CN109142135A - A method of the salinity of measurement shale pore water - Google Patents
A method of the salinity of measurement shale pore water Download PDFInfo
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- CN109142135A CN109142135A CN201811152405.1A CN201811152405A CN109142135A CN 109142135 A CN109142135 A CN 109142135A CN 201811152405 A CN201811152405 A CN 201811152405A CN 109142135 A CN109142135 A CN 109142135A
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- 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
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
- G01N5/045—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder for determining moisture content
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/96—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation using ion-exchange
Abstract
The invention discloses a kind of methods of salinity for measuring shale pore water, the specific steps are as follows: G1. acquires fresh shale core as shale samples first；G2. the hole water in ready shale samples is measured；G3. the dissolved matter of shale samples pore water is then extracted, and obtains the aqueous solution of dissolved matter；G4. the ion concentration in aqueous solution is detected, and the original salinity C of the shale pore water is calculatedWater.The present invention provide it is a kind of fast and accurately must measure the method that hole water quality carries out subsequent salinity calculating again for the problem that shale carries out drying weighing, overcome in the prior art because of the poor reason of shale permeability and can not direct displacement go out pore water.It simultaneously also avoids that water sample can not be extracted using the microanalysis such as electron probe technology, or directly measures the problem that shale samples porosity causes measured value not accurate, thus more convenient hole water salinity for efficiently and accurately obtaining shale samples.
Description
Technical field
The invention belongs to shale gas exploitation technical fields, and in particular to this area's shale is investigated before a kind of exploitation shale gas
The method of hole water salinity.
Background technique
Shale gas is the natural gas resource contained in rammell for exploitation, and Chinese shale gas recoverable reserves is larger.Page
The formation and enrichment of rock gas have the characteristics that itself uniqueness, are often distributed in that thickness in basin is larger, widespread shale hydrocarbon source
In rock stratum.Compared with conventional natural gas, shale gas exploitation has the advantages that production life of well is long and the production cycle is long, most of to produce
Shale gas has a very wide distribution, thickness is big, and universal gassiness, this enables shale gas well chronically to produce gas with stable rate.
Shale gas refer to preservation in rich organic matter mud shale and its interlayer, with absorption and free state be main existing way very
Advise natural gas, ingredient is a kind of cleaning, efficient energy resources and industrial chemicals based on methane, be mainly used for resident's combustion gas,
City heat supply, power generation, motor vehicle fuel and Chemical Manufacture etc., it is widely used.Generally without draining, production in shale gas production process
Period is long, and generally -50 years 30 years, exploration and development success rate was high, industrial economy value with higher.
The exploitation of unconventional gas reservoir is the Disciplinary Frontiers of current oil-gas reservoir exploitation, and reserves are much larger than conventional gas.?
In unconventional gas reservoir, shale gas is the focal point of oil and gas development in recent years.As shown in Figure 1, the shale reservoir can be divided into bone
Frame and hole two parts.Skeleton includes: that non-clay mineral (quartz, carbonate mineral etc.) and dry clay and kerogen etc. have
Machine matter.Contain in hole: free gas, capillary and clay-bound water.Hydrone in blowhole is that a kind of charge is incomplete
The polar molecule of balance.Since dry clay particle surface has negative electrical charge, attract polar water molecules by electrostatic attraction, thus viscous
Native surface forms water membrane, referred to as clay-bound water.A large amount of exchangeable cations are had accumulated in clay-bound water, but are free of
Anion, poorly conductive.Apart from surface of clay remote position in hole, water is not influenced by surface of clay negative electrical charge, tool
There are high conductivity, referred to as far water.Far water is by the constraint of capillary force, alternatively referred to as hollow billet irreducible water.Hollow billet irreducible water is in fine pore
In be full of hole, or in macrovoid in the form of moisture film preservation in hole wall.
Shale pore water is the hollow billet irreducible water referred generally in active porosity, wherein the inorganic salts member dissolved be known as Ca2+,
Mg2+, Na+, K+, Cl- etc..The salinity of shale pore water refers to that the summation of various Mineral Concentrations in hollow billet irreducible water is (single
Position: mg/litre), also referred to as water flooding salt content.Shale pore water salinity with higher.In the drilling well of shale gas reservoir
In Completion Operations, if working fluid salinity be less than shale pore water salinity (that is: the activity of working fluid be greater than shale hole
The activity of gap water), water activity difference caused by pressure difference under the influence of invade shale.After water in working fluid immerses shale hole,
The effective stress of shale is reduced, and the mechanical property of shale can also change a lot, and is also easy to produce damage under external force.When
It after the structural intergrity of mud page is destroyed, will cause the accidents such as hole collapse, endanger underground work safety.Therefore, page is accurately analyzed
The salinity of rock pore water, for ensureing that the safety work of shale gas well has great importance.
The combined influence that liquid drains is taken by compacting draining, hydrocarbon and vaporization, ultralow rich in foring in gas shale reservoir
Water saturation phenomenon.As shown in Fig. 2, Fig. 2 is the porosity type indicated in shale reservoir.With conventional sandstone or carbonate rock
Hole is different: shale contains a large amount of semi-connected hole and dead-end pore；Some hole is nanoscale hole in shale
(< 750nm), pore diameter is small.Therefore the pore water in shale cannot flow.According to domestic and international existing shale gas reservoir rock core
The test result of (coring under the conditions of oil-base mud), it was confirmed that although the initial water saturation of shale reservoir is high, be less than
The critical water saturation of reservoir.This is also the reason of shale gas production well only produces gas, do not produce water flooding in recovery process.
Because shale pore water under formation conditions cannot flow, it is unable to tripping in formation tester and obtains in stratum
Water sample.In laboratory, the sample of pore water can not be obtained from shale samples using displacement process.On the other hand, shale
Pore-size very little, by the interference of rock matrix mineral, with Microbeam Analysis Techniques such as electron probes, it is also difficult to direct drawing holes
Gap water, can not its analysis salinity.
Two kinds of prior arts presented below, wherein application benefit number is sought for one kind of CN201010612091.6 by rock core
In the method for formation water salinity, after needing rock core to dry, then using the pore volume of rock core magnetic nuclear resonance method acquisition rock core.
It is different from the hole of conventional sandstone or carbonate rock, a large amount of organic hole is contained in the kerogen of shale.In having for shale
In machine hole, only free gas, not fissure water.The method of this saturation distilled water can excessively measure the body of shale pore water
Product.On the other hand, magnetic nuclear resonance method it is measured directly be polarization after nuclear magnetic signal, be not pore volume.Nuclear magnetic signal
When being converted into pore volume, there is also certain errors.Therefore, this method is not suitable for shale.
Another passes through measurement application No. is in a kind of method of measurement formation water salinity of CN201510423168.8
Chloride content in rock sample, further calculates formation water salinity.This method mainly includes five steps: grinding, washes
Oil processing plus distilled water stirring and dissolving salinity, calculate salinity at the chloride ion content in survey solution.In the washing oil of this method
In processing, the asphalitine ingredient in shale can be removed, the excessive porosity for measuring shale.In the formation water salinity of this method
In calculating, two porosity φ, rock sample grain density ρ key parameters are needed.Since a part of hole of shale is nano grade pore
Gap (< 750nm), shale contain a large amount of semi-connected hole and dead-end pore, are difficult accurately to measure porosity.The skeleton mine of shale
Object complicated component typically contains quartz, carbonate mineral, clay mineral (illite, kaolinite etc.), is difficult accurately to estimate rock sample
Grain density.On the other hand, classified according to the Su Lin of water flooding, there are four types of water type altogether: chloride-calcium type, heavy carbonic sodium form, chlorination
Magnesium types, sodium sulfate type.This method only measures the chloride content in core sample, is not particularly suited for all stratum water type.Cause
This, this method is not suitable for shale.
In conclusion the water sample in shale hole can not be directly extracted in the existing analysis of oil and gas industry,
The salinity of pore water cannot directly be tested.Since the measurement error of the parameters such as shale porosity, skeletal density is big, value is tired
Difficulty, existing rock core method can not accurately analyze the salinity of shale pore water.
Summary of the invention
Salinity detection difficulty in order to solve the problems, such as the above-mentioned pore water of shale in the prior art is big, and the present invention provides one
Kind, which carries out drying weighing for shale, must fast and accurately measure the method that hole water quality carries out subsequent salinity calculating again.
The technical scheme adopted by the invention is as follows: a method of the salinity of measurement shale pore water, specific steps are such as
Under:
G1. fresh shale core is acquired first as shale samples；
G2. the hole water in ready shale samples is measured；
G3. the dissolved matter of shale samples pore water is then extracted, and obtains the aqueous solution of dissolved matter；
G4. the ion concentration in aqueous solution is detected, and is calculated to obtain the original mine of the shale pore water according to hole watermeter
Change degree CWater。
Further, specific step is as follows by the step G2:
(2.1) first ready shale samples are crushed, then claim its quality and is recorded as M1；
(2.2) the crushing shale samples after then crushing weighing are placed in the drying equipment of constant temperature and humidity and dry,
Claim its quality when quality is stablized and is recorded as M2；
(2.3) it is calculated by the following formula to obtain the pore water water content of the shale samples:
MWater=M1-M2
In formula: MWaterFor the quality of shale samples pore water, M1For the quality of shale samples before drying, and M2After drying
Shale samples quality.
Further, specific step is as follows by the step G3:
(3.1) the crushing shale samples after drying are added in distilled water, stirring forms mud mixture and stands；
(3.2) mud mixture after standing is obtained by filtration to the aqueous solution of ion.
Further, specific step is as follows by the step G3:
(3.1) weighing quality is M3Distilled water, ready shale samples are crushed and are dried, and to the powder after drying
It is M that quality, which is added, in broken shale samples3Distilled water in, and stir form mud mixture and stand；
(3.2) mud mixture after standing is obtained by filtration to the aqueous solution of ion.
Further, specific step is as follows by the step G4:
(4.1) the single ion concentration in deionized water solution obtained in step G3 is measured, and obtain it is each from
The content value C of sonSurvey i, the CSurvey iFor i ion deionized water solution content value；
(4.2) according to the C of measurementSurvey iTo calculate content value C of the i ion in the shale samples pore waterWater i, calculation formula
It is as follows:
CWater i=CSurvey i×M3/MWater
In formula: the MWaterQuality for the pore water measured in step (2.3)；
(4.3) finally the content value according to each ion in the shale samples pore water calculates total original salinity
CWater, calculation formula is as follows:
In formula: CWaterFor the total salinity of shale samples pore water；N is the ionic type number of shale samples pore water
Mesh.
Further, shale samples are crushed to 100 mesh as crushing shale samples in the step (2.1).
Further, it is being greater than 100 DEG C wherein will crush in shale samples merging climatic chamber and is being less than shale reservoir
Formation temperature under conditions of be dried to quality and stablize, weighed every 2h taking-up when drying, when crushing shale samples quality
The quality and baking of poor quality for being less than preset value and being determined as that quality is stable and stops drying, and weighs with this weighed compared with last time
Content value of the absolute value of the difference of the crushing shale samples quality weighed before dry as the shale samples pore water.
Further, in the step (3.1) quality of increased distilled water be drying after crushing shale samples quality
9-11 times.
Further, the cations in deionized water solution are measured using inductance coupling in the step (3.3)
Plasma atomic emission spectrometry measurement is closed, then using the anion-content in ion-chromatographic determination deionized water solution.
Further, every batch of shale samples prepare 3-5 detection group, and repeat detection 5-10 times to each detection group, will
The original salinity of all pore waters of every batch of shale samples is averaged to obtain the original of the average pore water of each shale samples
Beginning salinity.
The invention has the benefit that
Broken sample is made by acquiring fresh shale core in the present invention, is extracted using drying-crystallization-redissolution method
In shale hole after the inorganic salts of water, salinity is detected.It can not only obtain accurate shale hole water salinity, overcome simultaneously
The problem of in the prior art pore water can not being directly obtained because of the poor reason of shale permeability.It is extracted by this method
Shale hole water sample is detected, and also avoids that water sample or directly measurement can not be extracted using the microanalysis such as electron probe technology
The problem that rock sample porosity causes measured value not accurate, thus more convenient hole for efficiently and accurately obtaining shale samples
Gap water salinity.
Detailed description of the invention
Fig. 1 is in background of invention for illustrating the schematic diagram of pore water occurrence status.
Fig. 2 is in background of invention for illustrating the schematic diagram of porosity type in shale reservoir rock.
Specific embodiment
Embodiment:
The present embodiment be it is a kind of for detecting shale gas exploitation when corresponding region in shale pore water salinity measurement
Method, using crushing-weighing-drying-weighing method metering rock sample pore water quality；Drying-crystallization-redissolution is used again
Method extract shale pore water inorganic salts, test salinity, the salinity of water flooding in shale hole can be calculated.By
In parameters such as porosity, the skeletal densities for not needing measurement shale, computational accuracy is improved, testing cost is reduced.
Specific step is as follows:
Prepare shale samples first, the shale samples are fresh shale core, the rock core of sample preparation 3-5 block piston-shaped
Sample is for detection.
Then the hole water content in ready shale samples is measured, ready shale samples are crushed, are then claimed
Its quality is simultaneously recorded as M1；Then the crushing shale samples after weighing will be crushed and be placed in the drying equipment of constant temperature and humidity and dried
It is dry, claim its quality when quality is stablized and is recorded as M2。
It is calculated by the following formula to obtain the pore water water content of the shale samples:
MWater=M1-M2
In formula: MWaterFor the quality of shale samples pore water, M1For the quality of shale samples before drying, and M2After drying
Shale samples quality.
As shown in Fig. 2, hole includes: interconnected pore, semi-connected hole and dead-end pore in shale.The purpose of sample comminution
Be: semi-connected hole and dead-end pore are broken and open, and can more extract the inorganic salts in hole.The selection of broken sample partial size
Be a key point: the size of broken sample is smaller, and evaporation pore water is easier when drying and inorganic salts are precipitated.But if shale
Broken sample it is undersized, clay mineral grain in shale is easy to form colloid in water, influences subsequent filtering, and interfere
The hydrochemical analyse of solution.Shale samples can be crushed and obtain crushing shale sample after sieving with 100 mesh sieve screening by summary factor
Product.
It is mainly hole by the moisture evaporated after drying because the moisture being present in shale samples is mainly pore water
Water, thus by for a long time drying so that pore water evaporation completely, obtained from it is of poor quality be pore water quality.
Further, wherein the drying (range of temperature are as follows: be greater than 100 in shale samples merging climatic chamber will be crushed
DEG C, less than the formation temperature of shale reservoir) stablize to quality, it is weighed every 2h taking-up when drying, when crushing shale samples
The quality of poor quality for being less than preset value and being determined as that quality is stable and stops drying, and weighs with this that quality was weighed compared with last time
With content value of the absolute value as the shale samples pore water of the difference of the crushing shale samples quality weighed before drying.
The purpose of drying shale samples is: the hollow billet irreducible water in evaporation hole.In the drying course of shale, temperature
Selection is a key point, it may be assumed that cannot cause organic cracking, can not remove clay-bound water (that is: cannot destroy shale
Clay mineral in sample), it can just guarantee that the evaporation of shale pore water is to cause the mass change of the shale of drying front and back in this way
Sole cause.According to the law of indestructibility of matter, the quality difference for drying the shale of front and back is equal to the quality of shale pore water.Using
Precision is that the electronic balance of 0.01mg can meet test volume requirement.
The temperature of the rapid zone of transformation of the second of montmorillonite (S layers ± 20%) is 110-140 DEG C.Illite/smectite mixed layer disappearance zone (she
Sharp stone band) temperature be 170-200 DEG C.The shale gas reservoir of China is typically in mature-high stage of ripeness.Such as: the Sichuan Basin
Lower Jurassic Series gravity flow well group is mainly black shale rich in machine matter shale, and organic matter thermal maturity value is 0.9%-1.6%, is in
In the A2 stage of altricial rock, montmorillonite and illite/smectite mixed layer content are few, and formation temperature is greater than 110 DEG C.In this patent application, propose
The range of the drying temperature of shale samples are as follows: be greater than 100 DEG C, less than the formation temperature of shale reservoir.In this temperature range,
Pore water can effectively be evaporated and inorganic salts are precipitated, but not the organic matter in rock sample is caused to crack, also do not allow to easily cause
The evaporation loss of clay-bound water.
Then, the dissolved matter of shale samples pore water is extracted, and obtains the aqueous solution of dissolved matter；The step (3.1)
In the quality of increased distilled water be crushing 10 times of shale samples quality after drying.Add to the crushing shale samples after drying
Entering quality is M3Distilled water and stirring form mud mixture and stand.By the mud mixture after standing be obtained by filtration from
Sub- aqueous solution.Then the single ion concentration in deionized water solution is measured, and obtains the content value C of each ionSurvey i,
The CSurvey iFor i ion deionized water solution content value；According to the C of measurementSurvey iTo calculate i ion in the shale samples pore water
In content value CWater i, calculation formula is as follows:
CWater i=CSurvey i×M3/MWater
In formula: the MWaterQuality for the pore water measured in step (2.3).
It finally detects the ion concentration in aqueous solution and the salinity of the shale pore water is calculated.
Wherein, the cations in deionized water solution are measured using inductively coupled plasma body atomic emissions light
Spectrometry measurement, then using the anion-content in ion-chromatographic determination deionized water solution.
And total salinity CWaterCalculation formula it is as follows:
In formula: CWaterFor the total salinity of shale samples pore water；N is the ionic type number of shale samples pore water
Mesh.All hole water salinities of every batch of shale samples are averaged to obtain the average pore water mineralising of each shale samples
Degree.
The present invention is not limited to above-mentioned optional embodiment, anyone can show that other are each under the inspiration of the present invention
The product of kind form.Above-mentioned specific embodiment should not be understood the limitation of pairs of protection scope of the present invention, protection of the invention
Range should be subject to be defined in claims, and specification can be used for interpreting the claims.
Claims (10)
1. a kind of method for the salinity for measuring shale pore water, it is characterised in that: specific step is as follows:
G1. fresh shale core is acquired first as shale samples；
G2. the hole water in ready shale samples is measured；
G3. the dissolved matter of shale samples pore water is then extracted, and obtains the aqueous solution of dissolved matter；
G4. the ion concentration in aqueous solution is detected, and is calculated to obtain the original salinity of the shale pore water according to hole watermeter
CWater。
2. a kind of method of salinity for measuring shale pore water according to claim 1, it is characterised in that: the step
Specific step is as follows by G2:
(2.1) first ready shale samples are crushed, then claim its quality and is recorded as M1；
(2.2) the crushing shale samples after then crushing weighing are placed in the drying equipment of constant temperature and humidity and dry, until
Quality claims its quality and is recorded as M when stablizing2；
(2.3) it is calculated by the following formula to obtain the pore water water content of the shale samples:
MWater=M1-M2
In formula: MWaterFor the quality of shale samples pore water, M1For the quality of shale samples before drying, and M2For the page after drying
The quality of rock sample product.
3. a kind of method of salinity for measuring shale pore water according to claim 2, it is characterised in that: the step
Specific step is as follows by G3:
(3.1) quality is added in the crushing shale samples after drying is M3Distilled water in, stirring forms mud mixture and quiet
It sets；
(3.2) mud mixture after standing is obtained by filtration to the aqueous solution of ion.
4. a kind of method of salinity for measuring shale pore water according to claim 1, it is characterised in that: the step
Specific step is as follows by G3:
(3.1) ready shale samples are crushed and is dried, and it is M that quality, which is added, to the crushing shale samples after drying3Steaming
In distilled water, and stirs and form mud mixture and stand；
(3.2) mud mixture after standing is obtained by filtration to the aqueous solution of ion.
5. a kind of method of salinity for measuring shale pore water according to claim 3 or 4, it is characterised in that: described
Specific step is as follows by step G4:
(4.1) the single ion concentration in deionized water solution obtained in step G3 is measured, and obtains each ion
Content value CSurvey i, the CSurvey iFor i ion deionized water solution content value；
(4.2) according to the C of measurementSurvey iTo calculate content value C of the i ion in the shale samples pore waterWater i, calculation formula is as follows:
CWater i=CSurvey i×M3/MWater
In formula: the MWaterQuality for the pore water measured in step (2.3)；
(4.3) finally the content value according to each ion in the shale samples pore water calculates total original salinity CWater, meter
It is as follows to calculate formula:
In formula: CWaterFor the total salinity of shale samples pore water；N is the ionic type number of shale samples pore water.
6. a kind of method of salinity for measuring shale pore water according to claim 2 or 4, it is characterised in that: described
Shale samples are crushed to 100 mesh as crushing shale samples in step (2.1).
7. a kind of method of salinity for measuring shale pore water according to claim 2 or 4, it is characterised in that: wherein
It will crush and dried under conditions of being greater than 100 DEG C and being less than the formation temperature of shale reservoir in shale samples merging climatic chamber
Stablize to quality, weighed every 2h taking-up when drying, when crushing shale samples quality compared with of poor quality being less than of weighing last time
Preset value is determined as that quality is stable and stops drying, and the crushing shale samples weighed before the quality and drying weighed with this
Content value of the absolute value of the difference of quality as the shale samples pore water.
8. a kind of method of salinity for measuring shale pore water according to claim 3 or 4, it is characterised in that: described
The quality of increased distilled water is 9-11 times of the crushing shale samples quality after drying in step (3.1).
9. a kind of method of salinity for measuring shale pore water according to claim 3 or 4, it is characterised in that: described
Step is measured using inductively coupled plasma atomic emission spectrum the cations in deionized water solution in (3.3)
Method measurement, then using the anion-content in ion-chromatographic determination deionized water solution.
10. a kind of method of salinity for measuring shale pore water according to claim 1-4, feature exist
In: every batch of shale samples prepare 3-5 detection group, and repeat detection 5-10 times to each detection group, by every batch of shale samples
The original salinity of all pore waters is averaged to obtain the original salinity of the average pore water of each shale samples.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111852465A (en) * | 2020-08-27 | 2020-10-30 | 中国石油大学(华东) | Method for evaluating original water content of shale reservoir core obtained by water-based mud drilling |
| CN114368844A (en) * | 2021-12-15 | 2022-04-19 | 庆阳新庄煤业有限公司新庄煤矿 | Data monitoring method and device for high-salinity mine water treatment |
| CN114778796A (en) * | 2022-04-02 | 2022-07-22 | 江苏省地质调查研究院 | Method for deducing pore water chemical components of weakly permeable layer |
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