RU2796085C1 - Installation for measuring volume change of solid materials of organic and inorganic nature and method of carrying out such measurements - Google Patents

Abstract

FIELD: oil and gas industry; production of various plastic materials.

SUBSTANCE: invention is related in particular to installation and method for determining the degree of swelling and swelling kinetics of a substance in various media in a wide range of thermobaric conditions. The installation for measuring the change in the volume of solid materials of organic and inorganic nature over time includes a heating cabinet, two piston tanks hydraulically connected to each other and to a vacuum pump, installed in a heating cabinet, each said tank is also connected to its own high-pressure pump, with one of the containers made in form of a container with the tested fluid, and the second one is made in form of a container with the tested solid material, and in the container with the tested solid material there is a cell containing a bottom, a side cylindrical surface and a lid, and a metal mesh is installed in the cell under the lid, and through holes are made in its side and bottom surfaces. A method for measuring the change in the volume of solid materials of organic and inorganic nature over time is also claimed.

EFFECT: providing high-precision measurement of swelling of solid materials of organic and inorganic nature in various media in a wide range of thermobaric conditions.

10 cl, 5 dwg

Description

The field of technology to which the invention belongs

The invention relates to the oil and gas industry, as well as to the production of various plastic materials, and in particular to an installation and a method for determining the degree of swelling and swelling kinetics of a substance in various media in a wide range of thermobaric conditions.

State of the art

The Zhigach-Yarov device and models based on it are widely known [RU57006U1, 27.09.2006]. The principle of operation of this device is based on the movement of the piston during the expansion of the rock brought into contact with water. This piston is connected by means of a rod to a linear displacement sensor, the readings of which are determined as the degree of swelling. The disadvantages of this device are the impossibility of measurements at elevated (>40°C) temperatures and pressures other than atmospheric; the impossibility of measuring the swelling of poorly swelling substances; lack of physical meaning of the obtained quantity; the impossibility of obtaining data on the amount of liquid that interacted with the rock.

A device is known [RU119887U1, 27.08.2012], in which liquid is supplied to the measuring cell from a second tank, by changing the liquid level in which a conclusion is made about the amount of liquid that has interacted with the rock. The disadvantages are the impossibility of measurements under reservoir conditions, the impossibility of measuring the swelling of poorly swelling substances.

Known device [SU1012098A, 15.04.1983] for measuring the swelling of solid particles, also based on the displacement of the piston. In contrast to the devices described earlier, this setup uses a balancer in the form of an inverted cup placed on the particles under study, with a mesh at the end. This balancer drives a piston that pushes the water into the measuring tank. The disadvantage of the described approach is also the impossibility of measurement under reservoir conditions.

The closest physical analogue is the device [SU163789A1, 00.00.1964]. The test substance is placed in a device with a rod that is connected to a pen brought into contact with a foil on the inside of a cylindrical drum that rotates at an extremely slow speed. The required liquid pressure is supplied to the drum through the hydraulic system and placed in a heating cabinet. After the experiment, the foil is taken out and the kinetics of the change in the volume of the studied substance is determined from the obtained curve. The disadvantages of the design are the inability to provide high-precision measurement of swelling, extremely high metal consumption, technical complexity and difficulty in interpreting the results.

The claimed invention eliminates the above disadvantages.

Disclosure of invention

The technical problem is to create a solution for high-precision measurement of the swelling of solid materials of organic and inorganic nature in various media with high accuracy in a wide range of thermobaric conditions, while being technically simplified, having a low metal content and providing ease of interpretation of the results.

The technical result consists in providing high-precision measurement of the swelling of solid materials of organic and inorganic nature in various media in a wide range of thermobaric conditions.

The technical result is achieved due to the fact that the installation for measuring the change in the volume of solid materials of organic and inorganic nature over time includes a heating cabinet, two piston tanks hydraulically connected to each other and with a vacuum pump installed in the heating cabinet, each said container is also connected to its own high-pressure pump, wherein one of the containers is made in the form of a container with the investigated fluid, and the second is made in the form of a container with the investigated solid material, and a cell is installed in the container with the investigated solid material, having a bottom, a side cylindrical surface and a cover, and in the cell a metal mesh is installed under the cover, and through holes are made on its side and bottom surfaces.

In addition, the cell cover is made freely moving with through holes.

In addition, the cell is installed in a piston container with the investigated solid material in such a way that the cell lid is in close contact with the lid of this piston container.

In addition, high pressure pumps are designed to operate in constant pressure mode using a PID controller and thermally stabilized hydraulic fluid, both for compressing and supplying fluid, and for measuring volume change.

In addition, the piston tanks are made of metal.

A method for measuring the change in the volume of solid materials of organic and inorganic nature over time using an installation containing a heating cabinet, two containers hydraulically connected to each other and to a vacuum pump with pistons for compressing and supplying fluid and for measuring the volume of swelling, installed in a heating cabinet, each of which is connected to its own high pressure pump, and a cylindrical cell with the investigated solid material includes the following steps:

the test solid material is placed in the cell for measuring swelling;

the cell with the test solid material is loaded into the first piston tank for measuring swelling, which is closed, placed in a heating cabinet, connected to the first high-pressure pump, and the pressure in the under-piston space of the tank with the test solid material is increased to a pressure higher than atmospheric by 0.1 MPa;

then, the test fluid is placed in the second piston container;

close the second piston tank with the test fluid, place it in a heating cabinet, connect it to the second high-pressure pump, and raise the pressure in the sub-piston space of the tank with the test fluid to the test pressure;

include a heating cabinet, heating it to the required temperature, and a vacuum pump, after which the installation is thermally stabilized for several hours;

the piston container containing the test solid material is evacuated for several hours, after which the fluid is launched into the piston container with the test solid material, and then the fluid pressure is again raised to the required value;

further, the high-pressure pump connected to the piston tank with the investigated solid material is switched to the operating mode of maintaining a constant pressure with the required setting, while the high-pressure pump connected to the piston tank with the test fluid is also switched to the operating mode with the same setting.

for several days, the change in the volume of water pumped out by the pump is recorded, and the change in the volume of the investigated solid material is measured.

In addition, the cell is loaded into the piston container with the test solid material in such a way that the lid of the swelling cell is in close contact with the lid of the piston container.

In addition, both containers are interconnected by a hydraulic line.

In addition, the thermal stabilization of the installation is carried out for twelve hours.

In addition, the piston container containing the test solid material is evacuated for three hours.

Brief description of the drawings

Fig. 1 - General layout of the installation;

Fig. 2 - Diagram of a cell for measuring swelling;

Fig. 3 - Dependence of the degree of swelling of bentonite in NaOH solution on time at 40°C and 15 MPa;

Fig. 4 - Dependence of the degree of swelling of rubber in CO2 on time at 90°C and 15 MPa;

Fig. 5 - Dependence of the degree of swelling of shale rock in NaOH solution on time at 110°C and 12 MPa.

The figures indicate the following elements:

1 - needle valve with outlet to the vacuum pump;

2,3 - needle valves;

4 - piston tank with the studied fluid;

5 - piston container with the investigated solid material;

6 - cell for measuring swelling with the investigated solid material;

7 - test fluid;

8.9 - needle valves;

10, 11 - high pressure pumps;

12 - heating cabinet;

13 - vacuum pump;

14 - test material;

15 - metal meshes (200 mesh);

16 - freely moving cover with through holes;

17 - through holes in the cell wall;

18 - groove on the side wall of the cell;

19 - cell bottom with through holes;

20 - lateral cylindrical surface.

Implementation of the invention

The claimed installation for measuring the change in the volume of solid materials of organic and inorganic nature over time, includes a heating cabinet, high-pressure pumps, a vacuum pump, a cylindrical cell with a freely moving lid, a metal mesh and holes on the side and bottom surfaces, metal containers with pistons for compression and fluid supply and to measure the amount of swelling.

The invention is explained with the help of the following examples of measurements and is illustrated by figures 1-4.

The installation contains, located in the heating cabinet 12, two hydraulically connected piston tanks 4 and 5 for compressing and supplying fluid and for measuring the volume of swelling, each of which is hydraulically connected to its own high-pressure pump 10 and 11.

One of these containers 4 is designed for the test fluid 7, in the second container 5 there is a cylindrical cell 6 for measuring swelling, filled with the test solid material 14.

The cell 6 contains a bottom 19, a side cylindrical surface 20, a lid 16 and a metal mesh 15. The lid is made freely moving with through holes. Through holes are also made on the side and bottom surfaces. Holes in the side surface contribute to additional uniform wetting of the entire solid material by the fluid. A metal mesh can also be installed at the bottom of the cell. The metal meshes are designed to prevent the dispersion of rock from the cell.

The cell can be made from chemically and heat resistant PEEK (polyether ether ketone) polymer.

The high pressure pumps 10 and 11 are configured to operate in a constant pressure mode using a PID controller and thermally stabilized hydraulic fluid to compress and supply fluid and measure swelling.

Connection of elements among themselves hydraulic, by means of pipelines. To close and open the liquid supply, appropriate valves are provided, for example, needle valves, installed in the places necessary for this, for example, between tanks, pumps and tanks, in fact, as shown in Fig. 1.

EFFECT: invention makes it possible to measure the change in the volume of solid materials of organic and inorganic nature over time in organic and inorganic environments in the temperature range of 20-150°C and pressures of 0-70 MPa.

The method for carrying out measurements using the above installation in general includes preparing samples and installation, bringing to reservoir conditions, filling the cell with liquid, holding at reservoir conditions until the change in fluid volume stops. The used cell with a metal mesh filled with the investigated solid is placed in a piston tank with a pump connected to it, which acts as a means of measuring the change in the volume of the substance when interacting with the injected fluid. Fluid supply at elevated pressure is provided by a second pump. The creation of elevated temperatures is ensured by placing the components of the device in a heating cabinet.

More precisely, the method of carrying out measurements using the above installation, containing a heating cabinet, two piston tanks for compression and supply of fluid and for measuring the volume of swelling, installed in a heating cabinet, each of which is connected to its own high-pressure pump, a vacuum pump and a cylindrical cell with a test hard material, includes the following steps:

the test solid material is placed in the cell for measuring swelling;

the cell with the test solid material is loaded into the first piston vessel for measuring swelling, which is closed, placed in a heating cabinet, connected to the first high-pressure pump, and the pressure in the under-piston space of the vessel with the test solid material is raised to a pressure higher than atmospheric by 0.1 MPa;

then, the test fluid is placed in the second piston container;

close the second piston tank with the test fluid, place it in a heating cabinet, connect it to the second high-pressure pump, and raise the pressure in the sub-piston space of the tank with the test fluid to the test pressure;

include a heating cabinet, heating it to the required temperature, and a vacuum pump, after which the installation is thermally stabilized for several hours;

the piston container containing the test solid material is evacuated for several hours, after which the fluid is launched into the piston container with the test solid material, and then the fluid pressure is again raised to the required value;

further, the high-pressure pump connected to the piston tank with the investigated solid material is switched to the operating mode of maintaining a constant pressure with the required setting, while the high-pressure pump connected to the piston tank with the test fluid is also switched to the operating mode with the same setting.

for several days, the change in the volume of water pumped out by the pump is recorded, and the change in the volume of the investigated solid material is measured.

The cell is loaded into the piston container with the test solid material in such a way that the lid of the swelling cell is in close contact with the lid of the piston container.

Both tanks are interconnected by a hydraulic line.

The installation can be thermally stabilized within twelve hours.

The piston container containing the test solid material can be evacuated for three hours.

The operability of the installation is ensured as follows. Initially, valves 1, 2, 3 are closed, valves 8, 9 are open. The swelling cell 6 is filled with a solid material which, due to the presence of the mesh 15 and the lid 16, cannot leave the cell when it swells. The presence of holes 17 promotes uniform wetting of the entire solid material by the fluid. The assembled cell is loaded into the piston container 5 in such a way that the lid of the swelling cell is in close contact with the lid of the piston container. The piston tank 5 is connected to the pump 10, after which the pressure rises to a value of 0.2-0.3 MPa in the sub-piston space 5 with the help of hydraulic fluid and pump 10.

The test fluid 7 is loaded into the piston container 4, after which it is connected to the pump 11 and the pressure in the sub-piston space 4 is raised to the test pressure. The oven 12 is switched on, thermally stabilized for 12 hours, valves 1 and 3 are opened, the vacuum pump is turned on, and vacuum is applied for 3 hours. After that, they close 1 and 3, wait until the temperature of the cabinet stabilizes, and start fluid 7 through valves 2 and 3 into piston tank 5, after which the fluid pressure is again raised to the experimental pressure using pump 11. From this moment, pump 10 is switched to the “on pressure”, while the setting is the equilibrium pressure established on the plunger of the pump 10 at a pressure on the plunger of the pump 11 equal to the formation pressure.

When the test material 14 expands, it pushes the freely moving cover 16. Since it is close to the cover of the piston tank 5, it cannot move, as a result of which the piston of the piston tank 5 moves and the pressure increases on the pump plunger 10. Since the pump operates in the mode “by pressure”, it will pump out hydraulic fluid from the sub-piston space, while the amount of hydraulic fluid pumped out from the sub-piston space 5 will be equal to the increase in the volume of the test substance. The constancy of temperature is maintained by a heating cabinet 13, the constancy of pressure is maintained by a pump 11 connected to the piston of the tank 4 with fluid 7.

The experiment is carried out for several days, determining the dependence of the amount of hydraulic fluid pumped out on the time since the beginning of the experiment. The degree of swelling is defined as:

WhereV _o - initial volume of material (ml),V _{n i} is the volume of hydraulic fluid pumped out by the pump since the beginning of the experiment.

Examples of specific assays are provided below. They do not exhaust all possibilities of the claimed plant and method, but illustrate its main applications.

Example 1

49.05 grams of bentonite are placed in the cell. Based on a density of 1.75 g/ ^cm3 , its true volume is 28.02 ml. The cell is placed in a 200 ml piston container, which is closed and connected to a high pressure pump and placed in a heating cabinet.

200 ml of sodium hydroxide solution of “chemically pure” qualification (hereinafter - NaOH) in distilled water with a concentration of 2 g/l is placed in the second piston container, it is also closed, placed in a heating cabinet and connected to the second high pressure pump. Both containers are interconnected by a hydraulic line with two closed valves.

The heating cabinet is heated to 40°C, the pressure in the tank with NaOH is increased to 15 MPa. The system is thermally stabilized for twelve hours. The piston container containing bentonite is evacuated for three hours, after which the valves between the containers are opened. The pressure in the system is raised to 15 MPa, after which the pump connected to the tank with bentonite switches to the operating mode "by pressure - return stroke" with a setting of 15 MPa, the pump connected to the tank with NaOH switches to the operating mode "by pressure - forward run" with the same setting.

Within four days, the change in the volume of water pumped out by the pump running in reverse is recorded.

The result is shown in Figure 3.

Example 2

25.04 grams of rubber crumb fraction 0-0.63 mm is placed in the cell. Based on a density of 1.1 g/cm ³ , its true volume is 22.8 ml. The cell is placed in a 200 ml piston container, which is closed and connected to a high pressure pump and placed in a heating cabinet.

300 g of brand 4.5 carbon dioxide (hereinafter referred to as CO ₂ ) with a pressure of 5 MPa is placed into the second piston container from a cylinder. The container is placed in a heating cabinet and connected to the second high pressure pump. Both containers are interconnected by a hydraulic line with two closed valves.

The heating cabinet is heated to 90°C, the pressure in the tank with CO ₂ pump is increased to 15 MPa. The system is thermally stabilized for 12 hours. The piston container containing rubber is evacuated for 3 hours, after which the valves between the containers are opened. The pressure in the system rises to 15 MPa, after which the pump connected to the tank with rubber switches to the operating mode “by pressure - reverse stroke” with a setting of 15 MPa, the pump connected to the tank with CO ₂ switches to the operating mode “by pressure - direct run" with the same setting.

Within three days, the change in the volume of water pumped out by the pump running in reverse is recorded.

The result is shown in Figure 4.

Example 3

58.01 grams of shale reservoir rock is placed in the cell. Based on a density of 2.65 g/cm ³ , its true volume is 21.9 ml. The cell is placed in a 200 ml piston container, which is closed and connected to a high pressure pump and placed in a heating cabinet.

A solution of NaOH in water at a concentration of 2 g/l is placed in the second piston container. The container is placed in a heating cabinet and connected to the second high pressure pump. Both containers are interconnected by a hydraulic line with two closed valves.

The heating cabinet is heated to 110°C, the pressure in the tank with NaOH pump is increased to 12 MPa. The system is thermally stabilized for 12 hours. The piston tank containing the rock is evacuated for 3 hours, after which the valves between the tanks are opened. The pressure in the system rises to 12 MPa, after which the pump connected to the reservoir with rock switches to the operating mode "by pressure - return" with a setting of 12 MPa, the pump connected to the reservoir with naOH switches to the operating mode "by pressure - forward run" with the same setting.

Within two weeks of days, the change in the volume of water pumped out by the pump running in reverse is recorded.

The result is shown in Figure 5.

Thus, due to the advantages of the above, including through the use of a cell consisting of a cylinder with holes on the side surface for uniform impregnation, a free-floating cover and a metal mesh, the use of high-pressure pumps with the function of operating in constant pressure mode using PID controller and thermal stabilization of the hydraulic fluid, both for compressing and supplying the fluid, and for measuring the change in volume, using a metal container with a piston displaced during the swelling of the test material and pushing the hydraulic fluid, and using a metal container with a piston for compressing and supplying the test material fluid, it is possible to measure the swelling of solid materials of organic and inorganic nature with high accuracy over time in various media with high accuracy in a wide range of thermobaric conditions. At the same time, the installation is technically simplified, has a low metal consumption, and provides ease of interpretation of the results obtained.

Claims (18)

1. Installation for measuring the change in the volume of solid materials of organic and inorganic nature over time, characterized in that it includes a heating cabinet, two piston tanks hydraulically connected to each other and with a vacuum pump, installed in a heating cabinet, each said container is also connected to its own pump high pressure, while one of the containers is made in the form of a container with the test fluid, and the second is made in the form of a container with the test solid material, and in the container with the test solid material there is a cell containing a bottom, a side cylindrical surface and a cover, and in the cell under a metal mesh is installed on the lid, and through holes are made on its side and bottom surfaces. 2. Installation according to claim 1, characterized in that the cover of the cell is made freely moving with through holes. 3. Installation according to claim 1, characterized in that the cell is installed in a piston container with a solid material under study in such a way that the cell lid is in close contact with the lid of this piston container. 4. The installation according to claim 1, characterized in that the high pressure pumps are designed to operate in a constant pressure mode using a PID controller and thermally stabilize the hydraulic fluid, both for compressing and supplying fluid, and for measuring volume change. 5. Installation according to claim 1, characterized in that the piston tanks are made of metal. 6. A method for measuring the change in the volume of solid materials of organic and inorganic nature over time using an installation containing a heating cabinet, two containers hydraulically connected to each other and with a vacuum pump with pistons for compressing and supplying fluid and for measuring the volume of swelling, installed in a heating cabinet, each of which is connected to its own high pressure pump, and a cylindrical cell with the investigated solid material, characterized by the fact that it includes the following steps: the test solid material is placed in the cell for measuring swelling; the cell with the test solid material is loaded into the first piston vessel for measuring swelling, which is closed, placed in a heating cabinet, connected to the first high-pressure pump, and the pressure in the under-piston space of the vessel with the test solid material is raised to a pressure higher than atmospheric by 0.1 MPa; then, the test fluid is placed in the second piston container; close the second piston tank with the test fluid, place it in a heating cabinet, connect it to the second high-pressure pump, and raise the pressure in the sub-piston space of the tank with the test fluid to the test pressure; include a heating cabinet, heating it to the required temperature, and a vacuum pump, after which they are thermally stabilized for several hours; the piston container containing the test solid material is evacuated for several hours, after which the fluid is launched into the piston container with the test solid material, and then the fluid pressure is again raised to the required value; further, the high-pressure pump connected to the piston tank with the investigated solid material is switched to the operating mode of maintaining a constant pressure with the required setting, while the high-pressure pump connected to the piston tank with the test fluid is also switched to the operating mode with the same setting. for several days, the change in the volume of water pumped out by the pump is recorded, and the change in the volume of the investigated solid material is measured. 7. The method according to claim 6, characterized in that the cell is loaded into a piston container with the test solid material in such a way that the lid of the swelling cell is in close contact with the lid of the piston container. 8. The method according to claim 6, characterized in that both containers are interconnected by a hydraulic line. 9. The method according to claim 6, characterized in that the thermal stabilization of the installation is carried out for twelve hours. 10. The method according to claim 6, characterized in that the piston container containing the test solid material is evacuated for three hours.

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