CN106644875A - Shale capillary pressure and water saturation measurement method - Google Patents

Shale capillary pressure and water saturation measurement method Download PDF

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Publication number
CN106644875A
CN106644875A CN201610887320.2A CN201610887320A CN106644875A CN 106644875 A CN106644875 A CN 106644875A CN 201610887320 A CN201610887320 A CN 201610887320A CN 106644875 A CN106644875 A CN 106644875A
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quality
shale samples
saturation
wide
glassware
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沈伟军
鲁晓兵
李熙喆
张旭辉
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Institute of Mechanics of CAS
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Institute of Mechanics of CAS
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Priority to CN201610887320.2A priority Critical patent/CN106644875A/en
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/08Investigating permeability, pore-volume, or surface area of porous materials
    • G01N15/088Investigating volume, surface area, size or distribution of pores; Porosimetry
    • G01N15/0893Investigating volume, surface area, size or distribution of pores; Porosimetry by measuring weight or volume of sorbed fluid, e.g. B.E.T. method
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/08Investigating permeability, pore-volume, or surface area of porous materials
    • G01N15/082Investigating permeability by forcing a fluid through a sample
    • G01N15/0826Investigating permeability by forcing a fluid through a sample and measuring fluid flow rate, i.e. permeation rate or pressure change
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N5/00Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
    • G01N5/02Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by absorbing or adsorbing components of a material and determining change of weight of the adsorbent, e.g. determining moisture content
    • G01N5/025Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by absorbing or adsorbing components of a material and determining change of weight of the adsorbent, e.g. determining moisture content for determining moisture content
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/08Investigating permeability, pore-volume, or surface area of porous materials
    • G01N2015/0866Sorption

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  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Biochemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Dispersion Chemistry (AREA)
  • Fluid Mechanics (AREA)
  • Drying Of Solid Materials (AREA)

Abstract

The invention discloses a shale capillary pressure and water saturation measurement method. The method includes the steps of shale sample grinding, drying, cooling, moisture adsorption by a saline solution, desorption by a saline solution and measurement. The shale capillary pressure and water saturation measurement method can be used for pore structure studies and determination of porosity, relative permeability, shale wettability and irreducible water saturation of shale reservoir strata, and has extensive application value in terms of reservoir stratum performance evaluation and reserve calculation of shale. Measuring a relationship curve between capillary pressure and water saturation of the shale is of great significance to efficient development and utilization of unconventional shale gas resources.

Description

A kind of shale capillary pressure and water saturation measuring method
Technical field
The invention belongs to natural oil gas development technology field, more particularly to a kind of shale capillary pressure and water saturation Measuring method.
Background technology
With increase of the World Economics to petroleum resources demand, the exploitation of unconventional shale gas resource are extensively closed Note, progressively becomes the strategic supplement of conventional gas and oil resources development and utilization.Shale capillary pressure and saturation degree relation, are shale gas An important relationship curve in exploitation is hidden, can be used for the aspects such as evaluating reservoir, the reserves calculating of shale.It is usually used at present determining The method of rock capillary pressure curve mainly has:Semi-permeable plate method, centrifugal process and mercury injection method.What baffle method and centrifugal process were measured Highest capillary pressure is typically confined within 1000psi, and for hypotonic fine and close shale, pressure is still too low;Mercury injection method Required pressure (usual scope is in 5000~10 000psi) can be reached, but the hollow billet that converts is gone using non-reservoir fluid, condition Pressure can produce incorrect result, and can be bigger for the shale deviation containing clay.At present, for correct measurement shale hollow billet Research in terms of pressure extremely lacks, and research is set up a kind of measurement experimental provision and method of shale capillary pressure and seems and have very much It is necessary.
The content of the invention
The purpose of the present invention is:The measuring method of a kind of shale capillary pressure and water saturation is provided, shale is realized The measurement of the relation curve of particle capillary pressure and water saturation, for the exploitation of unconventional shale gas resource have weight Want meaning.
The technical scheme is that:The measuring method of a kind of shale capillary pressure and water saturation, including following step Suddenly:
A. shale samples are ground into the shale samples particle of different-grain diameter in 250 μm~800 μ ms;
B. shale samples particle is loaded into wide-mouth bottle;
C. will be equipped with the wide-mouth bottle of shale samples particle carries out 110 DEG C of drying in 24 hours;
D. by drying after the wide-mouth bottle equipped with shale samples particle be positioned over bottom equipped with drier glassware in It is cooled to room temperature;
E. the wide-mouth bottle that will be equipped with shale samples particle takes out from glassware of the bottom equipped with drier, claims its quality Afterwards, in being positioned over glassware of the bottom equipped with saturation LiCl salting liquid;
F. glassware of the bottom equipped with saturation LiCl salting liquid that placed the wide-mouth bottle of shale samples particle is put into In 50 DEG C of insulating box, the wide-mouth bottle equipped with shale samples particle was taken out from insulating box per 24 hours, its quality is claimed respectively;When When claiming the result of its quality to tend to fixed value daily, shale samples particle capillary pressure reaches balance, by shale samples particle Wide-mouth bottle from bottom equipped with saturation LiCl salting liquid glassware in take out, be placed on drying baker carry out 24 hours 110 DEG C Drying, after drying, claims its quality;
G. will from bottom equipped with saturation LiCl salting liquid glassware in take out, and dry claim its quality after equipped with page The wide-mouth bottle of rock sample particle, is positioned over bottom equipped with saturation MgCl2In the glassware of salting liquid, 50 DEG C of perseverance is then placed in In incubator, the wide-mouth bottle equipped with shale samples particle was taken out from insulating box per 24 hours, its quality is claimed respectively;Claim it when daily When the result of quality tends to fixed value, shale samples particle capillary pressure reaches balance, will be equipped with the wide of shale samples particle Mouth bottle is equipped with saturation MgCl from bottom2Take out in the glassware of salting liquid, being placed on drying baker carries out 110 DEG C of bakings in 24 hours It is dry, after drying, claim its quality;
H. saturation MgCl will be housed from bottom2In the glassware of salting liquid take out, and dry claim its quality after being equipped with The wide-mouth bottle of shale samples particle, in being positioned over glassware of the bottom equipped with saturation NaBr salting liquid, is then placed in 50 DEG C In insulating box, the wide-mouth bottle equipped with shale samples particle was taken out from insulating box per 24 hours, its quality is claimed respectively;Claim when daily When the result of its quality tends to fixed value, shale samples particle capillary pressure reaches balance, will be equipped with shale samples particle Wide-mouth bottle takes out from glassware of the bottom equipped with saturation NaBr salting liquid, and being placed on drying baker carries out 110 DEG C of bakings in 24 hours It is dry, after drying, claim its quality;
I. will from bottom equipped with saturation NaBr salting liquid glassware in take out, and dry claim its quality after equipped with page The wide-mouth bottle of rock sample particle, is positioned over bottom equipped with saturation NaNO3In the glassware of salting liquid, 50 DEG C of perseverance is then placed in In incubator, the wide-mouth bottle equipped with shale samples particle was taken out from insulating box per 24 hours, its quality is claimed respectively;Claim it when daily When the result of quality tends to fixed value, shale samples particle capillary pressure reaches balance, will be equipped with the wide of shale samples particle Mouth bottle is equipped with saturation NaNO from bottom3Take out in the glassware of salting liquid, being placed on drying baker carries out 110 DEG C of bakings in 24 hours It is dry, after drying, claim its quality;
J. saturation NaNO will be housed from bottom3In the glassware of salting liquid take out, and dry claim its quality after being equipped with The wide-mouth bottle of shale samples particle, in being positioned over glassware of the bottom equipped with saturation KCl salting liquid, is then placed in 50 DEG C of perseverance In incubator, the wide-mouth bottle equipped with shale samples particle was taken out from insulating box per 24 hours, its quality is claimed respectively;Claim it when daily When the result of quality tends to fixed value, shale samples particle capillary pressure reaches balance, will be equipped with the wide of shale samples particle Mouth bottle takes out from glassware of the bottom equipped with saturation KCl salting liquid, and being placed on drying baker carries out 110 DEG C of drying in 24 hours, After drying, claim its quality;
K. will from bottom equipped with saturation KCl salting liquid glassware in take out, and dry claim its quality after equipped with page The wide-mouth bottle of rock sample particle, is positioned over bottom equipped with saturation KNO3In the glassware of salting liquid, 50 DEG C of perseverance is then placed in In incubator, the wide-mouth bottle equipped with shale samples particle was taken out from insulating box per 24 hours, its quality is claimed respectively;Claim it when daily When the result of quality tends to fixed value, shale samples particle capillary pressure reaches balance, will be equipped with the wide of shale samples particle Mouth bottle is equipped with saturation KNO from bottom3Take out in the glassware of salting liquid, being placed on drying baker carries out 110 DEG C of drying in 24 hours, After drying, claim its quality;
L. saturation KNO will be housed from bottom3In the glassware of salting liquid take out, and dry claim its quality after equipped with page The wide-mouth bottle of rock sample particle, is positioned over bottom equipped with saturation K2SO4In the glassware of salting liquid, 50 DEG C of perseverance is then placed in In incubator, the wide-mouth bottle equipped with shale samples particle was taken out from insulating box per 24 hours, its quality is claimed respectively;Claim it when daily When the result of quality tends to fixed value, shale samples particle capillary pressure reaches balance, will be equipped with the wide of shale samples particle Mouth bottle is equipped with saturation K from bottom2SO4Take out in the glassware of salting liquid, being placed on drying baker carries out 110 DEG C of drying in 24 hours, After drying, claim its quality;
M. saturation K will be housed from bottom2Take out in the glassware of SO salting liquids, will be equipped with the wide-mouth of shale samples particle Bottle is positioned over bottom equipped with saturation KNO3In the glassware of salting liquid, in being then placed in 50 DEG C of insulating box, per 24 hours from The wide-mouth bottle equipped with shale samples particle is taken out in insulating box, its quality is claimed respectively;When the result for claiming its quality daily tends to solid During definite value, shale samples particle water vapor desorption reaches balance, will be equipped with the wide-mouth bottle of shale samples particle from bottom equipped with full And KNO3Take out in the glassware of salting liquid, being placed on drying baker carries out 110 DEG C of drying in 24 hours, after drying, claims its quality;
N. saturation KNO will be housed from bottom3Take out in the glassware of salting liquid, will be equipped with the wide-mouth of shale samples particle Bottle is positioned in glassware of the bottom equipped with saturation KCl salting liquid, in being then placed in 50 DEG C of insulating box, per 24 hours from perseverance The wide-mouth bottle equipped with shale samples particle is taken out in incubator, its quality is claimed respectively;When the result for claiming its quality daily tends to fixed During value, shale samples particle water vapor desorption reaches balance, and the wide-mouth bottle that will be equipped with shale samples particle is equipped with saturation from bottom Take out in the glassware of KCl salting liquids, being placed on drying baker carries out 110 DEG C of drying in 24 hours, after drying, claims its quality;
O. will take out from glassware of the bottom equipped with saturation KCl salting liquid, will be equipped with the wide-mouth of shale samples particle Bottle is positioned over bottom equipped with saturation NaNO3In the glassware of salting liquid, in being then placed in 50 DEG C of insulating box, per 24 hours from The wide-mouth bottle equipped with shale samples particle is taken out in insulating box, its quality is claimed respectively;When the result for claiming its quality daily tends to solid During definite value, shale samples particle water vapor desorption reaches balance, will be equipped with the wide-mouth bottle of shale samples particle from bottom equipped with full And NaNO3Take out in the glassware of salting liquid, being placed on drying baker carries out 110 DEG C of drying in 24 hours, after drying, claims its matter Amount;
P. saturation NaNO will be housed from bottom3Take out in the glassware of salting liquid, will be equipped with the wide of shale samples particle Mouth bottle is positioned in glassware of the bottom equipped with saturation NaBr salting liquid, in being then placed in 50 DEG C of insulating box, per 24 hours The wide-mouth bottle equipped with shale samples particle is taken out from insulating box, its quality is claimed respectively;Tend to when the result of its quality is claimed daily During fixed value, shale samples particle water vapor desorption reaches balance, and the wide-mouth bottle that will be equipped with shale samples particle is equipped with from bottom Take out in the glassware of saturation NaBr salting liquid, being placed on drying baker carries out 110 DEG C of drying in 24 hours, after drying, claims its matter Amount;
Q. will take out from glassware of the bottom equipped with saturation NaBr salting liquid, will be equipped with the wide-mouth of shale samples particle Bottle is positioned over bottom equipped with saturation MgCl2In the glassware of salting liquid, in being then placed in 50 DEG C of insulating box, per 24 hours from The wide-mouth bottle equipped with shale samples particle is taken out in insulating box, its quality is claimed respectively;When the result for claiming its quality daily tends to solid During definite value, shale samples particle water vapor desorption reaches balance, will be equipped with the wide-mouth bottle of shale samples particle from bottom equipped with full And MgCl2Take out in the glassware of salting liquid, being placed on drying baker carries out 110 DEG C of drying in 24 hours, after drying, claims its matter Amount;
R. saturation MgCl will be housed from bottom2Take out in the glassware of salting liquid, will be equipped with the wide of shale samples particle Mouth bottle is positioned in glassware of the bottom equipped with saturation LiCl salting liquid, in being then placed in 50 DEG C of insulating box, per 24 hours The wide-mouth bottle equipped with shale samples particle is taken out from insulating box, its quality is claimed respectively;Tend to when the result of its quality is claimed daily During fixed value, shale samples particle water vapor desorption reaches balance, and the wide-mouth bottle that will be equipped with shale samples particle is equipped with from bottom Take out in the glassware of saturation LiCl salting liquid, being placed on drying baker carries out 110 DEG C of drying in 24 hours, after drying, claims its matter Amount;
S. the porosity of shale samples particle is measuredAnd density pT, with reference to the unit mass page that step F to step R is obtained Water content W of rock sample particleg, calculate the water saturation of shale samples particle;
SwFor the water saturation of shale samples particle,For the porosity of shale samples particle, ρTFor shale samples particle Density, ρwFor the density of water, WgFor the water content of unit quality shale samples particle;
T. according to Kelvin equation, the capillary pressure of shale samples particle is calculated;
PcFor the capillary pressure of shale;R is universal gas constant;T is temperature;VmTo condense the molal volume of drop;P is Water vapor in air pressure;p0For saturated vapor pressure;
U. according to the water saturation and capillary pressure result of the above-mentioned shale samples particle for calculating, shale sample is obtained The relation curve of product particle capillary pressure and water saturation.
The present invention cannot be only used for the pore configuration research of shale reservoir, porosity, relative permeability, shale wetability and Irreducible water saturation determine, and shale reservoir performance assessment, reserves calculate etc. aspect be with a wide range of applications, survey The capillary pressure of amount shale and the relation curve of water saturation, have for the Efficient Development of unconventional shale gas resource is utilized Significance.
Description of the drawings
Fig. 1 is flow chart of the present invention;
Fig. 2 implements schematic diagram for the present invention.
Specific embodiment
Embodiment 1:Referring to Fig. 1, Fig. 2, the measuring method of a kind of shale capillary pressure and water saturation, including following step Suddenly:
A. shale samples are ground into the shale samples particle of different-grain diameter in 250 μm~800 μ ms;
B. shale samples particle is loaded into wide-mouth bottle;
C. will be equipped with the wide-mouth bottle of shale samples particle carries out 110 DEG C of drying in 24 hours;
D. by drying after the wide-mouth bottle equipped with shale samples particle be positioned over bottom equipped with drier glassware in It is cooled to room temperature;
E. the wide-mouth bottle that will be equipped with shale samples particle takes out from glassware of the bottom equipped with drier, claims its quality Afterwards, in being positioned over glassware of the bottom equipped with saturation LiCl salting liquid;
F. glassware of the bottom equipped with saturation LiCl salting liquid that placed the wide-mouth bottle of shale samples particle is put into In 50 DEG C of insulating box, the wide-mouth bottle equipped with shale samples particle was taken out from insulating box per 24 hours, its quality is claimed respectively;When When claiming the result of its quality to tend to fixed value daily, shale samples particle capillary pressure reaches balance, by shale samples particle Wide-mouth bottle from bottom equipped with saturation LiCl salting liquid glassware in take out, be placed on drying baker carry out 24 hours 110 DEG C Drying, after drying, claims its quality;
G. will from bottom equipped with saturation LiCl salting liquid glassware in take out, and dry claim its quality after equipped with page The wide-mouth bottle of rock sample particle, is positioned over bottom equipped with saturation MgCl2In the glassware of salting liquid, 50 DEG C of perseverance is then placed in In incubator, the wide-mouth bottle equipped with shale samples particle was taken out from insulating box per 24 hours, its quality is claimed respectively;Claim it when daily When the result of quality tends to fixed value, shale samples particle capillary pressure reaches balance, will be equipped with the wide of shale samples particle Mouth bottle is equipped with saturation MgCl from bottom2Take out in the glassware of salting liquid, being placed on drying baker carries out 110 DEG C of bakings in 24 hours It is dry, after drying, claim its quality;
H. saturation MgCl will be housed from bottom2In the glassware of salting liquid take out, and dry claim its quality after being equipped with The wide-mouth bottle of shale samples particle, in being positioned over glassware of the bottom equipped with saturation NaBr salting liquid, is then placed in 50 DEG C In insulating box, the wide-mouth bottle equipped with shale samples particle was taken out from insulating box per 24 hours, its quality is claimed respectively;Claim when daily When the result of its quality tends to fixed value, shale samples particle capillary pressure reaches balance, will be equipped with shale samples particle Wide-mouth bottle takes out from glassware of the bottom equipped with saturation NaBr salting liquid, and being placed on drying baker carries out 110 DEG C of bakings in 24 hours It is dry, after drying, claim its quality;
I. will from bottom equipped with saturation NaBr salting liquid glassware in take out, and dry claim its quality after equipped with page The wide-mouth bottle of rock sample particle, is positioned over bottom equipped with saturation NaNO3In the glassware of salting liquid, 50 DEG C of perseverance is then placed in In incubator, the wide-mouth bottle equipped with shale samples particle was taken out from insulating box per 24 hours, its quality is claimed respectively;Claim it when daily When the result of quality tends to fixed value, shale samples particle capillary pressure reaches balance, will be equipped with the wide of shale samples particle Mouth bottle is equipped with saturation NaNO from bottom3Take out in the glassware of salting liquid, being placed on drying baker carries out 110 DEG C of bakings in 24 hours It is dry, after drying, claim its quality;
J. saturation NaNO will be housed from bottom3In the glassware of salting liquid take out, and dry claim its quality after being equipped with The wide-mouth bottle of shale samples particle, in being positioned over glassware of the bottom equipped with saturation KCl salting liquid, is then placed in 50 DEG C of perseverance In incubator, the wide-mouth bottle equipped with shale samples particle was taken out from insulating box per 24 hours, its quality is claimed respectively;Claim it when daily When the result of quality tends to fixed value, shale samples particle capillary pressure reaches balance, will be equipped with the wide of shale samples particle Mouth bottle takes out from glassware of the bottom equipped with saturation KCl salting liquid, and being placed on drying baker carries out 110 DEG C of drying in 24 hours, After drying, claim its quality;
K. will from bottom equipped with saturation KCl salting liquid glassware in take out, and dry claim its quality after equipped with page The wide-mouth bottle of rock sample particle, is positioned over bottom equipped with saturation KNO3In the glassware of salting liquid, 50 DEG C of perseverance is then placed in In incubator, the wide-mouth bottle equipped with shale samples particle was taken out from insulating box per 24 hours, its quality is claimed respectively;Claim it when daily When the result of quality tends to fixed value, shale samples particle capillary pressure reaches balance, will be equipped with the wide of shale samples particle Mouth bottle is equipped with saturation KNO from bottom3Take out in the glassware of salting liquid, being placed on drying baker carries out 110 DEG C of drying in 24 hours, After drying, claim its quality;
L. saturation KNO will be housed from bottom3In the glassware of salting liquid take out, and dry claim its quality after equipped with page The wide-mouth bottle of rock sample particle, is positioned over bottom equipped with saturation K2SO4In the glassware of salting liquid, 50 DEG C of perseverance is then placed in In incubator, the wide-mouth bottle equipped with shale samples particle was taken out from insulating box per 24 hours, its quality is claimed respectively;Claim it when daily When the result of quality tends to fixed value, shale samples particle capillary pressure reaches balance, will be equipped with the wide of shale samples particle Mouth bottle is equipped with saturation K from bottom2SO4Take out in the glassware of salting liquid, being placed on drying baker carries out 110 DEG C of drying in 24 hours, After drying, claim its quality;
M. saturation K will be housed from bottom2Take out in the glassware of SO salting liquids, will be equipped with the wide-mouth of shale samples particle Bottle is positioned over bottom equipped with saturation KNO3In the glassware of salting liquid, in being then placed in 50 DEG C of insulating box, per 24 hours from The wide-mouth bottle equipped with shale samples particle is taken out in insulating box, its quality is claimed respectively;When the result for claiming its quality daily tends to solid During definite value, shale samples particle water vapor desorption reaches balance, will be equipped with the wide-mouth bottle of shale samples particle from bottom equipped with full And KNO3Take out in the glassware of salting liquid, being placed on drying baker carries out 110 DEG C of drying in 24 hours, after drying, claims its quality;
N. saturation KNO will be housed from bottom3Take out in the glassware of salting liquid, will be equipped with the wide-mouth of shale samples particle Bottle is positioned in glassware of the bottom equipped with saturation KCl salting liquid, in being then placed in 50 DEG C of insulating box, per 24 hours from perseverance The wide-mouth bottle equipped with shale samples particle is taken out in incubator, its quality is claimed respectively;When the result for claiming its quality daily tends to fixed During value, shale samples particle water vapor desorption reaches balance, and the wide-mouth bottle that will be equipped with shale samples particle is equipped with saturation from bottom Take out in the glassware of KCl salting liquids, being placed on drying baker carries out 110 DEG C of drying in 24 hours, after drying, claims its quality;
O. will take out from glassware of the bottom equipped with saturation KCl salting liquid, will be equipped with the wide-mouth of shale samples particle Bottle is positioned over bottom equipped with saturation NaNO3In the glassware of salting liquid, in being then placed in 50 DEG C of insulating box, per 24 hours from The wide-mouth bottle equipped with shale samples particle is taken out in insulating box, its quality is claimed respectively;When the result for claiming its quality daily tends to solid During definite value, shale samples particle water vapor desorption reaches balance, will be equipped with the wide-mouth bottle of shale samples particle from bottom equipped with full And NaNO3Take out in the glassware of salting liquid, being placed on drying baker carries out 110 DEG C of drying in 24 hours, after drying, claims its matter Amount;
P. saturation NaNO will be housed from bottom3Take out in the glassware of salting liquid, will be equipped with the wide of shale samples particle Mouth bottle is positioned in glassware of the bottom equipped with saturation NaBr salting liquid, in being then placed in 50 DEG C of insulating box, per 24 hours The wide-mouth bottle equipped with shale samples particle is taken out from insulating box, its quality is claimed respectively;Tend to when the result of its quality is claimed daily During fixed value, shale samples particle water vapor desorption reaches balance, and the wide-mouth bottle that will be equipped with shale samples particle is equipped with from bottom Take out in the glassware of saturation NaBr salting liquid, being placed on drying baker carries out 110 DEG C of drying in 24 hours, after drying, claims its matter Amount;
Q. will take out from glassware of the bottom equipped with saturation NaBr salting liquid, will be equipped with the wide-mouth of shale samples particle Bottle is positioned over bottom equipped with saturation MgCl2In the glassware of salting liquid, in being then placed in 50 DEG C of insulating box, per 24 hours from The wide-mouth bottle equipped with shale samples particle is taken out in insulating box, its quality is claimed respectively;When the result for claiming its quality daily tends to solid During definite value, shale samples particle water vapor desorption reaches balance, will be equipped with the wide-mouth bottle of shale samples particle from bottom equipped with full And MgCl2Take out in the glassware of salting liquid, being placed on drying baker carries out 110 DEG C of drying in 24 hours, after drying, claims its matter Amount;
R. saturation MgCl will be housed from bottom2Take out in the glassware of salting liquid, will be equipped with the wide of shale samples particle Mouth bottle is positioned in glassware of the bottom equipped with saturation LiCl salting liquid, in being then placed in 50 DEG C of insulating box, per 24 hours The wide-mouth bottle equipped with shale samples particle is taken out from insulating box, its quality is claimed respectively;Tend to when the result of its quality is claimed daily During fixed value, shale samples particle water vapor desorption reaches balance, and the wide-mouth bottle that will be equipped with shale samples particle is equipped with from bottom Take out in the glassware of saturation LiCl salting liquid, being placed on drying baker carries out 110 DEG C of drying in 24 hours, after drying, claims its matter Amount;
S. the porosity of shale samples particle is measuredAnd density pT, with reference to the unit mass page that step F to step R is obtained Water content W of rock sample particleg, calculate the water saturation of shale samples particle;
SwFor the water saturation of shale samples particle,For the porosity of shale samples particle, ρTFor shale samples particle Density, ρwFor the density of water, WgFor the water content of unit quality shale samples particle;
T. according to Kelvin equation, the capillary pressure of shale samples particle is calculated;
PcFor the capillary pressure of shale;R is universal gas constant;T is temperature;VmTo condense the molal volume of drop;P is Water vapor in air pressure;p0For saturated vapor pressure;
U. according to the water saturation and capillary pressure result of the above-mentioned shale samples particle for calculating, shale sample is obtained The relation curve of product particle capillary pressure and water saturation.

Claims (1)

1. the measuring method of a kind of shale capillary pressure and water saturation, it is characterised in that comprise the following steps:
A. shale samples are ground into the shale samples particle of different-grain diameter in 250 μm~800 μ ms;
B. shale samples particle is loaded into wide-mouth bottle;
C. will be equipped with the wide-mouth bottle of shale samples particle carries out 110 DEG C of drying in 24 hours;
D. by drying after the wide-mouth bottle equipped with shale samples particle be positioned over bottom equipped with drier glassware in it is cold and To room temperature;
E. the wide-mouth bottle that will be equipped with shale samples particle takes out from glassware of the bottom equipped with drier, after claiming its quality, In being positioned over glassware of the bottom equipped with saturation LiCl salting liquid;
F. glassware of the bottom equipped with saturation LiCl salting liquid that placed the wide-mouth bottle of shale samples particle is put into into 50 DEG C Insulating box in, per 24 hours from insulating box take out equipped with shale samples particle wide-mouth bottle, its quality is claimed respectively;When daily When claiming the result of its quality to tend to fixed value, shale samples particle capillary pressure reaches balance, by the wide of shale samples particle Mouth bottle takes out from glassware of the bottom equipped with saturation LiCl salting liquid, and being placed on drying baker carries out 110 DEG C of drying in 24 hours, After drying, claim its quality;
G. will from bottom equipped with saturation LiCl salting liquid glassware in take out, and dry claim its quality after equipped with shale sample The wide-mouth bottle of product particle, is positioned over bottom equipped with saturation MgCl2In the glassware of salting liquid, 50 DEG C of insulating box is then placed in In, the wide-mouth bottle equipped with shale samples particle was taken out from insulating box per 24 hours, its quality is claimed respectively;When claiming its quality daily Result when tending to fixed value, shale samples particle capillary pressure reaches balance, will be equipped with the wide-mouth bottle of shale samples particle Saturation MgCl is housed from bottom2Take out in the glassware of salting liquid, being placed on drying baker carries out 110 DEG C of drying in 24 hours, dries After dry, claim its quality;
H. saturation MgCl will be housed from bottom2In the glassware of salting liquid take out, and dry claim its quality after equipped with shale sample The wide-mouth bottle of product particle, in being positioned over glassware of the bottom equipped with saturation NaBr salting liquid, is then placed in 50 DEG C of insulating box In, the wide-mouth bottle equipped with shale samples particle was taken out from insulating box per 24 hours, its quality is claimed respectively;When claiming its quality daily Result when tending to fixed value, shale samples particle capillary pressure reaches balance, will be equipped with the wide-mouth bottle of shale samples particle Take out from glassware of the bottom equipped with saturation NaBr salting liquid, being placed on drying baker carries out 110 DEG C of drying in 24 hours, drying Afterwards, its quality is claimed;
I. will from bottom equipped with saturation NaBr salting liquid glassware in take out, and dry claim its quality after equipped with shale sample The wide-mouth bottle of product particle, is positioned over bottom equipped with saturation NaNO3In the glassware of salting liquid, 50 DEG C of insulating box is then placed in In, the wide-mouth bottle equipped with shale samples particle was taken out from insulating box per 24 hours, its quality is claimed respectively;When claiming its quality daily Result when tending to fixed value, shale samples particle capillary pressure reaches balance, will be equipped with the wide-mouth bottle of shale samples particle Saturation NaNO is housed from bottom3Take out in the glassware of salting liquid, being placed on drying baker carries out 110 DEG C of drying in 24 hours, dries After dry, claim its quality;
J. saturation NaNO will be housed from bottom3In the glassware of salting liquid take out, and dry claim its quality after equipped with shale sample The wide-mouth bottle of product particle, in being positioned over glassware of the bottom equipped with saturation KCl salting liquid, is then placed in 50 DEG C of insulating box In, the wide-mouth bottle equipped with shale samples particle was taken out from insulating box per 24 hours, its quality is claimed respectively;When claiming its quality daily Result when tending to fixed value, shale samples particle capillary pressure reaches balance, will be equipped with the wide-mouth bottle of shale samples particle Take out from glassware of the bottom equipped with saturation KCl salting liquid, being placed on drying baker carries out 110 DEG C of drying in 24 hours, drying Afterwards, its quality is claimed;
K. will from bottom equipped with saturation KCl salting liquid glassware in take out, and dry claim its quality after equipped with shale sample The wide-mouth bottle of product particle, is positioned over bottom equipped with saturation KNO3In the glassware of salting liquid, 50 DEG C of insulating box is then placed in In, the wide-mouth bottle equipped with shale samples particle was taken out from insulating box per 24 hours, its quality is claimed respectively;When claiming its quality daily Result when tending to fixed value, shale samples particle capillary pressure reaches balance, will be equipped with the wide-mouth bottle of shale samples particle Saturation KNO is housed from bottom3Take out in the glassware of salting liquid, being placed on drying baker carries out 110 DEG C of drying in 24 hours, drying Afterwards, its quality is claimed;
L. saturation KNO will be housed from bottom3In the glassware of salting liquid take out, and dry claim its quality after equipped with shale sample The wide-mouth bottle of product particle, is positioned over bottom equipped with saturation K2SO4In the glassware of salting liquid, 50 DEG C of insulating box is then placed in In, the wide-mouth bottle equipped with shale samples particle was taken out from insulating box per 24 hours, its quality is claimed respectively;When claiming its quality daily Result when tending to fixed value, shale samples particle capillary pressure reaches balance, will be equipped with the wide-mouth bottle of shale samples particle Saturation K is housed from bottom2SO4Take out in the glassware of salting liquid, being placed on drying baker carries out 110 DEG C of drying in 24 hours, drying Afterwards, its quality is claimed;
M. saturation K will be housed from bottom2Take out in the glassware of SO salting liquids, the wide-mouth bottle that will be equipped with shale samples particle is put Bottom is placed in equipped with saturation KNO3In the glassware of salting liquid, in being then placed in 50 DEG C of insulating box, per 24 hours from constant temperature The wide-mouth bottle equipped with shale samples particle is taken out in case, its quality is claimed respectively;Tend to fixed value when the result of its quality is claimed daily When, shale samples particle water vapor desorption reaches balance, and the wide-mouth bottle that will be equipped with shale samples particle is equipped with saturation from bottom KNO3Take out in the glassware of salting liquid, being placed on drying baker carries out 110 DEG C of drying in 24 hours, after drying, claims its quality;
N. saturation KNO will be housed from bottom3Take out in the glassware of salting liquid, the wide-mouth bottle that will be equipped with shale samples particle is put In being placed in glassware of the bottom equipped with saturation KCl salting liquid, in being then placed in 50 DEG C of insulating box, per 24 hours from insulating box It is middle to take out the wide-mouth bottle equipped with shale samples particle, its quality is claimed respectively;When the result for claiming its quality daily tends to fixed value, Shale samples particle water vapor desorption reaches balance, and the wide-mouth bottle that will be equipped with shale samples particle is equipped with saturation KCl salt from bottom Take out in the glassware of solution, being placed on drying baker carries out 110 DEG C of drying in 24 hours, after drying, claims its quality;
O. will take out from glassware of the bottom equipped with saturation KCl salting liquid, the wide-mouth bottle that will be equipped with shale samples particle is put Bottom is placed in equipped with saturation NaNO3In the glassware of salting liquid, in being then placed in 50 DEG C of insulating box, per 24 hours from constant temperature The wide-mouth bottle equipped with shale samples particle is taken out in case, its quality is claimed respectively;Tend to fixed value when the result of its quality is claimed daily When, shale samples particle water vapor desorption reaches balance, and the wide-mouth bottle that will be equipped with shale samples particle is equipped with saturation from bottom NaNO3Take out in the glassware of salting liquid, being placed on drying baker carries out 110 DEG C of drying in 24 hours, after drying, claims its quality;
P. saturation NaNO will be housed from bottom3Take out in the glassware of salting liquid, the wide-mouth bottle that will be equipped with shale samples particle is put In being placed in glassware of the bottom equipped with saturation NaBr salting liquid, in being then placed in 50 DEG C of insulating box, per 24 hours from constant temperature The wide-mouth bottle equipped with shale samples particle is taken out in case, its quality is claimed respectively;Tend to fixed value when the result of its quality is claimed daily When, shale samples particle water vapor desorption reaches balance, and the wide-mouth bottle that will be equipped with shale samples particle is equipped with saturation from bottom Take out in the glassware of NaBr salting liquids, being placed on drying baker carries out 110 DEG C of drying in 24 hours, after drying, claims its quality;
Q. will take out from glassware of the bottom equipped with saturation NaBr salting liquid, the wide-mouth bottle that will be equipped with shale samples particle is put Bottom is placed in equipped with saturation MgCl2In the glassware of salting liquid, in being then placed in 50 DEG C of insulating box, per 24 hours from constant temperature The wide-mouth bottle equipped with shale samples particle is taken out in case, its quality is claimed respectively;Tend to fixed value when the result of its quality is claimed daily When, shale samples particle water vapor desorption reaches balance, and the wide-mouth bottle that will be equipped with shale samples particle is equipped with saturation from bottom MgCl2Take out in the glassware of salting liquid, being placed on drying baker carries out 110 DEG C of drying in 24 hours, after drying, claims its quality;
R. saturation MgCl will be housed from bottom2Take out in the glassware of salting liquid, the wide-mouth bottle that will be equipped with shale samples particle is put In being placed in glassware of the bottom equipped with saturation LiCl salting liquid, in being then placed in 50 DEG C of insulating box, per 24 hours from constant temperature The wide-mouth bottle equipped with shale samples particle is taken out in case, its quality is claimed respectively;Tend to fixed value when the result of its quality is claimed daily When, shale samples particle water vapor desorption reaches balance, and the wide-mouth bottle that will be equipped with shale samples particle is equipped with saturation from bottom Take out in the glassware of LiCl salting liquids, being placed on drying baker carries out 110 DEG C of drying in 24 hours, after drying, claims its quality;
S. the porosity of shale samples particle is measuredAnd density pT, with reference to the unit mass shale sample that step F to step R is obtained Water content W of product particleg, calculate the water saturation of shale samples particle;
SwFor the water saturation of shale samples particle,For the porosity of shale samples particle, ρTFor the close of shale samples particle Degree, ρwFor the density of water, WgFor the water content of unit quality shale samples particle;
T. according to Kelvin equation, the capillary pressure of shale samples particle is calculated;
P c = - R T V m l n ( p / p 0 )
PcFor the capillary pressure of shale;R is universal gas constant;T is temperature;VmTo condense the molal volume of drop;P is air Middle water vapor pressure;p0For saturated vapor pressure;
U. according to the water saturation and capillary pressure result of the above-mentioned shale samples particle for calculating, shale samples are obtained The relation curve of grain capillary pressure and water saturation.
CN201610887320.2A 2016-10-11 2016-10-11 Shale capillary pressure and water saturation measurement method Pending CN106644875A (en)

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Publication number Priority date Publication date Assignee Title
CN107402169A (en) * 2017-07-28 2017-11-28 中国科学院力学研究所 A kind of devices and methods therefor for distinguishing shale reservoir matrix pores and microcrack
CN107727549A (en) * 2017-09-27 2018-02-23 中国科学院力学研究所 A kind of shale microscopic void measuring method and equipment
CN111157424A (en) * 2020-01-07 2020-05-15 中南大学 Rock material pore size distribution measuring method
CN112683718A (en) * 2020-12-28 2021-04-20 重庆大学 Device and method for measuring content of soil combined water and permeability coefficient

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Title
ASTM INTERNATIONAL: "《ASTM D1412-07 Standard Test Method for Equilibrium Moisture of Coal at 96 to 97 Percent Relative Humidity and 30℃》", 31 December 2007, ASTM INTERNATIONAL *
同济大学道路与交通工程研究所 等: "《半刚性基层沥青路面》", 30 November 1991, 人民交通出版社 *
李靖 等: "《页岩黏土孔隙含水饱和度分布及其对甲烷吸附的影响》", 《力学学报》 *
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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107402169A (en) * 2017-07-28 2017-11-28 中国科学院力学研究所 A kind of devices and methods therefor for distinguishing shale reservoir matrix pores and microcrack
CN107402169B (en) * 2017-07-28 2019-09-06 中国科学院力学研究所 A kind of devices and methods therefor for distinguishing shale reservoir matrix pores and microcrack
CN107727549A (en) * 2017-09-27 2018-02-23 中国科学院力学研究所 A kind of shale microscopic void measuring method and equipment
CN111157424A (en) * 2020-01-07 2020-05-15 中南大学 Rock material pore size distribution measuring method
CN112683718A (en) * 2020-12-28 2021-04-20 重庆大学 Device and method for measuring content of soil combined water and permeability coefficient
CN112683718B (en) * 2020-12-28 2022-02-18 重庆大学 Device and method for measuring content of soil combined water and permeability coefficient

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