CN112345020B - Device and method for measuring shale loss and desorption - Google Patents

Device and method for measuring shale loss and desorption Download PDF

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Publication number
CN112345020B
CN112345020B CN201910728573.9A CN201910728573A CN112345020B CN 112345020 B CN112345020 B CN 112345020B CN 201910728573 A CN201910728573 A CN 201910728573A CN 112345020 B CN112345020 B CN 112345020B
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sealed container
gas
shale
liquid
inner cavity
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CN112345020A (en
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端祥刚
胡志明
熊伟
常进
沈瑞
顾兆斌
陈学科
周广照
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Petrochina Co Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01FMEASURING VOLUME, VOLUME FLOW, MASS FLOW OR LIQUID LEVEL; METERING BY VOLUME
    • G01F22/00Methods or apparatus for measuring volume of fluids or fluent solid material, not otherwise provided for

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Abstract

The invention discloses a device and a method for measuring shale loss and desorption, wherein the device for measuring shale loss and desorption comprises the following components: a constant temperature system; a sealed container for placing the rock core and shale non-wetting liquid, wherein the sealed container is placed in a constant temperature system; a constant pressure displacement system connected to the inlet and outlet ends of the sealed vessel; and the inlet end of the gas-liquid metering system is connected with the outlet end of the constant-pressure displacement system. The invention also provides a method for measuring shale loss and desorption. The invention provides a device and a method for measuring shale loss gas and desorption gas, which establish an experimental device for recovering shale loss gas, and can accurately measure the loss gas and desorption gas in real time under the temperature and the pressure of a reservoir without calculation through a formula.

Description

Device and method for measuring shale loss and desorption
Technical Field
The invention relates to the technical field of shale gas exploration and development. And more particularly to an apparatus and method for measuring shale loss and de-inspiratory capacity.
Background
As an unconventional gas reservoir with great development potential, shale gas occurs in a different mode from the conventional gas reservoir, the shale gas mainly takes a free state and an adsorption state, the free gas mainly occurs in cracks, matrix pores or organic matter nanopores of a shale reservoir, and the adsorption gas mainly occurs on the surfaces of kerogen, clay particles and pores. Shale gas content is an important parameter for evaluating shale gas reservoir reserves, and has important influence on aspects such as optimizing shale gas reservoirs, designing shale gas development schemes and the like. Because the proportion of the dissolved gas in the shale gas reservoir is very small, the contribution of the dissolved gas to the shale gas content is generally ignored, and only the adsorbed gas and the free gas are considered.
The gas content determination includes in situ desorption, isothermal adsorption and well logging interpretation. The in-situ desorption method is the most direct method for measuring the total gas content of the shale, can reflect the gas content characteristics of the shale under the condition of simulating the actual environment of the stratum, is a basic method for measuring the gas content of the shale, and is usually completed in a coring site. The gas content measured by the desorption method consists of 3 parts, namely a loss gas amount, a desorption gas amount and a residual gas amount. The loss gas quantity is a main component of shale gas quantity, and the loss gas quantity is larger than 50% when the shale gas quantity of five peak groups-Longmaxi groups in Fuling basin areas of Sichuan of China is measured. The desorption gas quantity refers to the total quantity of gas desorbed after the core is filled into a desorption tank, and the desorption can be stopped when the average desorption quantity is smaller than 10cm 3/d in 1 week; the residual gas quantity refers to the part of gas still remained in the sample after the desorption is stopped, the gas quantity is generally smaller, the rock sample is required to be put into a closed ball milling tank for breaking, then the rock sample is put into a constant temperature device, the gas desorption is repeatedly carried out according to a specified time interval after the temperature of the reservoir is recovered, until the gas quantity of continuous 1 week desorption is smaller than 10cm 3/d, and the residual gas quantity is measured.
The accuracy of the calculation of the loss gas directly affects the accuracy of the measurement of the total gas content, and since the loss gas cannot be directly measured through experiments, the calculation is usually performed by using an empirical formula between the accumulated desorption gas under the slurry temperature condition and the square root of the desorption time, and the main method is as follows: USBM method, smith-Williams method, polynomial regression method, nonlinear regression method, and the like. At present, the gas content of shale is generally reversely calculated through the data of on-site desorption of a desorption tank after coring, but the gas is lost before the core is put into the desorption tank, and the loss rule cannot be confirmed; in addition, the amount of the lost gas and the loss law are affected by a plurality of factors such as a coring mode, a measuring method, an estimating method and the like, so that the method has larger workload and higher cost, and the obtained gas content is greatly different from the actual gas content.
Accordingly, the present invention provides an apparatus and method for measuring shale loss and desorption, to solve the above-mentioned problems.
Disclosure of Invention
It is an object of the present invention to provide a device for measuring shale loss and de-inspiratory capacity. The invention establishes an experimental device for recovering shale loss gas, and can accurately measure the loss gas amount and the desorption gas amount in real time under the reservoir temperature and the reservoir pressure without calculation through a formula.
It is another object of the present invention to provide a method of measuring shale loss and de-inspiratory capacity.
In order to achieve the above purpose, the invention adopts the following technical scheme:
An apparatus for measuring shale loss and de-inspiratory capacity, comprising:
The constant temperature system is used for keeping the sealed container in a constant temperature state;
A sealed container for placing the rock core and shale non-wetting liquid, wherein the sealed container is placed in a constant temperature system;
the constant-pressure displacement system is connected with the inlet end and the outlet end of the sealed container and is used for keeping the sealed container in a constant-pressure state all the time in the displacement process; and
And the inlet end of the gas-liquid metering system is connected with the outlet end of the constant-pressure displacement system and is used for metering the gas outlet quantity and the liquid outlet quantity in the sealed container.
Preferably, a permeable net is arranged in the inner cavity of the sealed container to divide the inner cavity of the sealed container into an upper inner cavity and a lower inner cavity.
Preferably, the permeable mesh is a stainless steel mesh.
Preferably, when the sealed container is used for placing the core and shale non-wetting liquid, the core is placed in an upper inner cavity of the sealed container, and the shale non-wetting liquid is placed in a lower inner cavity of the sealed container.
Preferably, the shale non-wetting liquid is white oil or oil-based mud.
Preferably, a piston for driving shale non-wetting liquid to rise is further arranged in the lower inner cavity of the sealed container.
Preferably, a chamfer wall is arranged between the top wall and the side wall of the inner cavity of the sealed container, so that bubbles are prevented from being accumulated at the top end and cannot be removed.
Preferably, the sealed container is made of 316L material and has a pressure resistance of 0-70MPa.
Preferably, the constant temperature system is a high temperature incubator with a temperature range of 0-150 ℃.
Preferably, the constant pressure displacement system is a group of reciprocating constant pressure displacement pumps, and has constant pressure injection and constant pressure liquid pumping modes, and the pressure range is 0-50MPa.
Preferably, the gas-liquid metering system is a sealed water container having a volume of at least 3L. According to the invention, the weight of the water discharged from the gas-liquid metering system is continuously measured by a balance weighing method, so that the gas-liquid amount is continuously and accurately metered.
The invention also provides a method for measuring shale loss and inspiration by using the device, which comprises the following steps:
Step one, placing a core sample with original water saturation in an upper inner cavity of a sealed container, and placing shale non-wetting liquid in a lower inner cavity of the sealed container;
heating the sealed container to the stratum temperature corresponding to the core sample sampling reservoir by adopting a constant temperature system;
Injecting shale gas into the sealed container until the pressure in the sealed container is the formation pressure corresponding to the core sample sampling reservoir;
Step four, adopting a constant-pressure displacement system, and rising the liquid level of shale non-wetting liquid to an upper inner cavity filled with the sealing container until the liquid flow at the outlet end of the sealing container is stable, and closing the constant-pressure displacement system; the stable liquid flow at the outlet end of the sealed container means that no bubbles are generated at the outlet end of the sealed container;
Step five, opening the sealed container, measuring the volumes of the exhaust gas and the liquid in the sealed container by adopting a gas-liquid metering system, and measuring the total volume of the exhaust gas and the liquid obtained by measurement as the loss gas volume when the pressure in the sealed container is reduced to 0;
And step six, after the pressure in the sealed container is reduced to 0, continuously measuring the volume of the exhaust gas in the sealed container by adopting a gas-liquid metering system, and ending the measurement when the average gas production rate in 1 week is less than 10cm 3/d, wherein the volume of the obtained exhaust gas is the desorption gas volume.
Preferably, in the first step, a permeable net is disposed in the sealed container to divide the inner cavity of the sealed container into an upper inner cavity and a lower inner cavity.
Preferably, the shale gas in step three comprises methane, ethane, carbon dioxide and nitrogen;
Further, in the shale gas, the volume of methane accounts for at least 98% of the total volume; the sum of the volumes of ethane, carbon dioxide and nitrogen accounts for 0.5-1% of the total volume.
Preferably, in the fourth step, a constant pressure displacement system is adopted to raise the liquid level of the shale non-wetting liquid to be full of the sealed container, which specifically comprises:
And driving a piston in the sealed container by adopting a constant-pressure displacement system, and lifting the liquid level of the shale non-wetting liquid to an upper inner cavity filled in the sealed container.
Preferably, in the fifth step, the volumes of the exhaust gas and the liquid in the sealed container are measured by using a gas-liquid metering system, specifically: the volumes of the discharged gas and liquid in the sealed container are measured by a balance weighing method by adopting a gas-liquid metering system.
Preferably, after the pressure in the sealed container in the step six is reduced to 0, the volume of the exhaust gas in the sealed container is continuously measured by adopting a gas-liquid metering system, specifically: and after the pressure in the sealed container is reduced to 0, continuously measuring the volume of the discharged gas in the sealed container by adopting a gas-liquid metering system through a balance weighing method.
Preferably, the method for measuring shale loss and inspiration further comprises the step of measuring shale residual gas after measuring shale loss and inspiration, and specifically comprises the following steps:
Taking out a core sample, measuring basic parameters of the core sample, and obtaining residual gas by adopting a crushing method; and the sum of the loss gas quantity, the desorption gas quantity and the residual gas quantity is the gas content of the core sample.
Preferably, the basic parameters of the core sample include length, diameter, and weight.
The beneficial effects of the invention are as follows:
The invention provides a device and a method for measuring shale loss gas and desorption gas, which establish an experimental device for recovering shale loss gas, and can accurately measure the loss gas and desorption gas in real time under the temperature and the pressure of a reservoir without calculation through a formula.
Drawings
The following describes the embodiments of the present invention in further detail with reference to the drawings.
FIG. 1 shows a schematic diagram of an apparatus for measuring shale loss and desorption according to the present invention;
FIG. 2 shows a graph of shale gas content over time for example 1 of the present invention;
the device comprises a 1-constant temperature system, a 2-sealed container, a 21-core, a 22-shale non-wetting liquid, a 23-permeable net, a 24-piston, a 25-chamfer wall, a 3-constant pressure displacement system and a 4-gas-liquid metering system.
Detailed Description
In order to more clearly illustrate the present invention, the present invention will be further described with reference to preferred embodiments. It is to be understood by persons skilled in the art that the following detailed description is illustrative and not restrictive, and that this invention is not limited to the details given herein.
The method has the advantages that the workload is large, the cost is high, the obtained gas content is greatly different from the actual gas content, and the device for measuring the shale gas loss and the desorption quantity is simple and easy to measure, so that the obtained gas loss and desorption quantity are accurate.
Specifically, referring to fig. 1, an apparatus for measuring shale loss and desorption, includes:
a constant temperature system 1 for keeping the sealed container in a constant temperature state;
a sealed container 2 for placing a core 21 and shale non-wetting fluid 22, the sealed container 2 being placed within the thermostatic system 1;
A constant pressure displacement system 3 connected to the inlet and outlet ends of the sealed container 2 for maintaining the sealed container 2 in a constant pressure state throughout the displacement process; and
And the gas-liquid metering system 4 is connected with the outlet end of the constant-pressure displacement system 3 at the inlet end and is used for metering the gas outlet quantity and the liquid outlet quantity in the sealed container 2.
As a preferred embodiment of the present invention, the inner cavity of the sealed container 2 is provided with a permeable net 23 for dividing the inner cavity of the sealed container 2 into an upper inner cavity and a lower inner cavity; further, the permeable net 23 is a stainless steel net.
As a preferred embodiment of the present invention, when the sealed container 2 is used for placing the core 21 and the shale non-wetting fluid 22, the core 21 is placed in an upper inner cavity of the sealed container 2, and the shale non-wetting fluid 22 is placed in a lower inner cavity of the sealed container 2; further, the shale non-wetting liquid is white oil or oil-based mud.
As a preferred embodiment of the present invention, a piston 24 is further disposed in the lower cavity of the sealed container 2, and the piston 24 is located below the shale non-wetting fluid 22 and is used for driving the shale non-wetting fluid to rise.
As a preferred embodiment of the present invention, a chamfer wall 25 is provided between the top wall and the side wall of the cavity of the sealed container 2, so as to avoid air bubbles from collecting at the top end and being unable to be removed.
As a preferred embodiment of the present invention, the sealed container 2 is made of 316L material and has a pressure resistance of 0-70MPa.
As a preferred embodiment of the present invention, the constant temperature system 1 is a high temperature incubator with a temperature range of 0-150 ℃.
As a preferred embodiment of the present invention, the constant pressure displacement system 3 is a set of reciprocating constant pressure displacement pumps, and has constant pressure injection and constant pressure pumping modes, and the pressure ranges from 0MPa to 50MPa.
As a preferred embodiment of the present invention, the gas-liquid metering system 4 is a sealed water container having a volume of at least 3L. According to the invention, the weight of the water discharged from the gas-liquid metering system is continuously measured by a balance weighing method, so that the gas-liquid amount is continuously and accurately metered.
As another aspect of the invention, the invention also provides a method for measuring shale loss and inspiration by using the device, which comprises the following steps:
s101, placing a core sample with original water saturation in an upper inner cavity of a sealed container 2, and placing shale non-wettability liquid 22 in a lower inner cavity of the sealed container 2; the core sample with the original water saturation can be a field coring fresh rock sample or a dry core to establish the original water saturation;
S102, heating the sealed container 2 to the stratum temperature corresponding to the core sample sampling reservoir by adopting the constant temperature system 1;
S103, injecting shale gas into the sealed container 2 until the pressure in the sealed container 2 is the formation pressure corresponding to the rock core sample sampling reservoir, wherein the formation pressure is generally 30-50 MPa, and stopping saturation when the pressure variation amplitude in the sealed container 2 is less than 0.1 MPa; the shale gas can be directly injected by adopting wellhead produced gas, or is injected after being prepared by adopting all pure gases according to the analysis result of a gas sample;
S104, adopting a constant-pressure displacement system 3, lifting the liquid level of shale non-wetting liquid 22 to the upper inner cavity filled with the sealed container 2, controlling the pressure of the sealed container 2 to be kept at the stratum pressure, measuring the liquid amount at the outlet end of the sealed container 2, and closing the constant-pressure displacement system 3 until the liquid flow at the outlet end of the sealed container 2 is stable; in the step, the stable flow of the liquid at the outlet end of the sealed container 2 means that no bubbles are generated at the outlet end of the sealed container 2;
S105, opening the sealed container 2, measuring the volumes of the exhaust gas and the liquid in the sealed container 2 by adopting a gas-liquid metering system 4, and ending the measurement when the pressure in the sealed container 2 is reduced to 0, wherein the total volume of the obtained exhaust gas and liquid is the loss gas quantity;
And S106, after the pressure in the sealed container 2 is reduced to 0, continuously measuring the volume of the exhaust gas in the sealed container 2 by adopting a gas-liquid metering system 4, and ending the measurement when the average gas production rate in 1 week is less than 10cm 3/d, wherein the volume of the obtained exhaust gas is the desorption gas volume.
As a preferred embodiment of the present invention, in step S101, the inside of the sealed container 2 is provided with a permeable net 23 dividing the inner cavity of the sealed container 2 into an upper inner cavity and a lower inner cavity.
As a preferred embodiment of the present invention, the shale gas in step S103 includes methane, ethane, carbon dioxide and nitrogen.
As a preferred embodiment of the present invention, the step S104 of raising the level of the shale non-wetting fluid 22 to fill the sealed container 2 by using the constant pressure displacement system 3 specifically comprises:
With constant pressure displacement system 3, piston 24 within sealed vessel 2 is driven to raise the level of shale non-wetting fluid 22 to fill the upper internal cavity of sealed vessel 2.
As a preferred embodiment of the present invention, the measurement of the volumes of the exhaust gas and the liquid in the sealed container 2 using the gas-liquid metering system 4 in step S105 is specifically: the volumes of the discharged gas and liquid in the sealed container 2 are measured by a balance weighing method by using a gas-liquid metering system 4.
As a preferred embodiment of the present application, after the pressure in the sealed container 2 drops to 0 in step S106, the gas-liquid metering system 4 is used to continuously measure the volume of the exhaust gas in the sealed container 2, specifically: after the pressure in the sealed container 2 is reduced to 0, the gas-liquid metering system 4 is adopted to continuously measure the volume of the discharged gas in the sealed container 2 through a balance weighing method. It should be understood by those skilled in the art that the balance weighing method is a conventional technical method, and the present application will not be described in detail.
As a preferred embodiment of the present invention, the method for measuring shale loss and desorption rate further comprises the step of measuring shale residual gas after measuring shale loss and desorption rate, specifically comprising:
Taking out a core sample, measuring basic parameters of the core sample, and obtaining residual gas by adopting a crushing method; and the sum of the loss gas quantity, the desorption gas quantity and the residual gas quantity is the gas content of the core sample. It should be understood by those skilled in the art that the pulverization method is a conventional technical method, and the present application will not be described in detail.
As a preferred embodiment of the present invention, the basic parameters of the core sample include length, diameter and weight.
The following is a further explanation of the present invention by way of examples.
Example 1
The embodiment provides a method for measuring shale loss gas and desorption gas, which uses a device shown in fig. 1, and specifically comprises the following steps:
1) Placing a core sample with original water saturation in an upper inner cavity of a sealed container, and placing shale non-wetting liquid in a lower inner cavity of the sealed container;
2) Heating the sealed container to 95 ℃ of the stratum temperature corresponding to the core sample sampling reservoir by adopting a constant temperature system;
3) Injecting shale gas into the sealed container, wherein the shale gas comprises 99vol% of methane and 1vol% of other gases, the other gases are ethane, carbon dioxide and nitrogen, and the pressure in the sealed container is 30MPa of the formation pressure corresponding to the core sample sampling reservoir;
4) Driving a piston in a sealed container by adopting a constant-pressure displacement system, lifting the liquid level of shale non-wetting liquid to an upper inner cavity filled with the sealed container, controlling the pressure of the sealed container to be 30MPa by adopting the constant-pressure displacement system, measuring the liquid amount at the outlet end of the sealed container until the liquid flow at the outlet end of the sealed container is stable, and closing the constant-pressure displacement system until the liquid flow at the outlet end of the sealed container is stable;
5) Opening the sealed container, recording the discharged liquid amount in real time through an electronic balance, recording the discharged gas amount in real time through a drainage method, ending measurement when the pressure in the sealed container is reduced to 0, and obtaining the total volume of the discharged gas and the liquid as the loss gas amount; as shown in FIG. 2, the amount of the measured loss gas was 509ml;
6) After the pressure in the sealed container is reduced to 0, continuously measuring the volume of the exhaust gas in the sealed container by adopting a gas-liquid metering system, ending the measurement when the average gas production rate in 1 week is less than 10cm 3/d, wherein the volume of the obtained exhaust gas is the desorption gas volume; the amount of desorption gas at this stage was 292ml;
7) Core samples were taken, basic parameters of the core samples including length, diameter and weight were measured, the calculated loss gas amount was 4.24m 3/t, and the desorption gas amount was 2.43m 3/t, as shown in FIG. 2.
It should be understood that the foregoing examples of the present invention are provided merely for clearly illustrating the present invention and are not intended to limit the embodiments of the present invention, and that various other changes and modifications may be made therein by one skilled in the art without departing from the spirit and scope of the present invention as defined by the appended claims.

Claims (4)

1. A method for measuring shale loss and desorption, the method being characterized in that the method is carried out using a device for measuring shale loss and desorption;
the device for measuring shale loss and inspiration comprises:
a constant temperature system;
A sealed container for placing the rock core and shale non-wetting liquid, wherein the sealed container is placed in a constant temperature system;
a constant pressure displacement system connected to the inlet and outlet ends of the sealed vessel; and
The inlet end of the gas-liquid metering system is connected with the outlet end of the constant-pressure displacement system;
The inner cavity of the sealed container is provided with a permeable net which divides the inner cavity of the sealed container into an upper inner cavity and a lower inner cavity, the rock core is placed in the upper inner cavity of the sealed container, and the shale non-wetting liquid is placed in the lower inner cavity of the sealed container; a piston is arranged in the lower inner cavity of the sealed container;
The method comprises the following steps:
Step one, placing a core sample with original water saturation in an upper inner cavity of a sealed container, and placing shale non-wetting liquid in a lower inner cavity of the sealed container;
heating the sealed container to the stratum temperature corresponding to the core sample sampling reservoir by adopting a constant temperature system;
Injecting shale gas into the sealed container until the pressure in the sealed container is the formation pressure corresponding to the core sample sampling reservoir;
Step four, adopting a constant-pressure displacement system, rising the liquid level of shale non-wetting liquid to an upper inner cavity filled with a sealed container, controlling the pressure of the sealed container to be kept at the stratum pressure, and closing the constant-pressure displacement system until the liquid flow at the outlet end of the sealed container is stable; wherein, adopt constant pressure displacement system, rise shale non-wettability liquid level to full sealed container, include: driving a piston in the sealed container by adopting a constant-pressure displacement system, and lifting the liquid level of shale non-wetting liquid to an upper inner cavity filled in the sealed container;
Step five, opening the sealed container, measuring the volumes of the exhaust gas and the liquid in the sealed container by adopting a gas-liquid metering system, ending the measurement when the pressure in the sealed container is reduced to 0, wherein the total volume of the obtained exhaust gas and liquid is the loss gas volume;
And step six, after the pressure in the sealed container is reduced to 0, continuously measuring the volume of the exhaust gas in the sealed container by adopting a gas-liquid metering system, and ending the measurement when the average gas production rate in1 week is less than 10cm < 3 >/d, wherein the volume of the obtained exhaust gas is the desorption gas volume.
2. The method of measuring shale loss and de-inspiratory capacity of claim 1, wherein the permeable mesh is a stainless steel mesh.
3. The method of measuring shale loss and de-inspiratory capacity of claim 1, wherein the shale non-wetting liquid is white oil or oil-based mud.
4. The method of measuring shale loss and de-inspiratory capacity of claim 1, wherein a chamfer wall is provided between the top wall and the side wall of the interior cavity of the sealed container.
CN201910728573.9A 2019-08-08 2019-08-08 Device and method for measuring shale loss and desorption Active CN112345020B (en)

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