121 solution samples were used to determine the ionic content and pH.
5) And cleaning the reacted sample polished section with deionized water, drying and weighing. In order to compare the micro-morphology characteristics of minerals such as calcite and the like before and after the experiment for SEM observation, and in order to know physical parameters such as porosity, permeability and the like before and after the experiment, CT scanning analysis is carried out on the sample, and after the steps are completed, phase analysis and the content of each component are carried out by using XRD.
6) Calculating the erosion amount and the erosion rate of the rock sample before and after the reaction, determining the pore development condition of the rock according to the AFM image and the CT scanning analysis result, and further determining Mg with different concentrations2+The effect of ions on carbonate erosion.
It should be understood that the above-mentioned embodiments of the present invention are only examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention, and it will be obvious to those skilled in the art that other variations or modifications may be made on the basis of the above description, and all embodiments may not be exhaustive, and all obvious variations or modifications may be included within the scope of the present invention.
Claims (10)
1. A simulation experiment method for influence of different magnesium ion concentrations on carbonate rock corrosion is characterized by comprising the following steps:
1) testing physical parameters, mineral compositions and micro-morphology of a plurality of parallel sample polished sections;
2) simulating formation water of research area with a series of Mg in different configurations2+An eroding fluid of ionic concentration;
3) cleaning, drying and weighing the sample polished section;
4) respectively placing each corrosion fluid into a closed system, respectively immersing a sample polished section in the closed system, and setting the temperature and the pressure to carry out water-rock reaction;
in the reaction process, the regression rate and the microscopic morphology of the carbonate corrosion step are observed at certain time intervals, and the component analysis is carried out on the reaction solution;
5) after the reaction is finished, cleaning, drying and weighing the sample polished section; then, the physical parameters, mineral composition and micro-morphology of the sample polished section are tested again to compare the change before and after the reaction;
6) calculating the erosion amount and the erosion rate before and after the reaction, and determining Mg by combining the physical parameters, mineral composition and micro-morphology change of the sample polished section before and after the reaction2+Influence of ion concentration on carbonate rock erosion.
2. A simulation experiment method according to claim 1, characterized in that when there is inclusion data of carbonate minerals in the formation of the investigation region, the composition of the simulated inclusions is configured with different Mg2+An eroding fluid of ionic concentration.
3. A simulation test method according to claim 1 or 2, characterized in that the formation water or inclusion in the simulation study area is provided with NaCl, CaCl in corresponding concentrations2、MgCl2、Na2SO4And 0.15M CH3The COOH mixed solution is used as an erosion fluid;
wherein, Mg is added according to preset different concentrations2+Adjustment of ion concentration MgCl2While correspondingly adjusting CaCl2To ensure that the ionic strength of the etching fluid is constant.
4. The simulation experiment method according to claim 1, wherein when the temperature and the pressure are set, the temperature and the pressure are set according to the geothermal gradient and the pressure gradient as follows: 40 ℃/10MPa, 80 ℃/30MPa, 120 ℃/40MPa or 160 ℃/50 MPa.
5. The simulation experiment method of claim 1, wherein the process of testing the physical parameters, mineral composition and micro-topography of the sample light sheet comprises:
observing the apparent micro-morphology of the rock polished section and marking a specific area;
determining mineral composition and semi-quantitative chemical components in the rock polished section;
phase identification and quantitative calculation of each mineral component content are carried out on the rock polished section, and the crystallinity, the order degree and the unit cell parameter information of the minerals are calculated;
measuring the surface potential of the rock polished section;
measuring the physical parameters of the porosity and permeability of the rock polished section;
preferably, observing the rock sample light-sheet apparent micro-morphology by using a scanning electron microscope and marking a specific area;
determining mineral composition and semi-quantitative chemical components in a rock sample polished section by utilizing energy spectrum analysis;
phase identification and quantitative calculation of each mineral component content are carried out by utilizing X-ray powder crystal diffraction, and the crystallinity, the order degree and the unit cell parameter information of the minerals are calculated according to diffraction peak data of the X-ray diffraction;
measuring the surface potential of the rock sample polished section by using a solid surface Zeta potential analyzer;
and carrying out electronic computed tomography scanning on the rock sample polished section to obtain physical parameters including porosity and permeability before and after reaction.
6. The simulation experiment method of claim 5, wherein the process of testing the physical parameters, mineral composition and micro-topography of the sample light sheet further comprises: observing the internal atomic arrangement structure of the sample light sheet;
preferably, the internal atomic arrangement structure of the sample light sheet is observed using a transmission electron microscope.
7. The simulation experiment method of claim 1, wherein the reaction process is performed by observing the fading rate and the microscopic morphology of the erosion step of the carbonate at intervals, and the analyzing the composition of the reaction solution comprises:
taking out rock polished sections at certain time intervals, directly observing the fading rate and the microscopic morphology of the carbonate corrosion step at a specific calibration position by using an atomic force microscope, and adopting a contact mode; simultaneously extracting a certain amount of reaction solution, immediately supplementing a corresponding amount of original corrosion fluid into the system, and performing ICP-MS analysis on the extracted reaction solution and the original corrosion fluid to analyze Ca2+、Mg2+And testing the ion content and the pH value.
8. The simulation experiment method as set forth in claim 1, wherein the size of the sample light sheet is 2.5cm x1.5cm x (300-.
9. The simulation experiment method of claim 1, wherein the sample light sheet is suspended and immersed in the erosion fluid during the immersion of the sample light sheet to increase the reaction area.
10. The simulation experiment method of claim 1, wherein the cleaning of the sample polished section is performed in an ultrasonic cleaning instrument by using deionized water.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010337473.6A CN111595763B (en) | 2020-04-26 | 2020-04-26 | Simulation experiment method for influence of different magnesium ion concentrations on carbonate corrosion |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010337473.6A CN111595763B (en) | 2020-04-26 | 2020-04-26 | Simulation experiment method for influence of different magnesium ion concentrations on carbonate corrosion |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111595763A true CN111595763A (en) | 2020-08-28 |
| CN111595763B CN111595763B (en) | 2023-06-30 |
Family
ID=72189117
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010337473.6A Active CN111595763B (en) | 2020-04-26 | 2020-04-26 | Simulation experiment method for influence of different magnesium ion concentrations on carbonate corrosion |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111595763B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113033114A (en) * | 2021-03-04 | 2021-06-25 | 中国石油大学(北京) | Optimization method for mineral kinetic parameters in reservoir water rock reaction simulation |
| CN113484217A (en) * | 2021-07-06 | 2021-10-08 | 西南石油大学 | Simulation experiment method for dolomization process |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101089118A (en) * | 2006-06-16 | 2007-12-19 | 长江大学 | Acidifying agent composition |
| MX2011001035A (en) * | 2011-01-27 | 2012-07-27 | Mexicano Inst Petrol | Procedure for the determination of effective and total porosity of carbonated sedimentary rocks, and morphology characterization of their micro and nanopores. |
| CN104407118A (en) * | 2014-12-01 | 2015-03-11 | 中国石油天然气股份有限公司 | Analysis method of corrosion action and corrosion effect of carbonate rock |
| CN105403929A (en) * | 2015-12-08 | 2016-03-16 | 中国石油天然气股份有限公司 | Method and device for determining carbonate oil and gas reservoir alteration degree caused by TSR |
-
2020
- 2020-04-26 CN CN202010337473.6A patent/CN111595763B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101089118A (en) * | 2006-06-16 | 2007-12-19 | 长江大学 | Acidifying agent composition |
| MX2011001035A (en) * | 2011-01-27 | 2012-07-27 | Mexicano Inst Petrol | Procedure for the determination of effective and total porosity of carbonated sedimentary rocks, and morphology characterization of their micro and nanopores. |
| CN104407118A (en) * | 2014-12-01 | 2015-03-11 | 中国石油天然气股份有限公司 | Analysis method of corrosion action and corrosion effect of carbonate rock |
| CN105403929A (en) * | 2015-12-08 | 2016-03-16 | 中国石油天然气股份有限公司 | Method and device for determining carbonate oil and gas reservoir alteration degree caused by TSR |
Non-Patent Citations (3)
| Title |
|---|
| 丁茜等: "高温高压条件下碳酸盐岩溶蚀过程控制因素", 《石油与天然气地质》 * |
| 任庆庆等: "富CO_2流体与砂岩储层水-岩反应实验研究与应用:以黄桥油气藏龙潭组砂岩为例", 《高校地质学报》 * |
| 佘敏等: "碳酸盐岩溶蚀模拟实验技术进展及应用", 《海相油气地质》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113033114A (en) * | 2021-03-04 | 2021-06-25 | 中国石油大学(北京) | Optimization method for mineral kinetic parameters in reservoir water rock reaction simulation |
| CN113033114B (en) * | 2021-03-04 | 2022-02-11 | 中国石油大学(北京) | Optimization method for mineral kinetic parameters in reservoir water rock reaction simulation |
| CN113484217A (en) * | 2021-07-06 | 2021-10-08 | 西南石油大学 | Simulation experiment method for dolomization process |
Also Published As
| Publication number | Publication date |
|---|---|
| CN111595763B (en) | 2023-06-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Rodrigues et al. | Reinforced concrete structures: A review of corrosion mechanisms and advances in electrical methods for corrosion monitoring | |
| Santos et al. | Roughness, wettability and water absorption of water repellent treated recycled aggregates | |
| CN111595764B (en) | Experimental method for simulating influence of sulfate ion concentration on carbonate corrosion | |
| Zhao et al. | Microstructural characteristics of natural gas hydrates hosted in various sand sediments | |
| Sagbana et al. | A critical review of carbonate reservoir wettability modification during low salinity waterflooding | |
| CN111595710A (en) | Water rock reaction simulation experiment method for carbonate rock corrosion under different temperature conditions | |
| CN111595763B (en) | Simulation experiment method for influence of different magnesium ion concentrations on carbonate corrosion | |
| CN111595712A (en) | Water rock simulation reaction method for carbonate rock corrosion under different temperature and pressure conditions | |
| CN106644873A (en) | Characterization method of pore volume of organic matters in shales | |
| Jun et al. | Simulation for the dissolution mechanism of Cambrian carbonate rocks in Tarim Basin, NW China | |
| Zhang et al. | Rate of H2S and CO2 attack on pozzolan-amended Class H well cement under geologic sequestration conditions | |
| CN109781966B (en) | Method for establishing temperature correction chart of diagenetic paleoid fluid of marine carbonate reservoir | |
| Colas et al. | Influence of the clay coating properties on the dilation behavior of sandstones | |
| Grounds et al. | Resistance of supersulfated cement to strong sulfate solutions | |
| Xu et al. | Influences of rock microstructure on acid dissolution at a dolomite surface | |
| Chen et al. | Microstructures evolution and chloride migration characteristics of concrete under ultra-deep underground environment | |
| CN109916939A (en) | The test method of existing Sewage concrete structures Surface layer's concrete corrosion depth | |
| Meng et al. | Using micro-computed tomography and scanning electron microscopy to assess the morphological evolution and fractal dimension of a salt-gypsum rock subjected to a coupled thermal-hydrological-chemical environment | |
| CN111595711A (en) | Water-rock reaction simulation experiment method for asphalt-containing carbonate rock corrosion | |
| Tan et al. | Experimental investigation on the effects of different fracturing fluids on shale surface morphology | |
| Zhang et al. | Degradation process of Ag/AgCl chloride-sensing electrode in cement extract with low chloride concentration | |
| Yan et al. | Degradation of chemical and mechanical properties of cements with different formulations in CO2-containing HTHP downhole environment | |
| Meng et al. | Multiscale evolution mechanism of sandstone under wet-dry cycles of deionized water: From molecular scale to macroscopic scale | |
| Chen et al. | Stray current induced chloride ion transport and corrosion characteristics of cracked ultra-high performance concrete | |
| Xiao et al. | Pore structure characteristics of an underground limestone chamber in the Three Gorges Reservoir area |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |