CN109828099A - A kind of rock-water-hydrocarbon analogue experiment method - Google Patents
A kind of rock-water-hydrocarbon analogue experiment method Download PDFInfo
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Abstract
The present invention relates to a kind of rock-water-hydrocarbon analogue experiment methods, the steps include: the salting liquid that S1, preparation of samples and pretreatment configuration ion concentration are C mol/L, prepare mineral samplers, deionized water and hydrocarbon sample；Prepare N root silver bar as mineral samplers reaction carriers；Mineral samplers are put into silver bar, experiment silver bar sample is obtained；S2, the simulated experiment of indoor water rock is carried out to sample；S3, the sample after experiment is tested, detection gas ingredient；Detection gas isotope；Test liquefied hydrocarbon；Detect solion ingredient；Test mineral characteristic and mineralogical composition；S4, analysis rock-water-hydrocarbon interaction.Present system analyzes in different type reservoir " rock-water-hydrocarbon " interaction characteristic and organic and inorganic Dynamic Evolution, and the research for solving " rock-water-hydrocarbon " organic-inorganic interaction process and interaction mechanism in reservoir after hydro carbons fills is of great significance.
Description
Technical field
The invention belongs to geochemistry experiment technical field, it is related to rock-water-hydrocarbon simulation skill after Hydrocarbon Formation Reservoirs in reservoir
Art, specifically, being related to a kind of rock-water-hydrocarbon analogue experiment method.
Background technique
During oil-gas bearing basin buries, the reaction of organic and inorganic in hydrocarbon source rock and reservoir exist with basin at hydrocarbon-at
Storage-is the hot and difficult issue problem of petroleum geology research at hiding and each process of oil-gas pool preservation.On stratum by low temperature morning
After diagenetic stage enters late diagenetic stage in high temperature and extensive life residence occurs, " rock-water " body in oil-gas bearing basin reservoir
System evolves as " rock-water-hydrocarbon " system, organic and inorganic reaction controlling under hot conditions in reservoir reservoir at storage, at hiding
And subsequent oil-gas pool preservation process.Carry out " fluid-rock " thermal simulation experiment room using high-temperature high-pressure reaction kettle and grind in laboratory
It is hot for " rock-water-hydrocarbon " in reservoir after Hydrocarbon Formation Reservoirs to study carefully the important technology of FLUID ROCK INTERACTION process and mechanism in reservoir
The problem of simulation experiment study, there is also following two aspects at present:
(1) influence that domestic and foreign scholars interact about rock-water-hydrocarbon at present recognizes disunity.About organic and inorganic phase
In the research of interaction thermal simulation experimental method, the heat of organic matter is drilled in source-storage system before being largely focused on hydrocarbon charge
The sour process of metaplasia hydrocarbon/life, organic origin acidic fluid corrosion reservoir Minerals form the adjoint organic-nothings such as secondary pore process
Machine interaction, and to inorganic reaction, organic reaction and its correlation in oil-gas reservoir " rock-water-hydrocarbon " system after hydro carbons filling
Property research it is still relatively weak.
(2) it is anti-in thermal simulation experiment often only to analyze organic component for the organic and inorganic thermal simulation experiment carried out at present
Raw variation only simple discusses the addition of inorganic mineral and fluid to the knot of hydrocarbon cracking process and hydrocarbon product influence
Fruit variation, does not analyze in experimentation that the variation characteristic of various ions and mineral influence hydrocarbon cracking in inorganic mineral and solution
The reason of, i.e., the correlation and its interaction machine not yet in effect for analyzing organic reaction and inorganic reaction in " rock-water-hydrocarbon " system
Reason.
Summary of the invention
The present invention for existing organic and inorganic thermal simulation realize present in have in analysis " rock-water-hydrocarbon " system not yet in effect
The above problems such as the correlation and its interaction mechanism of machine reaction and inorganic reaction, provide a kind of rock-water-hydrocarbon simulated experiment side
Method, the experimental method can analyze in different type reservoir " rock-water-hydrocarbon " interaction characteristic and organic and inorganic dynamic evolution
Process.
In order to achieve the above object, the present invention provides a kind of rock-water-hydrocarbon analogue experiment methods, the specific steps are that:
S1, preparation of samples and pretreatment
S11, preparation of samples
The salting liquid that ion concentration is C mol/L is configured, mineral samplers, deionized water and hydrocarbon sample are prepared；Prepare N root
Silver bar is as mineral samplers reaction carriers；
S12, sample pretreatment
Mineral samplers are put into silver bar, experiment silver bar sample is obtained；
S2, the simulated experiment of indoor water rock is carried out to sample；
S3, the sample after experiment is tested, the specific steps are that:
Detection gas ingredient；
Detection gas isotope；
Test liquefied hydrocarbon；
Detect solion ingredient；
Test mineral characteristic and mineralogical composition；
S4, analysis rock-water-hydrocarbon interaction
It is analyzed by mineral characteristic and solution characteristics and determines inorganic mineral response path, pass through gas componant and liquefied hydrocarbon
Feature determines organic hydrocarbon evolution Feature, by signature analysis determine hydro carbons filling after " rock-water-hydrocarbon " response feature, according to point
" rock-water-hydrocarbon " Organic-inorganic interaction correlation and the mechanism of action are summarized in analysis.
Preferably, in step S11, the m that ion concentration is C mol/L is configurediThe salting liquid of g prepares m 'iG deionized water and
MiG hydrocarbon sample；Prepare mineral samplers, mineralogical composition is tested by the sharp shadow X-ray diffractometer of Dutch Panaco；Prepare N root long
100mm, the silver bar that diameter is 3mm are as mineral samplers reaction carriers.
Preferably, in step S12, mineral samplers are put into silver bar, obtain experiment silver bar sample, specific steps
Are as follows:
(1) mineral samplers are crushed to the mineral grain of 1mm, clean mineral grain, mineral grain < 40 DEG C after cleaning are low
Temperature drying carries out metal spraying processing to the mineral samplers surface after drying, is put into scanning electron microscopic observation sample surfaces, repeated washing,
It drying, surface metal spraying and observes, up to the greasy dirt and impurity of mineral particle surface are cleared step 2-3 time of sample surfaces；
(2) multiple holes are bored on every silver bar surface, is divided into 1cm between adjacent two hole, the mineral grain after cleaning is put into
Kong Zhong, it is preliminary to obtain silver bar sample；
(3) cleaning silver bar sample, the silver bar sample < 60 DEG C low temperature drying after cleaning, to the silver bar sample surfaces after drying
Metal spraying processing is carried out, is put into scanning electron microscopic observation sample surfaces, repeated washing, drying, surface metal spraying and observation sample surfaces
Step 2-3 times obtains experiment silver bar sample until the greasy dirt and impurity of silver bar Minerals particle surface are cleared.
Preferably, in step S2, carry out the specific steps of indoor water rock simulated experiment to sample are as follows:
The experimental measuring of contrived experiment parameter and experiment parameter, the experiment parameter include reaction temperature, liquor capacity, hydrocarbon
Volume and experimental period；
High-temperature high-pressure reaction kettle is put into Muffle furnace and is heated to 750 DEG C of high temperature drying 8 hours, the high temperature after high temperature drying
Autoclave acetone and ultrapure water repeated flushing 1-2 times carry out 60 DEG C of low temperature drying；
Preconfigured salting liquid, hydrocarbon sample and silver bar sample are respectively put into i according to designed experimental measuring
In group high-temperature high-pressure reaction kettle, argon gas, encapsulation process are filled with into high-temperature high-pressure reaction kettle；I group high-temperature high-pressure reaction kettle is claimed
Weight, the i group high-temperature high-pressure reaction kettle after weighing are respectively put into pyrolysis oven, start pyrolysis oven, and according to the heating of setting speed
Degree is heated, and after temperature is heated to Ti DEG C, is kept heating Di days of Ti DEG C of temperature, pyrolysis oven is closed, by high temperature high pressure reverse
It is put into cold water after answering kettle to take out and carries out quenching cooling treatment.
Preferably, in step S3, the specific steps of detection gas ingredient are as follows: be put into high-temperature high-pressure reaction kettle after cooling
Into gas collector, gas collector is connected to gas chromatograph, by entire gas collector vacuumize process,
Make the pressure in gas collector less than 1 × 10-2Pa opens high-temperature high-pressure reaction kettle, true in gas collector
Gas enters gas chromatograph by gas collector in Altitude, carries out organic hydrocarbon gas and nothing by gas chromatograph
Machine gas carries out composition test.
Preferably, in step S3, organic hydrocarbon gas is carried out by gas chromatograph and inorganic gas carries out composition test
When, it is tested using external standard method, using helium as carrier；Temperature-rise period when test are as follows: be heated to 70 DEG C in 6 minutes, later
130 DEG C are heated to from 70 DEG C with 15 DEG C/min, is heated to 180 DEG C from 130 DEG C with 25 DEG C/min, is maintained 4 minutes at 180 DEG C.
Preferably, in step S3, the specific steps of detection gas isotope are as follows: after the completion of gas componant detection, from gas
The gas that 6-8ml is extracted in collection device is injected into isotope mass spectrometer and carries out isotope detection, when carrying out isotope detection, rises
Warm process are as follows: 50 DEG C of initial temperature, constant temperature 3min, then 180 DEG C are risen to the rate of 25 DEG C/min, constant temperature 8min；All carbon
Isotope distinguishes duplicate measurements at least twice.
Preferably, in step S3, the specific steps of liquefied hydrocarbon are tested are as follows: after the completion of gas componant detection, gas collection
C6-C10 light hydrocarbon component is collected into the glass container for filling 3ml pentane by the cooling method of liquid nitrogen in device, and will be high
The same injection of liquid hydrocarbon extraction in warm autoclave fills in the glass container of 3ml pentane；Utilize ultrasonic activation glass
It glass container 25 minutes, is then allowed to stand 72 hours；Pentane solution in glass container is directly injected into liquid chromatograph；Liquid
When hydro carbons is tested, carrier gas, temperature-rise period are done using nitrogen are as follows: 50 DEG C of initial temperature, constant temperature 5min, then with the rate of 2 DEG C/min
150 DEG C are risen to, is then warming up to 150 DEG C with the rate of 4 DEG C/min, constant temperature 15min.
Preferably, in step S3, the specific steps of solion composition detection are as follows: molten in extracting high-temperature autoclave
Liquid filters off the organic component in solution, filtered solution is divided into two parts, a solution is tested organic by ion chromatograph
Acid ion and anion, another solution test cation by ICP-OES.
Preferably, in step S3, the specific steps of mineral characteristic and ingredient are tested are as follows: after indoor water rock simulated experiment, silver
Item and mineral grain methylene chloride and deionized water repeated flushing 2-3 times, remove the remaining hydro carbons of mineral particle surface；It cleans
60 DEG C of low temperature drying afterwards, the sample after drying carry out the processing of surface metal spraying, then special with the reaction of scanning electron microscopic observation mineral surfaces
Sign recycles the ingredient of energy disperse spectroscopy detection authigenic mineral.
Compared with prior art, the beneficial effects of the present invention are:
The present invention constrains item based on reservoir medium environment and thermokinetics using short-term indoor high temperature and pressure thermal simulation experiment
Part combines, different location mineral type and signature analysis, experiment front and back hydrocarbon component class in the thermal simulation system of Binding experiment front and back
Type and signature analysis, solion ingredient and concentration feature, " rock-water-hydrocarbon " system hot-die under the conditions of primary study various combination
Solid-liquid-gas variation characteristic in draft experiment fore-and-aft architecture, the correlation and interaction of analysis feldspar alteration and Oil-gas evolution
Product is analyzed in conjunction with thermochemical process, illustrates " rock-water-hydrocarbon " system inorganic-organic interaction mechanism, for solving hydro carbons
The research of " rock-water-hydrocarbon " organic-inorganic interaction process and interaction mechanism is of great significance in reservoir after filling.
Detailed description of the invention
Fig. 1 is " rock-water-in the high-temperature high-pressure reaction kettle of the reaction of indoor water rock simulated experiment described in embodiment of the present invention front and back
Hydrocarbon " system status comparison diagram；
Fig. 2 is that crude oil of the embodiment of the present invention tests front and back GC-MS component-part diagram；
Fig. 3 A is spectra of embodiment of the present invention surface characteristics figure；
Fig. 3 B is that T-2 of the embodiment of the present invention tests andesine surface heavy oil schematic diagram；
Fig. 3 C is the asphalitine schematic diagram that T-2 of the embodiment of the present invention tests andesine surface；
Fig. 3 D is the pitting schematic diagram that S-2 of the embodiment of the present invention tests andesine particle surface；
Fig. 4 A is the ultrapure aqueous systems Minerals reaction path diagram of the embodiment of the present invention；
Fig. 4 B is NaCl of embodiment of the present invention system Minerals reaction path diagram.
In figure, 1, mineral samplers, 2, silver bar, 3, water layer, 4, oil reservoir, 5, oil-water-layer, 6, high-temperature high-pressure reaction kettle.
Specific embodiment
In the following, the present invention is specifically described by illustrative embodiment.It should be appreciated, however, that not into one
In the case where step narration, element, structure and features in an embodiment can also be advantageously incorporated into other embodiments
In.
Present invention discloses a kind of rock-water-hydrocarbon analogue experiment methods, the specific steps are that:
S1, preparation of samples and pretreatment
S11, preparation of samples
Configure the m that ion concentration is C mol/LiThe salting liquid of g prepares m 'iG deionized water and MiG hydrocarbon sample；Prepare
Mineral samplers；Preparing N root long 100mm, diameter is the silver bar of 3mm as mineral samplers reaction carriers.In order to improve the standard of experiment
True property, the mineral samplers preferably use single mineral samplers, specifically, using a kind of mineral as sample, the i.e. change of mineral
It is single to learn composition, such as: using chemical composition is the mineral of main potassium feldspar as sample.
S12, sample pretreatment
Mineral samplers are put into silver bar, experiment silver bar sample is obtained；The specific steps are that:
(1) mineral samplers are crushed to the mineral grain of 1mm, clean mineral grain, mineral grain < 40 DEG C after cleaning are low
Temperature drying carries out metal spraying processing to the mineral samplers surface after drying, is put into scanning electron microscopic observation sample surfaces, repeated washing,
It drying, surface metal spraying and observes, up to the greasy dirt and impurity of mineral particle surface are cleared step 2-3 time of sample surfaces；
(2) multiple holes are bored on every silver bar surface, is divided into 1cm between adjacent two hole, the mineral grain after cleaning is put into
Kong Zhong, it is preliminary to obtain silver bar sample；
(3) cleaning silver bar sample, the silver bar sample < 60 DEG C low temperature drying after cleaning, to the silver bar sample surfaces after drying
Metal spraying processing is carried out, is put into scanning electron microscopic observation sample surfaces, repeated washing, drying, surface metal spraying and observation sample surfaces
Step 2-3 times obtains experiment silver bar sample until the greasy dirt and impurity of silver bar Minerals particle surface are cleared.
Specifically, the deionized water that acetone and > 18.5M Ω are all made of when cleaning to mineral samplers and silver bar sample is clear
It washes；Mineral grain air dry oven < 40 DEG C low temperature drying after cleaning, silver bar sample air dry oven < 60 after cleaning
DEG C low temperature drying, mineral samplers and silver bar sample after drying pass through ion sputtering instrument and carry out the processing of surface metal spraying.
S2, the simulated experiment of indoor water rock is carried out to sample；The specific steps are that:
The experimental measuring of S21, contrived experiment parameter and experiment parameter, the experiment parameter include reaction temperature, solution body
Product, hydrocarbon volume and experimental period；The indoor water rock simulated experiment parameter of design is referring to table 1.
Table 1
S22, it high-temperature high-pressure reaction kettle is put into Muffle furnace is heated to 750 DEG C of high temperature and dries 8 hours, after high temperature drying
High-temperature high-pressure reaction kettle acetone and ultrapure water repeated flushing 1-2 times carry out 60 DEG C of low temperature drying.High temperature and pressure is put into sample
Before reaction kettle, high temperature drying is carried out to high-temperature high-pressure reaction kettle, the residual organic matter in high-temperature high-pressure reaction kettle is removed, avoids
Product result is generated to hydrocarbon degradation to interfere.
S23, preconfigured salting liquid, hydrocarbon sample and silver bar sample are respectively put into according to designed experimental measuring
Into i group high-temperature high-pressure reaction kettle, argon gas, encapsulation process are filled with into high-temperature high-pressure reaction kettle；By i group high-temperature high-pressure reaction kettle
Weighing, the i group high-temperature high-pressure reaction kettle after weighing are respectively put into pyrolysis oven, start pyrolysis oven, and according to the heating of setting
Speed is heated, and after temperature is heated to Ti DEG C, is kept heating Di days of Ti DEG C of temperature, pyrolysis oven is closed, by high temperature and pressure
Reaction kettle is put into cold water after taking out and carries out quenching cooling treatment.
Wherein, step S21, S22 sequence in no particular order, it may also is that S21, high-temperature high-pressure reaction kettle is put into Muffle furnace
In be heated to 750 DEG C of high temperature and dry 8 hours, the high-temperature high-pressure reaction kettle acetone and ultrapure water repeated flushing 1- after high temperature drying
2 times, carry out 60 DEG C of low temperature drying；The experimental measuring of S22, contrived experiment parameter and experiment parameter, the experiment parameter include anti-
Answer temperature, liquor capacity, hydrocarbon volume and experimental period.
S3, the sample after experiment is tested, the specific steps are that:
S31, detection gas ingredient, the specific steps are that:
High-temperature high-pressure reaction kettle after cooling is put into gas collector, gas collector is connected to gas phase
Entire gas collector vacuumize process is made the pressure in gas collector less than 1 × 10 by chromatograph-2Pa, by high temperature
Autoclave is opened in gas collector, and gas enters gas-chromatography by gas collector in vacuum environment
Instrument carries out organic hydrocarbon gas by gas chromatograph and inorganic gas carries out composition test.
Specifically, when carrying out organic hydrocarbon gas and inorganic gas progress composition test by gas chromatograph, using outer
Mark method is tested, using helium as carrier；Temperature-rise period when test are as follows: 70 DEG C are heated in 6 minutes, later with 15 DEG C/min
130 DEG C are heated to from 70 DEG C, is heated to 180 DEG C from 130 DEG C with 25 DEG C/min, is maintained 4 minutes at 180 DEG C.Measurement error <
0.5%.
S32, detection gas isotope, the specific steps are that:
After the completion of gas componant detection, the gas that 6-8ml is extracted from gas collector is injected into isotope mass spectrometer
Isotope detection is carried out, when carrying out isotope detection, temperature-rise period are as follows: 50 DEG C of initial temperature, constant temperature 3min, then with 25 DEG C/min
Rate rise to 180 DEG C, constant temperature 8min；All carbon isotope difference duplicate measurements at least twice, the error of duplicate measurements <
0.5‰。
Specifically, after gas componant test is completed, gas collector can be pierced through with the disposable syringe of 10ml
Diaphragm of rubber, extract 6-8ml gas injection isotope mass spectrometer.Preferably, wherein isotope mass spectrometer can be with
Using gas-chromatography-isotope mass spectrometer, chromatographic column uses long 30mm, the capillary column of internal diameter 0.32mm, and column head pressure is
58kPa；It, can also be using other inert gases such as nitrogen using helium as carrier gas；The extraction amount of gas can be 6ml,
6.5ml, 7ml, 7.5ml, 8ml etc..
S33, test liquefied hydrocarbon, the specific steps are that:
After the completion of gas componant detection, C6-C10 light hydrocarbon component is collected by the cooling method of liquid nitrogen in gas collector
3ml is being filled just into the glass container for filling 3ml pentane, and by the same injection of liquid hydrocarbon extraction in high-temperature high-pressure reaction kettle
In the glass container of pentane；Using ultrasonic activation glass container 25 minutes, it is then allowed to stand 72 hours；By in glass container just
Pentane solution is directly injected into liquid chromatograph；When liquefied hydrocarbon is tested, carrier gas, temperature-rise period are done using nitrogen are as follows: starting temperature
50 DEG C, constant temperature 5min of degree, then 150 DEG C are risen to the rate of 2 DEG C/min, 150 DEG C then are warming up to the rate of 4 DEG C/min, perseverance
Warm 15min.Specifically, when extracting liquid hydrocarbon, liquid hydrocarbon is extracted in high-temperature high-pressure reaction kettle using disposable syringe, just
In operation, easily controllable liquid hydrocarbon draw amount.
S34, detection solion ingredient, the specific steps are that:
Solution in extracting high-temperature autoclave filters off the organic component in solution, filtered solution is divided into two
Part, a solution tests organic acid anions and anion by ion chromatograph, another solution tests sun by ICP-OES
Ion.
Specifically, it using the solution in disposable syringe extracting high-temperature autoclave, is gone with C18 molecular sieve filtration molten
Filtered solution is divided into two parts by the organic component in liquid.A solution by ion chromatograph (such as: ICS-900 ion
Chromatograph) test organic acid anions and anion (such as: Cl-、SO42-And CO32-Deng), wherein the separation of ion chromatograph
Column is using the Ion Pac ASl5 type splitter of long 250mm, diameter 4mm, and the guard column of the splitter of ion chromatograph is using length
50mm, diameter 4mm measurement error less than 0.01%.Another solution by ICP-OES test cation (such as: Al3+、
SiO2(aq)Na+、Ca2+Deng), measurement error is less than 0.001ppm.
S35, test mineral characteristic and mineralogical composition, the specific steps are that:
After indoor water rock simulated experiment, silver bar and mineral grain methylene chloride and deionized water repeated flushing 2-3 times are gone
Except the remaining hydro carbons of mineral particle surface；60 DEG C of drying of low temperature after cleaning, the sample after drying carry out the processing of surface metal spraying, then
With scanning electron microscopic observation mineral surfaces response feature, the ingredient of energy disperse spectroscopy detection authigenic mineral is recycled.
Specifically, silver bar and mineral grain after cleaning by air dry oven (such as: one perseverance DHG-9145A of Shanghai is bulging
Wind drying box) 60 DEG C of low temperature drying, the sample after drying is glued on aluminum sample disk with conduction is put into ion sputtering instrument (example
Metal spraying processing such as: SPT-20 small ion sputter) is carried out to sample surfaces, then with the observation mineral surfaces reaction of surface sweeping Electronic Speculum
Feature recycles the ingredient of energy disperse spectroscopy (such as: Brooker energy disperse spectroscopy) detection authigenic mineral.
Wherein, step S32, S33 in no particular order sequence, it may also is that S32, test liquefied hydrocarbon；S33, detection gas are same
Position element.Step S31, the part of S34, S35 is successively in proper order.S31, detection solution may is that the testing procedure of sample after test
Ion component, S32, detection gas ingredient, S33, test liquefied hydrocarbon, S34, detection gas isotope, S35, test mineral are special
It seeks peace mineralogical composition；Either: S31, detection solion ingredient, S32, test mineral characteristic and mineralogical composition, S33, detection
Gas componant, S34, test liquefied hydrocarbon, S35, detection gas isotope.The testing procedure of sample after test may also is that
S31, test mineral characteristic and mineralogical composition, S32, detection solion ingredient, S33, detection gas ingredient, S34, test liquid
Hydro carbons, S35, detection gas isotope；Either: S31, test mineral characteristic and mineralogical composition, S32, detection gas ingredient,
S33, test liquefied hydrocarbon, S34, detection gas isotope, S35, detection solion ingredient.
S4, analysis rock-water-hydrocarbon interaction
It is analyzed by mineral characteristic and solution characteristics and determines inorganic mineral response path, pass through gas componant and liquefied hydrocarbon
Feature determines organic hydrocarbon evolution Feature, by signature analysis determine hydro carbons filling after " rock-water-hydrocarbon " response feature, according to point
" rock-water-hydrocarbon " Organic-inorganic interaction correlation and the mechanism of action are summarized in analysis.
Specifically, scanning electron microscope feature, characteristics of energy spectrum, the ion concentration feature, gas of sample after comprehensive Pyrolysis Experiment reacts
Body ingredient and liquefied hydrocarbon signature analysis, wherein it is analyzed by mineral characteristic and solution characteristics and determines inorganic mineral response path,
Organic hydrocarbon evolution Feature is determined by gas componant and liquefied hydrocarbon feature.By signature analysis determine hydro carbons filling after " rock-
Water-hydrocarbon " response feature, according to analysis and summary " rock-water-hydrocarbon " Organic-inorganic interaction correlation and the mechanism of action.
The above-mentioned experimental method of the present invention establishes the indoor Short-Term High Temperature high pressure " rock-water-hydrocarbon " of development and tests forward simulation reality
The systems approach tested with spectra Diagenetic alteration inorganic in clear practical oil-gas reservoir effect, organic hydrocarbon splitting action, has
The inorganic action path of machine-and interaction mechanism are target, using short-term indoor high temperature and pressure thermal modeling test, before Binding experiment
Different location mineral type and signature analysis, experiment front and back hydrocarbon component type and signature analysis, solution in thermal simulation system afterwards
Ion component and concentration feature, solid in acquisition " rock-water-hydrocarbon " system thermal simulation experiment fore-and-aft architecture under the conditions of various combination-
The variation characteristic of liquid-gas analyzes the product of feldspar alteration and the phase relation of Oil-gas evolution and interaction, in conjunction with thermochemical process
Analysis, illustrates " rock-water-hydrocarbon " system inorganic-organic interaction mechanism, for " rock-water-in reservoir after solution hydro carbons filling
The research of hydrocarbon " organic-inorganic interaction process and interaction principle has great importance.
From it is existing about the analysis of oil reservoir, water layer and oil-water-layer diagenesis evolution to be only limitted to static reservoir properties study different,
Invent above-mentioned experimental method, by embedded with mineral silver bar in oil reservoir, water layer and oil-water common-layer inorganic mineral and organic hydrocarbon
Evolution Feature analysis, systematically analyzes in different type reservoir " rock-water-hydrocarbon " interaction characteristic and organic and inorganic dynamic is drilled
Change process.
Below with the simulation of the high temperature and pressure indoor water rock of Shengli Oil Field somewhere Shahe street 3500m reservoir Crude Oil and feldspar
Analogue experiment method of the present invention is made furtherly for Organic-inorganic interaction in experimental analysis arkose reservoir
It is bright.
The specific steps of experiment are as follows:
S1, preparation of samples and pretreatment
S11, preparation of samples
The NaCl solution for configuring the 5g that ion concentration is 0.5mol/L, prepares 5 deionized waters and 2g hydrocarbon sample；Prepare potassium
Feldspar Within Monominerals sample tests mineralogical composition by the sharp X-ray diffractometer of Dutch Panaco, referring to table 2, wherein 87% is potassium
Feldspar, 9% is albite, and 3% is clay mineral；Prepare N root long 100mm, the silver bar that diameter is 3mm is reacted as mineral samplers
Carrier.
Table 2
| Sample | Potassium feldspar | Albite | Quartz | Clay mineral | It amounts to |
| Chemical equation | KAlSi3O8 | NaAlSi3O8 | SiO2 | - | - |
| Content/% | 87 | 9 | 1 | 3 | 100 |
S12, sample pretreatment
(1) the potassium feldspar mineral of bulk are crushed to the tiny potassium feldspar particle of 1mm by agate mortar, with acetone and >
The deionized water of 18.5M Ω cleans potassium feldspar particle, and it is dry that the potassium feldspar particle after cleaning is put into one perseverance DHG-9145A air blast of Shanghai
Dry case < 40 DEG C low temperature drying carries out at metal spraying the potassium feldspar sample surfaces after drying using SPT-20 small ion sputter
Reason, is put into Ku Saimu EM-30 high-resolution Table top type scanning electron microscopic observation sample surfaces, repeated washing, drying, surface metal spraying and
Step 2-3 times for observing sample surfaces, until the greasy dirt and impurity of mineral particle surface are cleared, to ensure that sample surfaces
Greasy dirt and impurity are cleared.
(2) referring to Fig. 1,9 holes is bored on every silver bar surface, are divided into 1cm between adjacent two hole, by the tiny potassium after cleaning
Feldspar particle is put into hole, preliminary to obtain silver bar sample；
(3) with the deionized water cleaning silver bar sample of acetone and > 18.5M Ω, the silver bar sample after cleaning is put into Shanghai one
Permanent air dry oven < 60 DEG C DHG-9145A low temperature drying, using SPT-20 small ion sputter to the silver bar sample after drying
Surface carries out metal spraying processing, is put into Ku Saimu EM-30 high-resolution Table top type scanning electron microscopic observation sample surfaces, repeated washing,
It drying, surface metal spraying and observes, up to the greasy dirt of potassium feldspar mineral particle surface in silver bar and miscellaneous step 2-3 time of sample surfaces
Matter is cleared, obtains experiment silver bar sample.
S2, the simulated experiment of indoor water rock is carried out to sample
The device that indoor water rock simulated experiment is related to includes: the high-temperature high-voltage reaction for accommodating mineral samplers, hydrocarbon, salting liquid
Kettle, outer diameter 20mm, thickness 5mm, the height 120mm of high-temperature high-pressure reaction kettle, temperature: -650 DEG C of room temperature；Pyrolysis oven, temperature
Degree: -650 DEG C of room temperature；Central reaction container, temperature: -650 DEG C of room temperature；The temperature sensor of central reaction vessel temp is measured,
Control the temperature controller (20 DEG C/h, 2 DEG C/h, temperature controller error is ± 1 DEG C) of central reaction vessel temp.
The specific steps of indoor water rock simulated experiment are as follows:
The experimental measuring of S21, contrived experiment parameter and experiment parameter, the experiment parameter include reaction temperature, solution body
Product, hydrocarbon volume and experimental period；The indoor water rock simulated experiment parameter of design is referring to table 3.
Table 3
S22, it high-temperature high-pressure reaction kettle is put into Muffle furnace is heated to 750 DEG C of high temperature and dries 8 hours, remove high temperature and pressure
Organic matter in reaction kettle, high temperature drying after high-temperature high-pressure reaction kettle acetone and ultrapure water repeated flushing 1-2 times after, be put into
One perseverance DHG-9145A air dry oven of Shanghai carries out 60 DEG C of low temperature drying.
S23, preconfigured NaCl solution, hydrocarbon sample and silver bar sample are put respectively according to the experimental measuring in table 3
Enter into 6 groups of high-temperature high-pressure reaction kettles, feldspar can react with crude oil, solution simultaneously in silver bar, and sample is put into backward
Argon gas is filled in high-temperature high-pressure reaction kettle, anti-room air influences high temperature pyrolysis reaction, encapsulation process after hot Buddhist nunnery；It is high by 6 groups
Warm autoclave weighing, 6 groups of high-temperature high-pressure reaction kettles after weighing are respectively put into pyrolysis oven, start pyrolysis oven, and press
High-temperature high-pressure reaction kettle be heated to 360 DEG C rapidly in 12 hours heat according to the 20 DEG C/h of heating rate of setting,
After temperature is heated to 360 DEG C, is kept for 360 DEG C of temperature heat 2 days and 6 days, pyrolysis oven is closed after experiment, by high temperature high pressure reverse
It is put into cold water after answering kettle to take out and carries out quenching cooling treatment.
S3, the sample after experiment is tested
S31, detection gas ingredient
After experiment, high-temperature high-pressure reaction kettle after cooling is put into gas collector, gas collection is filled
Set and be connected to gas chromatograph, by entire gas collector vacuumize process, make pressure in gas collector less than 1 ×
10-2Pa opens high-temperature high-pressure reaction kettle in gas collector, and gas is entered by gas collector in vacuum environment
To gas chromatograph, organic hydrocarbon gas is carried out by gas chromatograph and inorganic gas carries out composition test.Predominantly detect survey
C in gaseous hydrocarbons after examination T/S-1, T/S-3, T/S-6 reaction1-C5、CO2、H2Ingredient and content, table 4 be experiment in C1-C5、
CO2And H2The yield and gas yield ratio and content of gas.
Table 4
Referring to table 4, in dry oil system, CO2, low molecule alkane (C1-C5) low output, H2Yield is high.
With continued reference to table 4, and referring to fig. 2, in the experiment of ultrapure aqueous systems in (T-3, S-3), mineral reaction promotes original
Oil-breaking generates more C1-C5Alkane, carbon dioxide gas, however H2Generation obviously significantly inhibited.Work as isomeric alkane
When the smaller change of the ratio of hydrocarbon and n-alkane, C1/C2, C2/C3, C1/C2+C3, C1/(C1~C5), C2ene/C2, C3ene/C3Slightly
Reduce.
With continued reference to table 4 and Fig. 2, in sodium chloride system (T-6, S-6), the cracking of crude oil of the response inhabitation of mineral,
Result in less H2、CO2, low molecule alkane (C1-C5) generate.C1/C2、C2/C3、C1/C2+C3、C1/(C1~C5)、C2ene/C2、
C3ene/C3Increase with the ratio of isoparaffin and n-alkane.
With continued reference to table 4, compared with anhydrous (T/S-1) system, ultrapure aqueous systems (T/S-3) and NaCl (T/S-6) system
In, more low molecular hydrocarbons and carbon dioxide generate.In addition to this, referring to table 6, a large amount of organic acids produce in crude oil pyrolysis
It is raw.The reduction of more low molecular hydrocarbons and macromolecule hydro carbons shows that water promotes the cracking of crude oil.More organic acids and two
The generation of carbonoxide shows that water provides additional hydrogen and hydroxyl for the cracking of crude oil.
With continued reference to table 4, in experiment in two days (T1/T3/T6), the presence of water results in H2Yield increase.At 6 days
Experiment in, compared with experiment in two days, H2Yield there is no increase, and low molecular hydrocarbon increase, isoparaffin with just
The ratio of structure alkane reduces, and shows that additional hydrogen largely consumes in forming low molecule alkane.
S32, detection gas isotope
Gas isotope mainly tests the same position of gaseous hydrocarbons C1-C5 gaseous hydrocarbons carbon after T/S-1, T/S-3, T/S-6 reaction
Element, table 5 are gas δ in experiment13C content.
Table 5
Referring to C in experiment in table 5,6 days1~C5δ13C experiment in than 2 days is low, shows the progress with experiment, low molecular
Hydro carbons is easier to crack.
S33, test liquefied hydrocarbon, the specific steps are that:
Pass through liquid hydrocarbon in crude oil after the non-heating in crude oil of liquid chromatograph test and T/S-1, T/S-3, T/S-6 reaction
Ingredient and changes of contents.
With continued reference to Fig. 2, compared with liquid hydrocarbon ingredient in unheated crude oil and content, the experiment of ultrapure aqueous systems (T-3,
S-3 in), mineral reaction promotes crude oil pyrolysis and generates more C10-C15Alkane, however H2、C6-C9Alkane, pentamethylene, methyl
The generation of hexamethylene, toluene, dimethylbenzene is obviously significantly inhibited.
With continued reference to Fig. 2, compared with liquid hydrocarbon ingredient in unheated crude oil and content, in sodium chloride system (T-6,
S-6 in), the cracking of crude oil of the response inhabitation of mineral results in less H2、CO2, organic acid, low molecule alkane (C1-C10)、
Pentamethylene, hexahydrotoluene, toluene and dimethylbenzene generate.
S34, detection solion ingredient, the specific steps are that:
By the solution extraction in the high-temperature high-pressure reaction kettle after reaction, after filtration treatment, surveyed by ion chromatograph
Try solution organic acid anions after T/S-1, T/S-3, T/S-6 react, Cl-、SO4 2-And CO3 2-Equal anion and Al3+、SiO2
(aq)、K+、Na+、Ca2+Equal cations.Solution lining concentration is referring to table 6 after experiment.
Table 6
With continued reference to table 6, in ultrapure aqueous systems experiment (T-3, S-3), mineral reaction promotes crude oil pyrolysis and generates more
Organic acid.
With continued reference to table 6, in sodium chloride system in (T-6, S-6), the cracking of crude oil of the response inhabitation of mineral causes
Less organic acid generates.
S35, test mineral characteristic and mineralogical composition
The processing of surface metal spraying, scanning electron microscopic observation sample are carried out using the sample after the drying of SPT-20 small ion sputter
It can be seen that: feldspar smooth surface before reacting (referring to Fig. 3 A).In dry oil system, the visible a large amount of heavy oil in feldspar surface and
Asphalitine (referring to Fig. 3 B, Fig. 3 C).Show that feldspar particle surface produces pole after reaction in 2-6 days by scanning electron microscope
A small amount of pitting (Fig. 3 D), feldspar particle surface do not have any secondary mineral to generate.
By the features of mineral surfaces after scanning electron microscope and Brooker energy disperse spectroscopy observing response and detection authigenic mineral at
Analysis can obtain:
In the experimental group (T-3 and S-3) of oil-ultrapure water-and the silver bar with potassium feldspar, wherein to silver-colored in 2 days T-3 experimental groups
Potassium feldspar surface on item is it has been observed that can be good at the rodlike boehmite of 4-8 μm of idiomorphism (referring to figure in the feldspar of water layer reaction
4A-5), the boehmite (A-3 referring to fig. 4) of 1-2 μm of corynebacterium, visible silk hair-like Erie in oil reservoir can be good in oil-water common-layer
Stone (A-1 referring to fig. 4).It observes potassium feldspar surface in 6 days S-3 experimental groups to find, the visible higher flower of euhedral degree in water layer
Shape mica aggregate (A-6 referring to fig. 4), visible flower-shaped mica aggregate and half flower-shaped mica sheet (A- referring to fig. 4 in oil-water common-layer
4), the visible octagonal mica sheet of idiomorphism (A-2 referring to fig. 4) in oil reservoir.
It can be obtained in conjunction with 6 days and 6 days andesine Mineral changes, it is longer than potassium in system in this low sodium potassium of oil-ultrapure water-feldspar
Stone response path are as follows: potassium feldspar is initially formed boehmite (referring to a2) after corrosion (referring to a1) occurs, and boehmite corrosion later is formed
Illite (referring to a3, a4) ultimately forms mica (referring to a5).Specifically, ultrapure aqueous systems Minerals response path are as follows:
KAlSi3O8(potassium feldspar)+4H+=2H2O+K++Al3++3SiO2(aq) (a1)
2H2O+Al3+=AlO (OH) (boehmite)+3H+ (a2)
3Al3++3SiO2(aq)+K++6H2O=KAl2Si3O10(OH)2(illite/mica)+10H+ (a3)
3AlO (OH) (boehmite)+3SiO2(aq)+Na+=KAlSi3O10(OH)2(mica)+H+ (a4)
3KAlSi3O8(potassium feldspar)+2H+=KAl2Si3O10(OH)2(illite/mica)+6SiO2+2K++6SiO2(aq)
(a5)
It is real in 2 days T-6 in the experimental group (T-6 and S-6) of oil -0.5mol/LNaCl solution-and the silver bar with potassium feldspar
It tests in group, the rodlike boehmite (B-5 referring to fig. 4) of 50 μm of idiomorphisms can be good in water layer, 10-30 μm can be good in oil-water common-layer
The rodlike boehmite of subhedral and radial, pencil boehmite aggregate (B-3 referring to fig. 4), the visible sodium cloud master slice in oil reservoir
Surround boehmite (B-1 referring to fig. 4).The experimental group andesine surface T-3 discovery in 6 days is observed, it is visible cellular in water layer
Paragonite aggregate (B-6 referring to fig. 4), the visible hypautomorphic paragonite thin slice (B-4 referring to fig. 4) in oil-water common-layer, in oil
Visible cellular paragonite and short cylinder albite (B-2 referring to fig. 4) in layer.
It can be obtained in conjunction with 6 days and 6 days andesine Mineral changes, it is longer than in system in this high sodium potassium of oil-NaCl solution-feldspar
Stone response path are as follows: corrosion (referring to b1) occurs for potassium feldspar first, later boehmite precipitating (referring to b2), after boehmite corrosion
(referring to b3), paragonite form (referring to b4, b5), eventually form albite (referring to b6, b7, b8).Specifically, in NaCl system
Mineral response path:
KAlSi3O8(potassium feldspar)+4H+=2H2O+K++Al3++3SiO2(aq) (b1)
2H2O+Al3+=AlO (OH) (boehmite)+3H+ (b2)
3Al3++3SiO2(aq)+Na++6H2O=NaAl2Si3O10(OH)2(paragonite)+10H+ (b3)
3AlO (OH) (boehmite)+3SiO2(aq)+Na+=KAlSi3O10(OH)2(paragonite)+H+ (b4)
KAlSi3O8(potassium feldspar)+Na++2H+=NaAl2Si3O10(OH)2(paragonite)+6SiO2(aq)+3K+ (b5)
Na++Al3++3SiO2(aq)+2H2O=NaAl2Si3O8(albite)+4H+ (b6)
NaAl2Si3O10(OH)2(paragonite)+6SiO2(aq)+2Na+=NaAl2Si3O8(albite)+2H+ (b7)
KAlSi3O8(potassium feldspar)+Na+=NaAl2Si3O8(albite)+K+ (b8)
S4, analysis rock-water-hydrocarbon interaction
The scanning electron microscope feature of sample after comprehensive Pyrolysis Experiment reaction, characteristics of energy spectrum, ion concentration feature, gas componant and
Liquefied hydrocarbon signature analysis, wherein analyzed by mineral characteristic and solution characteristics and determine inorganic mineral response path, pass through gas
Ingredient and liquefied hydrocarbon feature determine organic hydrocarbon evolution Feature." rock-water-hydrocarbon " is anti-after determining hydro carbons filling by signature analysis
Feature is answered, according to analysis and summary " rock-water-hydrocarbon " Organic-inorganic interaction correlation and the mechanism of action.
By potassium feldspar ensaying as it can be seen that the alteration of potassium feldspar is stronger than in water layer in oil reservoir, show the cracking of crude oil
It can promote the alteration of mineral (referring to Fig. 3 A, Fig. 3 B).In NaCl solution system (T/S-6), (T/ compared with ultrapure aqueous systems
S-3), more gases, liquid hydrocarbon and organic acid generate show the addition of NaCl promote hydro carbons cracking (referring to fig. 2, table 4,
Table 6).Comprehensive front analysis test shows that one side water energy enough promotes the cracking of crude oil, and on the other hand, water energy enough dissolves feldspar
Mineral.Feldspar alteration, which is promoted, in the cracking of water-crude oil-feldspar system Crude Oil forms stronger turn with mineral of authigenic mineral
Change.The generation of a large amount of mineral alteration and low molecular hydrocarbon shows that water is anti-in organic and inorganic in Crude oil-water-feldspar system simultaneously
Bridge beam action is played in answering.Organic-inorganic interaction has different response paths in different geochemical systems, and
Cause to generate different influences to buried oily arkose reservoir.It is tested by the cracking of the above high temperature and pressure and its relevant
Analysis test can find that the cracking of oil reservoir Crude Oil can produce liquid and gaseous hydrocarbons and a large amount of asphalitine and hydrogen,
A small amount of carbon dioxide and organic acid.Since the generation of a large amount of asphalitines leads to the quality decline of crude oil.Simultaneously as asphalitine
Blocking hole and pore throat cause the quality of reservoir to decline.Continue to crack in arkose Crude Oil.Water can generate additional
Hydrogen and hydroxyl generate more organic acids and carbon dioxide so that crude oil pyrolysis be promoted to generate more liquid and gaseous hydrocarbon.It is former
The organic acid and carbonic acid that oil-breaking generates can dissolve silicate mineral to generate secondary pore, and secondary pore can be used as future
The important place of hydrocarbon charge.Meeting crude oil for inhibiting cracking is reacted in brine layer Minerals to save to be conducive to crude oil to deep layer.
So organic and inorganic reacts the quality that can improve reservoir and hydro carbons in oil-water common-layer.
Embodiment provided above only with illustrating the present invention for convenience, and it is not intended to limit the protection scope of the present invention,
Technical solution scope of the present invention, person of ordinary skill in the field make various simple deformations and modification, should all include
In the above claim.
Claims (10)
1. a kind of rock-water-hydrocarbon analogue experiment method, which is characterized in that the specific steps are that:
S1, preparation of samples and pretreatment
S11, preparation of samples
The salting liquid that ion concentration is C mol/L is configured, mineral samplers, deionized water and hydrocarbon sample are prepared；Prepare N root silver bar
As mineral samplers reaction carriers；
S12, sample pretreatment
Mineral samplers are put into silver bar, experiment silver bar sample is obtained；
S2, the simulated experiment of indoor water rock is carried out to sample；
S3, the sample after experiment is tested, the specific steps are that:
Detection gas ingredient；
Detection gas isotope；
Test liquefied hydrocarbon；
Detect solion ingredient；
Test mineral characteristic and mineralogical composition；
S4, analysis rock-water-hydrocarbon interaction
It is analyzed by mineral characteristic and solution characteristics and determines inorganic mineral response path, pass through gas componant and liquefied hydrocarbon feature
It determines organic hydrocarbon evolution Feature, " rock-water-hydrocarbon " response feature after hydro carbons filling is determined by signature analysis, it is total according to analysis
Tie " rock-water-hydrocarbon " Organic-inorganic interaction correlation and the mechanism of action.
2. rock-water-hydrocarbon analogue experiment method as described in claim 1, which is characterized in that in step S11, configure ion concentration
For the m of C mol/LiThe salting liquid of g prepares m 'iG deionized water and MiG hydrocarbon sample；Prepare mineral samplers, is received by Dutch pa
The sharp shadow X-ray diffractometer of section tests mineralogical composition；Prepare N root long 100mm, the silver bar that diameter is 3mm is reacted as mineral samplers
Carrier.
3. rock-water-hydrocarbon analogue experiment method as claimed in claim 2, which is characterized in that in step S12, mineral samplers are put
Enter in silver bar, obtains experiment silver bar sample, the specific steps are that:
(1) mineral samplers are crushed to the mineral grain of 1mm, clean mineral grain, the mineral grain < 40 DEG C low temperature after cleaning dries
It is dry, metal spraying processing is carried out to the mineral samplers surface after drying, is put into scanning electron microscopic observation sample surfaces, repeated washing, drying,
Step 2-3 times of surface metal spraying and observation sample surfaces, until the greasy dirt and impurity of mineral particle surface are cleared；
(2) multiple holes are bored on every silver bar surface, are divided into 1cm between adjacent two hole, the mineral grain after cleaning is put into hole,
It is preliminary to obtain silver bar sample；
(3) cleaning silver bar sample, the silver bar sample < 60 DEG C low temperature drying after cleaning carry out the silver bar sample surfaces after drying
The step of metal spraying processing, is put into scanning electron microscopic observation sample surfaces, repeated washing, drying, surface metal spraying and observation sample surfaces
2-3 times, until the greasy dirt and impurity of silver bar Minerals particle surface are cleared, obtain experiment silver bar sample.
4. rock-water-hydrocarbon analogue experiment method as claimed in claim 2 or claim 3, which is characterized in that in step S2, carry out to sample
The specific steps of indoor water rock simulated experiment are as follows:
The experimental measuring of contrived experiment parameter and experiment parameter, the experiment parameter include reaction temperature, liquor capacity, hydrocarbon volume
And experimental period；
High-temperature high-pressure reaction kettle is put into Muffle furnace and is heated to 750 DEG C of high temperature drying 8 hours, the high temperature and pressure after high temperature drying
Reaction kettle acetone and ultrapure water repeated flushing 1-2 times carry out 60 DEG C of low temperature drying；
Preconfigured salting liquid, hydrocarbon sample and silver bar sample are respectively put into i group height according to designed experimental measuring
In warm autoclave, argon gas, encapsulation process are filled with into high-temperature high-pressure reaction kettle；I group high-temperature high-pressure reaction kettle is weighed, is claimed
I group high-temperature high-pressure reaction kettle after weight is respectively put into pyrolysis oven, starts pyrolysis oven, and carry out according to the heating rate of setting
Heat treatment after temperature is heated to Ti DEG C, keeps heating Di days of Ti DEG C of temperature, closes pyrolysis oven, high-temperature high-pressure reaction kettle is taken
It is put into after out in cold water and carries out quenching cooling treatment.
5. rock-water-hydrocarbon analogue experiment method as claimed in claim 4, which is characterized in that in step S3, detection gas ingredient
Specific steps are as follows: high-temperature high-pressure reaction kettle after cooling is put into gas collector, gas collector is connected
Make the pressure in gas collector less than 1 × 10 entire gas collector vacuumize process to gas chromatograph-2Pa,
High-temperature high-pressure reaction kettle is opened in gas collector, gas enters gas phase by gas collector in vacuum environment
Chromatograph carries out organic hydrocarbon gas by gas chromatograph and inorganic gas carries out composition test.
6. rock-water-hydrocarbon analogue experiment method as claimed in claim 5, which is characterized in that in step S3, pass through gas-chromatography
When instrument carries out organic hydrocarbon gas and inorganic gas progress composition test, tested using external standard method, using helium as load
Body；Temperature-rise period when test are as follows: be heated to 70 DEG C within 6 minutes, be heated to 130 DEG C from 70 DEG C with 15 DEG C/min later, with 25 DEG C/
Min is heated to 180 DEG C from 130 DEG C, maintains 4 minutes at 180 DEG C.
7. rock-water-hydrocarbon analogue experiment method as claimed in claim 5, which is characterized in that in step S3, the same position of detection gas
The specific steps of element are as follows: after the completion of gas componant detection, the gas that 6-8ml is extracted from gas collector is injected into isotope
Mass spectrograph carries out isotope detection, when carrying out isotope detection, temperature-rise period are as follows: and 50 DEG C of initial temperature, constant temperature 3min, then with 25
DEG C/rate of min rises to 180 DEG C, constant temperature 8min；All carbon isotope difference duplicate measurements are at least twice.
8. rock-water-hydrocarbon analogue experiment method as claimed in claim 5, which is characterized in that in step S3, test liquefied hydrocarbon
Specific steps are as follows: after the completion of gas componant detection, C6-C10 light hydrocarbon component passes through the cooling side of liquid nitrogen in gas collector
Method is collected into the glass container for filling 3ml pentane, and the same injection of liquid hydrocarbon extraction in high-temperature high-pressure reaction kettle is contained
In the glass container for having 3ml pentane；Using ultrasonic activation glass container 25 minutes, it is then allowed to stand 72 hours；Glass is held
Pentane solution in device is directly injected into liquid chromatograph；When liquefied hydrocarbon is tested, carrier gas, temperature-rise period are done using nitrogen
Are as follows: 50 DEG C of initial temperature, constant temperature 5min, then 150 DEG C are risen to the rate of 2 DEG C/min, then it is warming up to the rate of 4 DEG C/min
150 DEG C, constant temperature 15min.
9. rock-water-hydrocarbon analogue experiment method as claimed in claim 4, which is characterized in that in step S3, solion ingredient
The specific steps of detection are as follows: the solution in extracting high-temperature autoclave filters off the organic component in solution, will be filtered molten
Liquid is divided into two parts, and a solution tests organic acid anions by ion chromatograph and anion, another solution pass through ICP-
OES test cation.
10. rock-water-hydrocarbon analogue experiment method as claimed in claim 4, which is characterized in that in step S3, test mineral characteristic
With the specific steps of ingredient are as follows: after indoor water rock simulated experiment, silver bar and mineral grain methylene chloride and deionized water are repeatedly
It rinses 2-3 times, removes the remaining hydro carbons of mineral particle surface；60 DEG C of drying of low temperature after cleaning, the sample after drying carry out surface
Metal spraying processing, then uses scanning electron microscopic observation mineral surfaces response feature, recycles the ingredient of energy disperse spectroscopy detection authigenic mineral.
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| CN110176165A (en) * | 2019-06-20 | 2019-08-27 | 中国石油大学(华东) | A kind of thermal simulation synthesis experiment method of " hydrocarbon-water-rock " interaction |
| CN115015404A (en) * | 2022-04-27 | 2022-09-06 | 中国石油大学(华东) | Isotope-tracing-based hydrocarbon-water-rock interaction thermal simulation experiment method |
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| CN108614076A (en) * | 2018-04-27 | 2018-10-02 | 中国石油大学(华东) | A kind of carbon dioxide geologic sequestration evaluation method |
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| CN110176165A (en) * | 2019-06-20 | 2019-08-27 | 中国石油大学(华东) | A kind of thermal simulation synthesis experiment method of " hydrocarbon-water-rock " interaction |
| CN110176165B (en) * | 2019-06-20 | 2022-02-15 | 中国石油大学(华东) | Thermal simulation comprehensive experiment method for hydrocarbon-water-rock interaction |
| CN115015404A (en) * | 2022-04-27 | 2022-09-06 | 中国石油大学(华东) | Isotope-tracing-based hydrocarbon-water-rock interaction thermal simulation experiment method |
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