CN106168565A - A kind of device and method measuring shale substrate air content - Google Patents
A kind of device and method measuring shale substrate air content Download PDFInfo
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- CN106168565A CN106168565A CN201510424979.XA CN201510424979A CN106168565A CN 106168565 A CN106168565 A CN 106168565A CN 201510424979 A CN201510424979 A CN 201510424979A CN 106168565 A CN106168565 A CN 106168565A
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Abstract
The invention discloses a kind of device and method measuring shale substrate air content, belong to shale gas production technique field.The device of this measurement shale substrate air content includes calorstat, core holding unit, gas injection section, confined pressure portion and thermometer；Core holding unit is arranged in calorstat, and rock sample is clamped in core holding unit；Gas injection section is connected with the entrance of core holding unit, and confined pressure portion is connected with core holding unit.The present invention is by the hot environment of calorstat simulation down-hole, environment under high pressure by simulation down-hole, confined pressure portion, so that the content error of the shale gas of adsorbed state is less in surveyed rock sample, and by the first Pressure gauge, the 3rd Pressure gauge and the setting of the first valve, the reading that the shale gas content of adsorbed state and the shale gas content of free state can be shown by the first Pressure gauge and the 3rd Pressure gauge calculates and obtains, it is easy to set up the content ratio of the shale gas of the shale gas of adsorbed state in rock sample and free state, improves the accuracy of the gassiness evaluation to shale substrate.
Description
Technical field
The present invention relates to shale gas production technique field, particularly to a kind of dress measuring shale substrate air content
Put and method.
Background technology
Shale gas is as the important supplement of conventional energy resource, and its development and utilization is conducive to alleviating petroleum resources shortage,
Increase clean energy resource supply.Shale gas with absorption or free state be present in mud stone, high-carbon mud stone, shale and
In the shale substrate such as aleuritic texture rock, before exploitation, the gas-bearing property of shale substrate need to be evaluated, wherein,
The shale gas content measuring adsorbed state has vital effect for the gas-bearing property evaluating shale substrate.
At present by the containing of the shale gas of adsorbed state under shale adsorption isotherm experiment measurement device different temperatures
Amount.Shale adsorption isotherm experiment device include gas cylinder, force (forcing) pump, calorstat, sample cylinder, with reference to cylinder and from
Dynamic acquisition systems etc., rock sample is that rock sample is placed in sample cylinder, sample by the fritter rock gathered in shale substrate
Product cylinder is arranged in calorstat, and the pressurized pump of gas cylinder connects with sample cylinder, automated collection systems and sample cylinder and
Connect with reference to cylinder, gather sample cylinder and with reference to the data in cylinder by automated collection systems, according to collect
Data calculate the shale gas content of adsorbed state in rock sample, thus make an appraisal the gas-bearing property of shale substrate.
During realizing the present invention, inventor finds that prior art at least there is problems in that
Existing adsorption isotherm experiment device can not simulate the environment under high pressure of down-hole, and pressure with in shale substrate
The shale gas relation with contents of adsorbed state is close, causes measuring result error bigger.
Summary of the invention
The environment under high pressure of down-hole can not be simulated to solve existing adsorption isotherm experiment device, cause measuring knot
The problem that really error is bigger, embodiments provides a kind of device measuring shale substrate air content and side
Method.Described technical scheme is as follows:
On the one hand, it is provided that a kind of device measuring shale substrate air content, described measurement shale substrate gassiness
The device of amount is for measuring shale gas total content, the shale gas content of free state and the adsorbed state in rock sample
Shale gas content, the device of described measurement shale substrate air content includes calorstat, core holding unit, note
Gas portion, confined pressure portion and thermometer；
By described calorstat simulation down-hole hot environment；
Described core holding unit is arranged in described calorstat, and described rock sample is clamped in described core holding unit；
Described gas injection section is connected with the entrance of described core holding unit, described core holding unit and described gas injection section
Between be provided with the first Pressure gauge and the first valve, and described first Pressure gauge is positioned at described first valve and described
Between gas injection section；
Described confined pressure portion is connected with described core holding unit, described confined pressure portion along the circumference of described rock sample to described
Rock sample applies pressure, is provided with the second valve and the second Pressure gauge between described confined pressure portion and described core holding unit,
Described second Pressure gauge is between described second valve and described core holding unit；
The outlet line of described core holding unit is provided with the 3rd Pressure gauge and the 3rd valve, and described 3rd pressure
Power epi-position is between described core holding unit and described 3rd valve；
Described thermometer is arranged on inside described calorstat, is detected inside described calorstat by described thermometer
Temperature.
Further, described gas injection section includes gas cylinder, high-pressure pump and high pressure intermediate receptacle；
Described gas cylinder is connected with described high pressure intermediate receptacle through described high-pressure pump, and described high-pressure pump and institute
Stating and be provided with the 4th valve between high pressure intermediate receptacle, described high pressure intermediate receptacle is through described first Pressure gauge and institute
State the first valve to be connected with the entrance of described core holding unit.
Specifically, described confined pressure portion is hydraulic pump.
Further, the device of described measurement shale substrate air content also includes single-chip microcomputer and display；
Described single-chip microcomputer and described thermometer, described first Pressure gauge, described second Pressure gauge and the described 3rd
Pressure gauge connects, and calculates temperature that described rock sample shows at described thermometer and described the by described single-chip microcomputer
Shale gas total content, the shale gas content of free state and adsorbed state under the confined pressure that two Pressure gauges show
Shale gas content；
Described display is connected with described single-chip microcomputer, is shown that by described display the calculating of described single-chip microcomputer is tied
Really.
Specifically, described core holding unit includes fixing cylinder and packing element, wraps up described rock sample by described packing element,
Hold described rock sample by described fixing collet chuck, and described packing element is positioned at inside described fixing cylinder.
Specifically, described rock sample is cylinder, and a diameter of 2.5 centimetres or 7 cun of described rock sample, described rock sample
Length between 2.5～7.6 centimetres.
On the other hand, it is provided that a kind of method measuring shale substrate air content, described measurement shale substrate contains
The method of tolerance applies the device of described measurement shale substrate air content, described measurement shale substrate air content
Method comprises the steps:
Step 100: connect and correct the device of described measurement shale substrate air content；
Step 200: rock sample is fixed in core holding unit；
Step 300: get rid of the air in the device of described measurement shale substrate air content, and close all valves；
Step 400: open the second valve, adds confined pressure by confined pressure portion to rock sample, until the second manometric reading
When number reaches to preset confined pressure, close the second valve；
Step 500: open the 4th valve, the methane gas in gas cylinder is pumped into and holds in the middle of high pressure by high-pressure pump
In device, when the first manometric reading reaches preset pressure, close the 4th valve；
Step 600: record the first manometric reading P1After open the first valve, make in high pressure intermediate receptacle
Methane gas enter in rock sample, after the first manometric reading is reduced to certain limit, close the first valve
Door, records the first manometric reading P2, until after the 3rd manometric stable reading, recording the 3rd pressure
The reading P of table3；
Step 700: judge the 3rd manometric reading P3Whether reach formation gas pressure, when the 3rd Pressure gauge
Reading P3When reaching formation gas pressure, enter step 800, as the 3rd manometric reading P3Not up to
During formation gas pressure, enter step 600；
Step 800: process experimental data, provide the gassiness evaluation result of shale substrate.
Specifically, described default confined pressure calculates according to equation below (1):
P=Z × g × ρR×10-6 (1)
Wherein:
P is confined pressure；
Z is the vertically layer depth of described rock sample position；
ρRDensity for described rock sample；
G is acceleration of gravity.
Further, described step 800: process experimental data, provide the gassiness evaluation result of shale substrate
Including:
According to the first manometric reading P1, the first manometric reading P2With the 3rd manometric reading P3Meter
Calculate at the 3rd manometric reading P3Under, the shale gas total content in rock sample, the shale gas content of free state
Shale gas content with adsorbed state；
According to the 3rd different manometric reading P3Under shale gas total content, the shale gas of free state contains
The shale gas content of amount and adsorbed state provides the gassiness evaluation result of shale substrate.
The technical scheme that the embodiment of the present invention provides has the benefit that
The present invention is by the hot environment of calorstat simulation down-hole, by the environment under high pressure of simulation down-hole, confined pressure portion,
So that the content error of the shale gas of adsorbed state is less in surveyed rock sample, and by the first Pressure gauge,
3rd Pressure gauge and the setting of the first valve so that the shale gas content of adsorbed state and the shale of free state
The reading that Gas content can be shown by the first Pressure gauge and the 3rd Pressure gauge calculates and obtains, it is simple to sets up in rock sample and inhales
The shale gas of attached state and the content ratio of the shale gas of free state, improve the gas-bearing property to shale substrate and comment
The accuracy of valency.
Accompanying drawing explanation
For the technical scheme being illustrated more clearly that in the embodiment of the present invention, institute in embodiment being described below
The accompanying drawing used is needed to be briefly described, it should be apparent that, the accompanying drawing in describing below is only the present invention
Some embodiments, for those of ordinary skill in the art, on the premise of not paying creative work,
Other accompanying drawing can also be obtained according to these accompanying drawings.
Fig. 1 is the structural representation of the device measuring shale substrate air content that the present invention one implements to provide；
Fig. 2 is the flow chart of the method measuring shale substrate air content that further embodiment of this invention provides；
Fig. 3 is the flow chart of the method measuring shale substrate air content that further embodiment of this invention provides；
Fig. 4 is that the utilization that further embodiment of this invention provides measures the method for shale substrate air content to certain rock sample
Carry out the experimental result schematic diagram tested.
Wherein:
1 gas cylinder,
2 high-pressure pumps,
3 the 4th valves,
4 high pressure intermediate receptacles,
5 first Pressure gauges,
6 first valves,
7 calorstats,
8 fix cylinder,
9 packing elements,
10 rock samples,
11 the 3rd valves,
12 the 3rd Pressure gauges,
13 thermometers,
14 second valves,
15 second Pressure gauges,
A gas injection section,
B confined pressure portion,
C rock core adds holder,
S adsorbed gas content critical point.
Detailed description of the invention
For making the object, technical solutions and advantages of the present invention clearer, below in conjunction with accompanying drawing to the present invention
Embodiment is described in further detail.
Embodiment one
As it is shown in figure 1, embodiments provide a kind of device measuring shale substrate air content, this survey
The device of amount shale substrate air content is used for shale gas total content, the shale gas of free state measuring in rock sample
The shale gas content of content and adsorbed state, the device measuring shale substrate air content includes calorstat 7, rock core
Clamper C, gas injection section A, confined pressure portion B and thermometer 13；
Down-hole hot environment is simulated by calorstat 7；
Core holding unit C is arranged in calorstat 7, and rock sample 10 is clamped in core holding unit C；
Gas injection section A is connected with the entrance of core holding unit C, is provided with between core holding unit C and gas injection section A
First Pressure gauge 5 and the first valve 6, and the first Pressure gauge 5 is between the first valve 6 and gas injection section A；
Confined pressure portion B is connected with core holding unit C, and confined pressure portion B applies along the circumference of rock sample 10 to rock sample 10
Pressure, is provided with the second valve 14 and the second Pressure gauge 15 between confined pressure portion B and core holding unit C, and second
Pressure gauge 15 is between the second valve 14 and core holding unit C；
The outlet line of core holding unit C is provided with the 3rd Pressure gauge 12 and the 3rd valve 11, and the 3rd pressure
Table 12 is between core holding unit C and the 3rd valve 11；
It is internal that thermometer 13 is arranged on calorstat 7, detects the temperature within calorstat 7 by thermometer 13.
The present invention simulates the hot environment of down-hole by calorstat 7, by the high pressure of confined pressure portion B simulation down-hole
Environment, so that the content error of the shale gas of adsorbed state is less in surveyed rock sample 10, and by first
Pressure gauge the 5, the 3rd Pressure gauge 12 and the setting of the first valve 6 so that the shale gas content of adsorbed state and
Reading that the shale gas content of free state can be shown by the first Pressure gauge 5 and the 3rd Pressure gauge 12 calculate and
, it is simple to set up the shale gas of adsorbed state in rock sample 10 and the content ratio of the shale gas of free state, carry
The high accuracy to shale substrate gassiness evaluation.
As it is shown in figure 1, in embodiments of the present invention, gas injection section A includes gas cylinder 1, high-pressure pump 2 and
High pressure intermediate receptacle 4；
Gas cylinder 1 is connected with high pressure intermediate receptacle 4 through high-pressure pump 2, and high-pressure pump 2 and high pressure centre hold
Being provided with the 4th valve 3 between device 4, high pressure intermediate receptacle 4 is through the first Pressure gauge 5 and the first valve 6 and rock core
The entrance of clamper C connects.By gas cylinder 1 storing methane, wherein, the purity of methane is more than 99%,
Methane in gas cylinder 1 is pumped in high pressure intermediate receptacle 4 by high-pressure pump 2.
As it is shown in figure 1, core holding unit C includes fixing cylinder 8 and packing element 9, wrap up rock sample by packing element 9
10, clamp rock sample 10 by fixing cylinder 8, and packing element 9 is positioned at fixing cylinder 8 inside.
In embodiments of the present invention, rock sample 10 is cylinder, and a diameter of 2.5 centimetres or 7 cun of rock sample 10,
The length of rock sample 10 is between 2.5～7.6 centimetres, and it is internal that rock sample 10 is wrapped in packing element 9, and confined pressure portion B is liquid
Press pump or pulsometer, when confined pressure portion B is hydraulic pump, by hydraulic pump between fixing cylinder 8 and packing element 9
Gap in infusion liquid, thus packing element 9 is applied the pressure along rock sample 10 circumference, owing to packing element 9 is soft
Property material, so that the pressure of liquid all acts on rock sample 10, it is achieved along the circumference of rock sample 10 to rock
Sample 10 applies pressure, namely adds confined pressure, simulation down-hole high pressure environment residing for rock sample 10 to rock sample 10.
And in the present embodiment, the device measuring shale substrate air content also includes single-chip microcomputer and display；
Single-chip microcomputer is connected with thermometer the 13, first Pressure gauge the 5, second Pressure gauge 15 and the 3rd Pressure gauge 12,
Calculated at temperature that rock sample 10 show at thermometer 13 and the confined pressure that the second Pressure gauge 15 shows by single-chip microcomputer
Shale gas total content, the shale gas content of free state and the shale gas content of adsorbed state；
Display is connected with single-chip microcomputer, by the result of calculation of display display single-chip microcomputer.
By single-chip microcomputer and thermometer the 13, first Pressure gauge the 5, second Pressure gauge 15 and the 3rd Pressure gauge 12
Connecting, process experimental data, and show measurement result by display, wherein, measurement result can
Thinking diagrammatic form, the gas-bearing property of shale substrate by by the shale gas organizing the rock sample 10 that experimental data obtains more
Adsorpting characteristic curve represents, intuitively by Experimental results show to operator.
Certainly, it will be understood by those skilled in the art that owing to shale gas adsorbs the process on rock sample 10 and suction
The process that the shale gas of attached state and rock sample 10 desorb is inverse process, therefore it is can also be applied to survey
The desorption properties curve of amount rock sample 10.
Embodiment two
As in figure 2 it is shown, embodiments provide a kind of method measuring shale substrate air content, this survey
The device measuring shale substrate air content in the method Application Example one of amount shale substrate air content, this survey
The method of amount shale substrate air content comprises the steps:
Step 100: connect and correct the device of described measurement shale substrate air content；
Step 200: rock sample is fixed in core holding unit；
Step 300: get rid of the air in the device of described measurement shale substrate air content, and close all valves；
Step 400: open the second valve, adds confined pressure by confined pressure portion to rock sample, until the second manometric reading
When number reaches to preset confined pressure, close the second valve；
Step 500: open the 4th valve, the methane gas in gas cylinder is pumped into and holds in the middle of high pressure by high-pressure pump
In device, when the first manometric reading reaches preset pressure, close the 4th valve；
Step 600: record the first manometric reading P1After open the first valve, make in high pressure intermediate receptacle
Methane gas enter in rock sample, after the first manometric reading is reduced to certain limit, close the first valve
Door, records the first manometric reading P2, until after the 3rd manometric stable reading, recording the 3rd pressure
The reading P of table3；
Step 700: judge the 3rd manometric reading P3Whether reach formation gas pressure, when the 3rd Pressure gauge
Reading P3When reaching formation gas pressure, enter step 800, as the 3rd manometric reading P3Not up to
During formation gas pressure, enter step 600；
Step 800: process experimental data, provide the gassiness evaluation result of shale substrate.
The present invention is by the hot environment of calorstat simulation down-hole, by the environment under high pressure of simulation down-hole, confined pressure portion,
So that the content error of the shale gas of adsorbed state is less in surveyed rock sample, and by the first Pressure gauge,
3rd Pressure gauge and the setting of the first valve so that the shale gas content of adsorbed state and the shale of free state
The reading that Gas content can be shown by the first Pressure gauge and the 3rd Pressure gauge calculates and obtains, it is simple to sets up in rock sample and inhales
The shale gas of attached state and the content ratio of the shale gas of free state, improve shale substrate gassiness evaluation
Accuracy.
In embodiments of the present invention, the overlying rock pressure that size is stratum, rock sample place of confined pressure is preset, in advance
If confined pressure calculates according to equation below (1):
P=Z × g × ρR×10-6 (1)
Wherein:
P is confined pressure, namely rock sample actually covers rock pressure in down-hole；
Z is the vertically layer depth of described rock sample position；
ρRDensity for described rock sample；
G is acceleration of gravity.
Down well placement residing for rock sample is different, and the size of the stratum overlying rock pressure that rock sample is undertaken is also
Difference, by arranging confined pressure in core holding unit, the down-hole high pressure environment at simulation rock sample place so that survey
Amount result is the most accurate.
In embodiments of the present invention, processing experimental data, the gassiness evaluation result providing shale substrate includes；
According to the first manometric reading P1, the first manometric reading P2With the 3rd manometric reading P3Meter
Calculate at the 3rd manometric reading P3Under, the shale gas total content in rock sample, the shale gas content of free state
Shale gas content with adsorbed state；
According to the 3rd different manometric reading P3Under shale gas total content, the shale gas of free state contains
The shale gas content of amount and adsorbed state provides the gassiness evaluation result of shale substrate.
Wherein, ignore high pressure intermediate receptacle to the volume of the pipeline between core holding unit, then hold in the middle of high pressure
The amount of the gas reduced in device is the total content of shale gas in rock sample, and in rock sample, the total content of shale gas is permissible
Calculate according to formula (2):
Vso=(ρ1×V1-ρ2×V1)/ρs (2)
In formula (2),
VsoFor the methane gas in rock sample at the cumulative volume of the status of criterion；
ρ1For opening before the first valve the density of methane gas, ρ in high pressure intermediate receptacle1Count according to formula (3)
Calculate:
V1Volume for high pressure intermediate receptacle；
ρ2For closing after the first valve the density of methane gas, ρ in high pressure intermediate receptacle2Count according to formula (4)
Calculate；
ρsFor methane gas density at standard conditions；
In formula (3) and formula (4),
P1For opening the first manometric reading before the first valve；
P2For closing the first manometric reading after the first valve；
M is the molecular weight of methane gas；
T is the reading of thermometer；
Z1It is P for pressure1Time the compressibility factor of methane gas；
Z2It is P for pressure2Time the compressibility factor of methane gas；
R is constant, and R=0.008314MPa.m3/ (kmol.K).
Owing to having discharged the air in high pressure core holding unit before opening the first valve, open the first valve
After, the methane gas in high pressure intermediate receptacle enters through the first valve and is wrapped in inside the packing element outside rock sample,
And saturated with rock sample, therefore ignoring the first valve to the volume of the pipeline between core holding unit and rock sample and glue
On the premise of gap between Tong, in rock sample, the shale gas content of free state can be according to the 3rd manometric reading
The free space volumes of number change and rock sample calculates, therefore in rock sample, the content of the shale gas of free state can
Calculate according to formula (5):
Vsy=ρ3×V2/ρs (5)
In formula (5):
VsyFor the methane gas of free state volume at standard conditions in rock sample；
ρ3For the gas density closed after the first valve in high pressure core holding unit, ρ3Calculate according to formula (6):
V2For the free space volumes of high pressure core holding unit, V2Calculate according to formula (7):
V2=φ π d2L/4/100 (7)
ρsFor methane gas density at standard conditions；
In formula (6):
P3For closing the 3rd manometric reading after the first valve；
M is the molecular weight of methane gas；
T is the reading of thermometer；
Z3It is P for pressure3Time the compressibility factor of methane gas；
R is constant, and R=0.008314MPa.m3/ (kmol.K)
In formula (7):
φ is the porosity of rock sample；
D is the diameter of rock sample；
L is the length of rock sample.
Wherein, length L of the porosity φ of rock sample, the diameter d of rock sample and rock sample can be measured according to conventional methods.
The content of the shale gas of adsorbed state calculates according to formula (8):
Vsx=Vso-Vsy (8)
In formula (8):
VsxFor the methane gas of adsorbed state volume at standard conditions in rock sample；
VsoFor the methane gas in rock sample at the cumulative volume of the status of criterion；
VsyFor the methane gas of free state volume at standard conditions in rock sample.
Wherein, the status of criterion refer to temperature be 0 DEG C (273.15K) and pressure be 101.325 kPas (1 normal atmosphere,
760 millimetress of mercury) situation.
Thus set up the content ratio of the shale gas of free state and the shale gas of adsorbed state, and to shale substrate
Overall gas-bearing property is made an appraisal, and certainly, skilled person will appreciate that, in order to obtain sufficiently accurate survey
Amount result, should measure multi-group data as much as possible, and shale substrate entirety is contained by the result of comprehensive each group data
Gas is made an appraisal.
Embodiment three
As it is shown on figure 3, embodiments provide a kind of method measuring shale substrate air content, this survey
The device measuring shale substrate air content provided in the method Application Example one of amount shale substrate air content.
In embodiments of the present invention, before the experiments were performed, the size of rock sample, dry weight, permeability need to be measured
And porosity, measure the volume of high pressure intermediate receptacle, the volume in space between packing element and rock sample and the first valve
Door is to the volume of the pipeline between core holding unit.
Wherein, the method for this measurement shale substrate air content comprises the steps:
In a step 101, connect the device measuring shale substrate air content, be specially gas cylinder, height
Press pump, high pressure intermediate receptacle, core holding unit are coupled together by pipeline, and by confined pressure portion by pipeline with
Core holding unit couples together, and core holding unit and high pressure intermediate receptacle is arranged in calorstat, wherein,
The maximum temperature of calorstat is 150 degrees Celsius.
In a step 102, the device of shale substrate air content is measured in correction, and wherein, shale base is measured in correction
The device of matter air content specially opens the first valve and the 4th valve, closes the 3rd valve, in the middle of high pressure
Container pumps into methane gas, is then shut off the 4th valve, waits for a period of time quietly, if the first Pressure gauge and
3rd manometric reading is not changed in, then prove that the air-tightness measuring the device of shale substrate air content is good,
Can test, otherwise, then need to reconnect measure the device of shale substrate air content and re-calibrate,
Require until the air-tightness measuring the device of shale substrate air content meets design.
In step 103, rock sample is fixed on rock core and adds in holder, wherein, rock sample is fixed on rock core folder
Being specially in holder wraps in inside packing element by rock sample, and packing element forms sealing to rock sample, then along the radial direction of rock sample
Fix in the rock sample being wrapped in packing element is clamped in fixing cylinder.
At step 104, get rid of the air in the device measuring shale substrate air content, wherein, get rid of and survey
Air in the device of amount shale substrate air content can be to change high-pressure pump into vacuum pump, open the first valve
Door and the 4th valve, carry out evacuation by vacuum pump to the device of this measurement shale substrate air content, thus
Air in core holding unit is all removed.Certainly, skilled person will appreciate that, it is possible at the 4th valve
Door be connected vacuum pump by pipeline between high-pressure pump and carry out evacuation.
In step 105, all valves are closed, it is to avoid air enters the device measuring shale substrate air content
In.
In step 106, open the second valve, add confined pressure by confined pressure portion to rock sample, wherein, confined pressure portion
Can be hydraulic pump or pulsometer, by confined pressure portion pumping liquid or gas in core holding unit, to rock core
Rock sample fixing in clamper adds confined pressure, the environment under high pressure of simulation down-hole.
In step 107, when the second manometric reading reaches to preset confined pressure, close the second valve, this
Time the second Pressure gauge on the numerical value of display be the confined pressure of rock sample.
Wherein, preset confined pressure to calculate according to equation below (1):
P=Z × g × ρR×10-6 (1)
Wherein:
P is confined pressure, namely rock sample actually covers rock pressure in down-hole；
Z is the vertically layer depth of rock sample；
ρRDensity for rock sample；
G is acceleration of gravity.
In step 108, opening the 4th valve, the methane gas in gas cylinder is pumped into high pressure by high-pressure pump
In intermediate receptacle, when the first manometric reading reaches preset pressure, close the 4th valve.
In step 109, record the first manometric reading P1After open the first valve, make in the middle of high pressure
Methane gas in container enters in rock sample, after the first manometric reading is reduced to certain limit, closes
First valve, and record now the first manometric reading P2.Wherein, reduce when the first manometric reading
To P1Reading 85%～96% time, close the first valve, make methane gas the most saturated with rock sample, the time
It it is 24 hours.
In step 110, after the 3rd manometric stable reading, record the 3rd manometric reading P3。
After methane gas and rock sample are the most saturated, methane gas absorption amount on rock sample surface is not further added by, the
Three manometric readings start stable.
In step 111, it is judged that the 3rd manometric reading P3Whether reach formation gas pressure, when the 3rd
Manometric reading P3When reaching formation gas pressure, enter step 112, as the 3rd manometric reading P3Not
When reaching formation gas pressure, enter step 109.
In step 112, according to the first manometric reading P1, the first manometric reading P2With the 3rd pressure
The reading P of power table3Calculate at the 3rd manometric reading P3Shale gas total content in lower rock sample, free state
Shale gas content and the shale gas content of adsorbed state.
Wherein, ignore high pressure intermediate receptacle to the volume of the pipeline between core holding unit, then hold in the middle of high pressure
The shale gas total content that the amount of the gas reduced in device is in rock sample, the shale gas total content in rock sample is permissible
Calculate according to formula (2):
Vso=(ρ1×V1-ρ2×V1)/ρs (2)
In formula (2),
VsoFor the methane gas in rock sample at the cumulative volume of the status of criterion；
ρ1For opening before the first valve the density of methane gas, ρ in high pressure intermediate receptacle1Count according to formula (3)
Calculate:
V1Volume for high pressure intermediate receptacle；
ρ2For closing after the first valve the density of methane gas, ρ in high pressure intermediate receptacle2Count according to formula (4)
Calculate；
ρsFor methane gas density at standard conditions；
In formula (3) and formula (4),
P1For opening the first manometric reading before the first valve；
P2For closing the first manometric reading after the first valve；
M is the molecular weight of methane gas；
T is the reading of thermometer；
Z1It is P for pressure1Time the compressibility factor of methane gas；
Z2It is P for pressure2Time the compressibility factor of methane gas；
R is constant, and R=0.008314MPa.m3/ (kmol.K).
Owing to having discharged the air in high pressure core holding unit before opening the first valve, open the first valve
After, the methane gas in high pressure intermediate receptacle enters through the first valve and is wrapped in inside the packing element outside rock sample,
And saturated with rock sample, therefore ignore the first valve and to the volume of the pipeline between core holding unit and rock sample with
On the premise of gap between packing element, in rock sample, the shale gas content of free state can be manometric according to the 3rd
The free space volumes of reading change and rock sample calculates, therefore the content of the shale gas of free state in rock sample
Calculate according to formula (5):
Vsy=ρ3×V2/ρs (5)
In formula (5):
VsyFor the methane gas of free state volume at standard conditions in rock sample；
ρ3For the gas density closed after the first valve in high pressure core holding unit, ρ3Calculate according to formula (6):
V2For the free space volumes of high pressure core holding unit, V2Calculate according to formula (7):
V2=φ π d2L/4/100 (7)
ρsFor methane gas density at standard conditions；
In formula (6):
P3For closing the 3rd manometric reading after the first valve；
M is the molecular weight of methane gas；
T is the reading of thermometer；
Z3It is P for pressure3Time the compressibility factor of methane gas；
R is constant, and R=0.008314MPa.m3/ (kmol.K)
In formula (7):
φ is the porosity of rock sample；
D is the diameter of rock sample；
L is the length of rock sample.
The content of the shale gas of adsorbed state calculates according to formula (8):
Vsx=Vso-Vsy (8)
In formula (8):
VsxFor the methane gas of adsorbed state volume at standard conditions in rock sample；
VsoFor the methane gas in rock sample at the cumulative volume of the status of criterion；
VsyFor the methane gas of free state volume at standard conditions in rock sample.
Certainly, skilled person will appreciate that, in order to obtain more accurate measurement result, available first valve
Door replaces in formula (2) to the volume of pipeline between high pressure intermediate receptacle with the volume sum of high pressure intermediate receptacle
The volume V of high pressure intermediate receptacle1, and with the volume of pipeline between the first valve to core holding unit, rock sample
And the free space volumes in the volume in the gap between core holding unit and rock sample replaces the height in formula (5)
The free space volumes V of pressure core holding unit2。
Wherein, the status of criterion refers to that temperature is 0 DEG C (273.15 open) and pressure is 101.325 kPas of (1 standard atmospheres
Pressure, 760 millimetress of mercury) situation.
In step 113, according to the 3rd different manometric reading P3Under shale gas total content, free
The shale gas content of state and the shale gas content of adsorbed state, by the gassiness of display display shale substrate
Property evaluation result, specifically, experimental result is sent to display by single-chip microcomputer after processing experimental data,
Experimental result is shown by display with the form of image or chart.Wherein, as the 3rd manometric reading P3
When reaching formation gas pressure, in rock sample, the shale gas content of storage is stored in subsurface environment closest to rock sample
Adsorbed gas content.
Embodiment four
It is that the method measuring shale substrate gas-bearing property provided according to embodiments of the present invention is to certain rock as shown in Figure 4
Sample carries out testing the experimental result picture of gained, and wherein, transverse axis is the 3rd manometric reading P3, the longitudinal axis be
Shale gas total content in rock sample, the shale gas content of adsorbed state and the suction of free state under this pressure condition
Attached Gas content, wherein, the shale gas content of adsorbed state, along with the rising first increases and then decreases of pressure, is being inhaled
Time at attached Gas content critical point s, the adsorbed gas content in this rock sample reaches maximum, and the shale gas of free state
Content and shale gas total content are all gradually increased along with the rising of pressure.
The invention described above embodiment sequence number, just to describing, does not represent the quality of embodiment.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all the present invention's
Within spirit and principle, any modification, equivalent substitution and improvement etc. made, should be included in the present invention's
Within protection domain.
Claims (9)
1. the device measuring shale substrate air content, it is characterised in that described measurement shale substrate gassiness
The device of amount is for measuring shale gas total content, the shale gas content of free state and the adsorbed state in rock sample
Shale gas content, the device of described measurement shale substrate air content includes calorstat, core holding unit, note
Gas portion, confined pressure portion and thermometer；
By described calorstat simulation down-hole hot environment；
Described core holding unit is arranged in described calorstat, and described rock sample is clamped in described core holding unit；
Described gas injection section is connected with the entrance of described core holding unit, described core holding unit and described gas injection section
Between be provided with the first Pressure gauge and the first valve, and described first Pressure gauge is positioned at described first valve and described
Between gas injection section；
Described confined pressure portion is connected with described core holding unit, described confined pressure portion along the circumference of described rock sample to described
Rock sample applies pressure, is provided with the second valve and the second Pressure gauge between described confined pressure portion and described core holding unit,
Described second Pressure gauge is between described second valve and described core holding unit；
The outlet line of described core holding unit is provided with the 3rd Pressure gauge and the 3rd valve, and described 3rd pressure
Power epi-position is between described core holding unit and described 3rd valve；
Described thermometer is arranged on inside described calorstat, is detected inside described calorstat by described thermometer
Temperature.
The device of measurement shale substrate air content the most according to claim 1, it is characterised in that described
Gas injection section includes gas cylinder, high-pressure pump and high pressure intermediate receptacle；
Described gas cylinder is connected with described high pressure intermediate receptacle through described high-pressure pump, and described high-pressure pump and institute
Stating and be provided with the 4th valve between high pressure intermediate receptacle, described high pressure intermediate receptacle is through described first Pressure gauge and institute
State the first valve to be connected with the entrance of described core holding unit.
The device of measurement shale substrate air content the most according to claim 1, it is characterised in that described
Confined pressure portion is hydraulic pump.
The device of measurement shale substrate air content the most according to claim 1, it is characterised in that described
The device measuring shale substrate air content also includes single-chip microcomputer and display；
Described single-chip microcomputer and described thermometer, described first Pressure gauge, described second Pressure gauge and the described 3rd
Pressure gauge connects, and calculates temperature that described rock sample shows at described thermometer and described the by described single-chip microcomputer
Shale gas total content, the shale gas content of free state and adsorbed state under the confined pressure that two Pressure gauges show
Shale gas content；
Described display is connected with described single-chip microcomputer, is shown that by described display the calculating of described single-chip microcomputer is tied
Really.
The device of measurement shale substrate air content the most according to claim 1, it is characterised in that described
Core holding unit includes fixing cylinder and packing element, wraps up described rock sample by described packing element, by described fixing cylinder
Clamp described rock sample, and described packing element is positioned at inside described fixing cylinder.
6. according to the device measuring shale substrate air content described in claim 1-5 any one claim,
It is characterized in that, described rock sample is cylinder, and a diameter of 2.5 centimetres or 7 cun of described rock sample, described rock sample
Length between 2.5～7.6 centimetres.
7. the method measuring shale substrate air content, it is characterised in that described measurement shale substrate gassiness
The device measuring shale substrate air content described in the method application claim 1-6 any one claim of amount,
The method of described measurement shale substrate air content comprises the steps:
Step 100: connect and correct the device of described measurement shale substrate air content；
Step 200: rock sample is fixed in core holding unit；
Step 300: get rid of the air in the device of described measurement shale substrate air content, and close all valves；
Step 400: open the second valve, adds confined pressure by confined pressure portion to rock sample, until the second manometric reading
When number reaches to preset confined pressure, close the second valve；
Step 500: open the 4th valve, the methane gas in gas cylinder is pumped into and holds in the middle of high pressure by high-pressure pump
In device, when the first manometric reading reaches preset pressure, close the 4th valve；
Step 600: record the first manometric reading P1After open the first valve, make in high pressure intermediate receptacle
Methane gas enter in rock sample, after the first manometric reading is reduced to certain limit, close the first valve
Door, records the first manometric reading P2, until after the 3rd manometric stable reading, recording the 3rd pressure
The reading P of table3；
Step 700: judge the 3rd manometric reading P3Whether reach formation gas pressure, when the 3rd Pressure gauge
Reading P3When reaching formation gas pressure, enter step 800, as the 3rd manometric reading P3Not up to
During formation gas pressure, enter step 600；
Step 800: process experimental data, provide the gassiness evaluation result of shale substrate.
The method of measurement shale substrate air content the most according to claim 7, it is characterised in that described
Preset confined pressure to calculate according to equation below (1):
P=Z × g × ρR×10-6 (1)
Wherein:
P is confined pressure；
Z is the vertically layer depth of described rock sample position；
ρRDensity for described rock sample；
G is acceleration of gravity.
The method of measurement shale substrate air content the most according to claim 7, it is characterised in that described
Step 800: processing experimental data, the gassiness evaluation result providing shale substrate includes:
According to the first manometric reading P1, the first manometric reading P2With the 3rd manometric reading P3Meter
Calculate at the 3rd manometric reading P3Under, the shale gas total content in rock sample, the shale gas content of free state
Shale gas content with adsorbed state；
According to the 3rd different manometric reading P3Under shale gas total content, the shale gas of free state contains
The shale gas content of amount and adsorbed state provides the gassiness evaluation result of shale substrate.
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| CN106840536A (en) * | 2017-01-25 | 2017-06-13 | 中国地质大学（北京） | A kind of shale rock sample device for detecting sealability and its method for conducting leak test |
| CN108872529A (en) * | 2018-04-12 | 2018-11-23 | 中国石油大学(北京) | For measuring shale rupture methane lost imitative experimental appliance and its method |
| CN110095375A (en) * | 2019-05-14 | 2019-08-06 | 中国石油大学(北京) | Shale air content test device and method |
| CN111122380A (en) * | 2019-12-25 | 2020-05-08 | 中煤科工集团重庆研究院有限公司 | Device and method for measuring gas content of rock |
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| CN106840536A (en) * | 2017-01-25 | 2017-06-13 | 中国地质大学（北京） | A kind of shale rock sample device for detecting sealability and its method for conducting leak test |
| CN108872529A (en) * | 2018-04-12 | 2018-11-23 | 中国石油大学(北京) | For measuring shale rupture methane lost imitative experimental appliance and its method |
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| CN111122380B (en) * | 2019-12-25 | 2022-08-23 | 中煤科工集团重庆研究院有限公司 | Device and method for measuring gas content of rock |
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| CN113670768A (en) * | 2021-08-18 | 2021-11-19 | 中国石油大学(北京) | Method, device and system for determining sea phase shale in-situ gas volume recovery |
| CN113670769A (en) * | 2021-08-18 | 2021-11-19 | 中国石油大学(北京) | Method for simulating gas content change in marine shale stratum lifting process |
| CN113670769B (en) * | 2021-08-18 | 2022-10-18 | 中国石油大学(北京) | Method for simulating gas content change in marine shale stratum lifting process |
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