CN108088874A - A kind of leaching method of black shale soluble salt - Google Patents
A kind of leaching method of black shale soluble salt Download PDFInfo
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- CN108088874A CN108088874A CN201711325067.2A CN201711325067A CN108088874A CN 108088874 A CN108088874 A CN 108088874A CN 201711325067 A CN201711325067 A CN 201711325067A CN 108088874 A CN108088874 A CN 108088874A
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- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
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Abstract
The invention discloses a kind of leaching methods of black shale soluble salt, it comprises the following steps：1. black shale is prepared into the Centimeter Level bulk sample of arbitrary shape；2. drying sample using vacuum drying chamber, and weigh；3. adding in distilled water and organic reducing agent acetoxime in container, aqueous solution is made to be in strong reducing environment (Eh values are less than 200mV)；4. shale bulk sample is totally submerged in step 3. middle aqueous solution, and monitor aqueous solution Eh values, electrical conductivity in real time respectively using oxidation-reduction potentiometer, conductivity meter；5. controlling the addition of acetoxime during leaching experiment, aqueous solution is made to keep strong reducing environment (Eh values are less than 200mV)；6. when aqueous solution conductivity values are not further added by, the leaching liquid of the soluble salt containing black shale is obtained.Using the present invention it is possible to prevente effectively from soluble salt leaching process mineral oxide, corrosion, and prevent sample making course soluble salt from losing, so as to obtain accurate black shale soluble salt ions composition data.
Description
Technical field
The present invention relates to oil and gas production technique field core analysis methods, and in particular to leaching black shale can
The experimental method of dissolved salt.
Background technology
Water flooding and Reservoir rocks Long Term Contact, under oil-gas reservoir high-temperature and high-pressure conditions, multi mineral is (such as length in rock
Stone, calcite, dolomite, clay mineral etc.) corrosion, phase transformation occurs, cause water flooding salt containing various metals, such as sylvite, sodium
Salt, calcium salt, magnesium salts etc., therefore water flooding is also referred to as brine.Formation water salinity (i.e. salt content) represents anions and canons in water and contains
The summation of amount, unit are mg/L or ppm.Formation water salinity difference is very big in Reservoir rocks, from thousands of, tens of thousands of to hundreds of thousands
Mg/litre, but main zwitterion species is only several, if anion is Cl-、SO4 2-、CO3 2-Or HCO3 -, cation is Na+、K+、
Ca2+、Mg2+。
It is that indoor simulation oil-gas reservoir environment carries out rock core displacement reality to understand each zwitterion type, content in water flooding in advance
Working solution (such as drilling fluid, fracturing fluid) and water flooding ionic species when testing the basis of evaluation and understanding, prevention Reservoir Development
Type, which is incompatible, induces the premise of damage.
Using solvent leach soluble salt in rock be obtain water flooding ionic type, content important method.Particularly, page
Rock gas reservoir prime stratum water content is extremely low, and stratum coring or recovery process can not obtain water flooding, therefore can in leaching rock
Dissolved salt is to determine shale gas reservoir water flooding ionic type, the unique method of content.
China-styled Certain Industry Field standard SY/T5336-2006《Core analysis method》, Chinese invention patent publication number CN
103411817 A disclose the experimental method using methanol cleaning rock soluble salt, and methanol is injected blowhole by this method, profit
It, can soluble salt effectively in lashing hole with the characteristic of the soluble inorganic salts of methanol.But methanol belongs to organic solvent, with water
The physicochemical properties of solution are there are huge difference, therefore the soluble salt of methanol leaching is difficult to use in ion chromatography, inductive coupling
Plasma mass (ICP-MS) detects, and so as to add soluble salt ions type, content detection difficulty, reduces ion detection
Precision.In addition, methanol is volatile, and it is big to human toxicity, so as to limit the use that rock soluble salt is leached using methanol as solvent
Scope.
China-styled Certain Industry Field standard SY/T5336-2006《Core analysis method》, Chinese invention patent (publication number CN
106353411 A), Chinese invention patent (102169115 A of publication number CN) disclose leaching rock in salinity experiment side
Rock is ground to grain size less than 1mm by method, this method, and using distilled water as the extracting solvent of soluble salt.This method is for leaching
Soluble salt in sandstone, carbonate rock has better effects, but be derived from the black shale sample of shale gas reservoir mineral composition, can
Dissolved salt and rock compactness extent are very unique, are had the following disadvantages when leaching black shale soluble salt using this method：
First, under the distilled water immersion effect containing dissolved oxygen, black shale mineral dissolution causes to leach solvable salt content
It is sharply increased.Black shale generally contains pyrite, and strong reducing environment is formed in the mineral, and iron, element sulphur are in also original state
State.Domestic and international open source literature data shows that under surface water and oxygen effect pyrite in water easily with dissolving in black shale
Oxygen chemically reacts, generation sulfate radical (SO4 2-), hydrogen ion (H+), ferric ion (Fe3+), and H+Further corrosion shale
Middle carbonate mineral, and generate Ca2+、Mg2+Ion.The distilled water that method disclosed above uses, can not effectively remove molten in water
Oxygen is solved, leaching process pyrite is caused easily to be aoxidized, SO in the leaching liquid of acquisition4 2-、Fe3+、Ca2+、Mg2+Ion is seriously inclined
It is high.
Second is that the solvable salt content of black shale is high, crushes, grind, screening process soluble salt easy to be lost.According to the open text of foreign countries
Data is offered, well fracturing fluid is entered in fracturing process, and (bulk composition is water, and salinity is less than 1 × 103Mg/L it is) long-term with shale reservoir
Contact, fracturing fluid salinity is more than 1 × 10 when causing the row of returning5Mg/L, the value change much larger than sandstone reservoir fracturing fluid salinity
Amount reflects that solvable salt content is much larger than sandstone in shale hole.Therefore, indoor crushing, grinding (grain size is less than 1mm), screening
During shale, shale soluble salt is easily caused to be lost, the solvable salt content for making unit mass or unit volume shale is seriously relatively low.
Third, black shale hole is Nano grade, matrix permeability is in and receives darcy scope, more conventional sandstone, carbonate
Rock is more fine and close, and water is more very long the time required to entering shale hole leaching soluble salt, and the leaching time of the above method is set
It is subjective judgement when small (such as 1 or 1 day), can not ensures whether leach shale soluble salt completely in setting time.
Described in summary, at present in petroleum gas field core analysis technology, removed using methanol or distilled water, extraction
Soluble salt is feasible method in sandstone, carbonate rock, but black shale part mineral (such as pyrite) is oxidizable, solvable salt content
High, leaching time is not known, it has been disclosed that experimental method can not effectively obtain the leaching liquid of the soluble salt containing black shale.
The content of the invention
It is an object of the invention to overcome the oxidizable corrosion of leaching process mineral, sample making course existing for existing method solvable
Salt is easy to be lost and leaching time setting not science the defects of, propose a kind of leaching method of black shale soluble salt, this method
Centimeter Level massive shale sample is selected, using organic reducing agent extracting solvent (i.e. distilled water) is kept to be in anaerobic state, and led to
The electrical conductivity of monitoring leaching liquid is crossed rationally to determine leaching time, can accurately obtain the leaching liquid of the soluble salt containing black shale, is protected
Shale gas reservoir water flooding ionic type, the accurate evaluation of content are demonstrate,proved.
The present invention is achieved by the following technical solutions：1. the Centimeter Level that black shale is prepared into arbitrary shape is block
Sample；2. drying sample using vacuum drying chamber, and weigh；3. distilled water and organic reducing agent acetoxime are added in container,
Aqueous solution is made to be in strong reducing environment (Eh values are less than -200mV)；4. by shale bulk sample be totally submerged in step 3. in it is water-soluble
Liquid, and monitor aqueous solution Eh values, electrical conductivity in real time respectively using oxidation-reduction potentiometer, conductivity meter；5. leaching experiment process
The addition of middle control acetoxime makes aqueous solution keep strong reducing environment (Eh values are less than -200mV)；6. when aqueous solution electrical conductivity
When numerical value is not further added by, the leaching liquid of the soluble salt containing black shale is obtained.
Acetoxime is a kind of strong reductant, it is easy to react, can thoroughly eliminate molten in aqueous solution with dissolved oxygen in aqueous solution
Oxygen is solved, and does not change pH value of water solution.Meanwhile acetoxime is a kind of organic reagent, after adding in aqueous solution, will not be introduced and stratum
Water forms similar zwitterion, avoids foreign substance pollution.When adding in acetoxime in aqueous solution makes Eh values less than -200mV
(i.e. reduction water body environment by force), pyrite will be in chemical stabilization state, avoid the oxidation corrosion of shale minerals.With water-soluble
Liquid enters shale samples hole, and the soluble salt of internal pore surface dissolves, and passes through diffusion way and make the inside and outside aqueous solution of hole
Progressively reach ion concentration balance.Aqueous solution conductivity value preferably reflects effects of ion concentration, therefore passes through monitoring
Aqueous solution conductivity value can rationally determine leaching time, so as to obtain accurate solvable salt content.
A kind of leaching method of black shale soluble salt, comprises the following steps successively：
(1) Sichuan Basin XX shale gas well black shales are chosen, arbitrary shape is quickly prepared under dry air environment
Centimeter Level massive shale sample；
(2) massive shale sample is put into vacuum drying chamber, under temperature 60 C state, sample is dried, after weighing drying
Sample quality；
(3) distilled water is added in container, is inserted into oxidation-reduction potentiometer, monitors water body oxidation-reduction potential (Eh), and
Organic reducing agent acetoxime is continuously added into, until aqueous solution Eh values are less than -200mV；
(4) massive shale sample is totally submerged in step (3) aqueous solution after weighing, insertion oxidation-reduction potentiometer,
Conductivity meter, sealing container；
(5) aqueous solution Eh values are monitored during leaching experiment in real time, when Eh values are higher than -200mV, add in acetone again
Oxime makes aqueous solution Eh values be less than -200mV；
(6) aqueous solution electrical conductivity, when conductivity values are not further added by, leaching experiment are monitored during leaching experiment in real time
Terminate, obtain the leaching liquid containing soluble salt.
Compared with prior art, the present invention has following outstanding feature：
(1) present invention had both been avoided outer using dissolved oxygen in organic reducing agent acetoxime removal leaching reagent (distilled water)
Carry out Substances Pollution, also effectively prevent oxidation, the corrosion of shale minerals, greatly improved black shale soluble salt ions composition,
The accuracy of content measuring result；
(2) different using powdered rock sample (grain size is less than 1mm) from open method, the present invention is using arbitrary shape
Centimeter Level bulk sample, for the black shale of high solvable salt content, Centimeter Level bulk sample preparation process is simple, fast
Speed avoids the loss of soluble salt；
(3) present invention has taken into full account the characteristics of compactness shale nano-pore rate of water absorption is slow, soluble salt leaching time is long,
Therefore rational leaching time is determined by monitoring leaching liquid conductivity value, it is ensured that the complete leaching of black shale soluble salt
It takes.
Description of the drawings
Fig. 1 is the experimental provision schematic diagram of present invention leaching black shale soluble salt.
In figure：1- massive shale samples；2- has the container of sealing function；3- distilled water (or aqueous solution)；4- redox
Current potential (Eh) is counted；5- conductivity meters.
Specific embodiment
The present invention will be described in detail with embodiment below in conjunction with the accompanying drawings.
A kind of leaching method of black shale soluble salt, comprises the following steps successively：
(1) Sichuan Basin XX shale gas well black shales are chosen, arbitrary shape is quickly prepared under dry air environment
Centimeter Level massive shale sample 1；
(2) massive shale sample 1 is put into vacuum drying chamber, under temperature 60 C state, sample is dried, after weighing drying
Sample quality (40.05g)；
(3) distilled water 3 (400mL) of known volume is added in container 2, insertion oxidation-reduction potentiometer 4 monitors water body
Oxidation-reduction potential (Eh), and organic reducing agent acetoxime is continuously added into, until aqueous solution Eh values are less than -200mV；
(4) massive shale sample 1 is totally submerged in aqueous solution 3 after weighing, insertion oxidation-reduction potentiometer 4, conductance
Rate instrument 5, sealing container 2；
(5) aqueous solution Eh values are monitored during leaching experiment in real time, when Eh values are higher than -200mV, add in acetone again
Oxime makes aqueous solution Eh values be less than -200mV；
(6) aqueous solution electrical conductivity, when conductivity values are not further added by, leaching experiment are monitored during leaching experiment in real time
Terminate, obtain the leaching liquid containing soluble salt.
To verify effectiveness of the invention, a small amount of leaching liquid is taken, is utilized respectively ion chromatography (IC), inductively coupled plasma
Cl in constitution spectrum (ICP-MS) detection leaching liquid-、SO4 2-、HCO3 2-、Fe3+、Ca2+、Mg2+、Na+、K+Ion concentration utilizes this
The specific data of black shale soluble salt that invention leaching method obtains are shown in Table 1.
Black shale soluble salt ions content that table 1 is leached according to experimental method of the present invention (shale quality 40.05g,
Distill water consumption 400mL)
1 test result of table shows that the Main Anions of black shale soluble salt are Cl-, dominant cation Na+, containing a small amount of
Ca2+、Mg2+Ion, the ion concentration reflect that oxidation, corrosion do not occur for mineral.The result and shale gas well site fracturing outlet liquid
(aqueous solution after long period of soaking shale) ion concentration feature is similar.
Further to examine the reliability of the present invention, using China-styled Certain Industry Field standard SY/T5336-2006《Core analysis side
Method》, Chinese invention patent (102169115 A of publication number CN) soluble salt leaching method, utilize the black of above-mentioned identical coring depth
Color shale samples (40.84g), sample was ground to 60 mesh sieves (grain size is less than 250 microns), and distilled water 400mL is added (not remove
Oxygen, Eh values are more than 400mV) dissolving 1 day is impregnated, a small amount of leaching liquid is taken, analyzes soluble salt ions content, concrete outcome is shown in Table 2.
(shale quality 40.84g steams the black shale soluble salt ions content that table 2 is leached according to open experimental method
Distilled water dosage 400mL)
Anion is with SO in 2 test result of table4 2-Based on, cation is with Ca2+、Fe3+、Mg2+Based on, the result and shale gas
Well fracturing outlet liquid (aqueous solution after long period of soaking shale) ion characteristic difference is huge.Compared with table 1, SO in table 24 2-、Ca2+、
Fe3+、Mg2+It is seriously higher Deng 4 kinds of ion concentrations, it was confirmed that the oxidation of leaching process pyrite and carbonate mineral (CaCO3、
MgCa(CO3)2) acid corrosion, and Cl-、Na+Ion concentration significantly reduces, and possible cause is grinding, screening shale samples
When, the loss of shale soluble salt or distilled water immersion time are too short, and soluble salt is not sufficiently dissolved.
Contrast table 1, table 2 are as can be seen that of the invention it is possible to prevente effectively from oxidation, corrosion, and system occur for shale part mineral
Sample process will not cause soluble salt to lose, and pass through and monitor leaching liquid conductivity value and be reasonably determined leaching time, it is ensured that black
The complete leaching of color shale soluble salt.
Above specific embodiment has been combined drawings and examples and the method for the present invention is described in detail, but
It is the invention is not limited in above-mentioned specific embodiment, above-mentioned specific embodiment is only schematical, is not
It is restricted, those of ordinary skill in the art under the enlightenment of the present invention, if in the main scope without departing from the present invention,
Experiment condition and object can flexibly be changed, within these are all belonged to the scope of protection of the present invention.
Claims (1)
1. a kind of leaching method of black shale soluble salt, comprises the following steps successively：
(1) not contaminated, not oxidized black shale is chosen, centimetre of arbitrary shape is quickly prepared under dry air environment
Grade massive shale sample；
(2) massive shale sample is put into vacuum drying chamber, under temperature 60 C state, dries sample, weigh sample after drying
Quality；
(3) distilled water is added in container, oxidation-reduction potentiometer, monitoring water body oxidation-reduction potential (Eh) is inserted into, and continues
Organic reducing agent acetoxime is added in, until aqueous solution Eh values are less than -200mV；
(4) massive shale sample is totally submerged in step (3) aqueous solution after weighing, insertion oxidation-reduction potentiometer, conductance
Rate instrument, sealing container；
(5) aqueous solution Eh values are monitored during leaching experiment in real time, when Eh values are higher than -200mV, acetoxime are added in again, makes
Aqueous solution Eh values are less than -200mV；
(6) aqueous solution electrical conductivity, when conductivity values are not further added by, leaching experiment knot are monitored during leaching experiment in real time
Beam obtains the leaching liquid containing soluble salt.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109944588A (en) * | 2019-03-19 | 2019-06-28 | 西南石油大学 | High porosity reservoir containing soluble salt protects drilling fluid composition optimization method |
| CN110132678A (en) * | 2019-06-03 | 2019-08-16 | 西南石油大学 | Oxygen-sensitive oil and gas reservoir rock core flowing experiment sample pretreating method |
| CN115059460A (en) * | 2022-07-14 | 2022-09-16 | 重庆大学 | Method for reducing self-water-absorbing capacity of hydraulic fracturing shale reservoir |
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| CN109944588A (en) * | 2019-03-19 | 2019-06-28 | 西南石油大学 | High porosity reservoir containing soluble salt protects drilling fluid composition optimization method |
| CN110132678A (en) * | 2019-06-03 | 2019-08-16 | 西南石油大学 | Oxygen-sensitive oil and gas reservoir rock core flowing experiment sample pretreating method |
| CN115059460A (en) * | 2022-07-14 | 2022-09-16 | 重庆大学 | Method for reducing self-water-absorbing capacity of hydraulic fracturing shale reservoir |
| CN115059460B (en) * | 2022-07-14 | 2024-05-03 | 重庆大学 | Method for reducing self-water absorption of hydraulically fractured shale reservoir |
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