CN111208281B - Test device and method for liquid-plastic-solid three-state volume change during cement hydration - Google Patents

Abstract

The invention provides a testing device for liquid-plastic-solid three-state volume change during cement hydration, including a sealed slurry cup for holding cement slurry, and a shearing device for collecting shearing waves of the cement slurry is installed on the sealed slurry cup. Wave acquisition device, longitudinal wave acquisition device for collecting longitudinal waves of cement slurry, pressure control system for controlling the pressure in the sealed slurry cup, volume acquisition system for measuring the volume change of the cement slurry in the sealed slurry cup, for heating the cement slurry A heating measurement device; the shear wave acquisition device, the longitudinal wave acquisition device, the pressure control system, the volume acquisition system, and the heating measurement device are connected to a computer system. The invention can not only accurately measure the volume change of the cement slurry in the three stages of liquid state, plastic state and solid state, but also facilitate monitoring which stage the expansion agent mainly acts on the volume shrinkage of the cement slurry, which is important for the evaluation and optimization of the expansion agent. meaning.

Description

Test device and method for liquid-plastic-solid three-state volume change during cement hydration

technical field

The invention relates to the technical field of oil drilling and cementing engineering, in particular to a testing device and method for the volume change of liquid-plastic-solid three-state during cement hydration.

Background technique

During the cementing process, the cement slurry is filled in the annular space between the casing and the wellbore, and the cement sheath formed after condensation and solidification supports the well wall, protects the casing, and seals the oil and gas water layers. Usually, the cement slurry itself will produce volume shrinkage, which leads to the failure of the cementation quality of the cement ring in the later stage, causing problems such as interlayer channeling and annular pressure. By monitoring the time-varying process of the volume shrinkage of the cement slurry, it is of great significance to rationally develop the expansion cement slurry system and solve the problem of the volume shrinkage of the cement slurry. After years of research and development, great progress has been made in cement slurry volume shrinkage testing devices at home and abroad (for example: Wang Xiaojing. An oil well cement high temperature and high pressure volume expansion and shrinkage tester: CN102928578A, Li Ning. Cement slurry volume change test Instrument and test method: CN103245773A, Zhang Hua. Volume expansion and shrinkage rate test device: CN205138938U, etc.), although these devices can measure the volume shrinkage of cement slurry, they cannot distinguish the liquid state, plastic state, and solid state of three stages of cement slurry. Volume shrinkage, at present, there is no reliable test method for the plastic shrinkage and hardened body shrinkage of cement slurry, and it is impossible to accurately and effectively test the liquid-plastic-solid three-state volume change during the hydration process of cement slurry.

The best way to inhibit the volume shrinkage of cement slurry is to add oil well cement expansion agent. There are many kinds of expansion agents. For oil well cement, the best way to effect expansion material is when the cement slurry is in a plastic state, so that the volume of the cement slurry does not shrink. Micro-expansion occurs when the cement slurry is in the solid state, which not only reduces the volume shrinkage of the cement slurry, but also does not damage the internal structure of the cement stone due to excessive expansion in the later stage. Therefore, a volumetric expansion and contraction test device is required to monitor the volume change of the cement slurry during the entire process from liquid to solid state, and to accurately measure the volume change of the cement slurry in the three stages of liquid, plastic and solid, so as to monitor the expansion. The effect of the agent mainly acts on which stage of the cement slurry, and the expansion agent can be evaluated and optimized more precisely.

SUMMARY OF THE INVENTION

The purpose of the present invention is to solve the above-mentioned defects of the prior art, and to provide a test device and method that can not only monitor the change of cement slurry volume continuously but also distinguish the volume change of three stages of liquid, plastic and solid in the hydration process.

A testing device for liquid-plastic-solid three-state volume change during cement hydration, comprising a sealed slurry cup for holding cement slurry, a shear wave collection device for collecting shear waves of cement slurry is installed on the sealed slurry cup , Longitudinal wave acquisition device for collecting the longitudinal wave of cement slurry, pressure control system for controlling the pressure in the sealed slurry cup, volume acquisition system for measuring the volume change of the cement slurry in the sealed slurry cup, heating measurement device for heating the cement slurry ;

The shear wave acquisition device, the longitudinal wave acquisition device, the pressure control system, the volume acquisition system, and the heating measurement device are connected to the computer system.

Further, in the above-mentioned test device for liquid-plastic-solid three-state volume change during cement hydration, the shear wave acquisition device includes a shear wave transmitter, a shear wave receiver, and a sound wave acquisition system; the longitudinal wave The acquisition device includes a longitudinal wave transmitter, a longitudinal wave receiver, and an acoustic wave acquisition system;

One end of the shear wave transmitter and the longitudinal wave transmitter is respectively probed into the cement slurry, and the other end is respectively connected with the sound wave acquisition system; the longitudinal wave receiver and the shear wave receiver are respectively installed on the top of the sealed slurry cup. cover; the longitudinal wave transmitter and the shear wave transmitter are respectively installed on the bottom cover of the sealed paddle cup.

Further, in the test device of the liquid-plastic-solid three-state volume change in the above-mentioned cement hydration process, the surfaces of the shear wave transmitter, shear wave receiver, longitudinal wave transmitter and longitudinal wave receiver are respectively coated with a Layer of high temperature resistant lubricating oil.

Further, in the above-mentioned test device for the volume change of liquid-plastic-solid three-state in the cement hydration process, the pressure control system includes a pressurization and pressure relief port, a pressure sensor, and a pressure control system arranged on the sealed slurry cup. , the liquid medium placed on the upper surface of the cement slurry in the sealed slurry cup;

The pressurization and pressure relief ports are connected to the pressure control system through hydraulic lines, and the pressure control system can control the flow of liquid medium flowing into or out of the sealed cup through the hydraulic lines; the signal collection end of the pressure sensor is connected to the pressure control system connection, the signal output end of the pressure sensor is connected with the computer system;

The diameter of the cement slurry is d cm, the height is h ₁ cm, the upper end face is in direct contact with the liquid medium, and the direct contact between the liquid medium and the cement slurry will not affect the hydration reaction and later strength of the upper end face of the cement slurry, and the height of the liquid medium is h ₂ cm, The cement slurry expansion height h ₃ cm satisfies h ₁ >>h ₂ >h ₃ .

Further, in the above-mentioned test device for liquid-plastic-solid three-state volume change in the cement hydration process, the volume acquisition system includes: a precision flow sensor and a volume change acquisition system;

The collection end of the precision flow sensor is installed on the hydraulic pipeline for measuring the flow of the liquid medium passing through the hydraulic pipeline, and its signal output end is connected to the volume change collection system, which is connected to the computer system.

Further, in the above-mentioned test device for liquid-plastic-solid three-state volume change in the cement hydration process, the heating measurement device includes: a heater, an externally coupled temperature sensor for measuring the heating temperature of the heater, and a temperature sensor for measuring cement. Internal coupling temperature sensor and temperature control system for pulp temperature;

The inner coupled temperature sensor, the signal output end of the outer coupled temperature sensor, and the heater are respectively connected with the temperature control system, and the signal output end of the temperature control system is connected with the computer system.

A method for testing the volume change of liquid-plastic-solid three-state during cement hydration, comprising testing the volume change of liquid-plastic-solid three-state through a testing device for liquid-plastic-solid three-state volume change during cement hydration; the cement hydration process The test device for the volume change of liquid-plastic-solid three-state includes: top cover, liquid medium, sealed slurry cup, heater, cement slurry, pressurization and pressure relief port, bottom cover, internal coupling temperature sensor, external coupling temperature sensor, temperature Control system, pressure sensor, pressure control system, precision flow sensor, volume change acquisition system, longitudinal wave transmitter, longitudinal wave receiver, shear wave transmitter, shear wave receiver, acoustic wave acquisition system, computer system;

The measurement method specifically includes the following steps:

(1) Install the bottom cover on the lower end face of the slurry cup through the bottom thread of the slurry cup, and install the longitudinal wave transmitter, shear wave transmitter and internal coupling temperature sensor on the bottom cover through the sealing ring, and all three are in direct contact with the cement slurry. , In order to facilitate disassembly, a layer of high temperature resistant lubricating oil can be applied on its surface respectively;

(2) Prepare the cement slurry of the corresponding system according to the formula requirements, then inject it into the h ₁ cm scale inside the slurry cup, install the top cover on the upper end face of the slurry cup through the top thread of the slurry cup, and install the longitudinal wave receiver and shear wave receiver. It is installed on the top cover through the sealing ring, and both of them are in direct contact with the cement slurry.

(3) Connect the internal coupling temperature sensor and the external coupling temperature sensor to the temperature control system through the data cable, connect the heating pipeline at one end of the heater to the temperature control system, and connect the temperature sensor port on the temperature control system through the data cable. on a computer system;

(4) One end of the pressure sensor is connected to the pressure control system, and the other end is connected to the computer system; one end of the hydraulic pipeline is connected to the pressure control system, and the other end is connected to the booster and pressure relief ports through a nut buckle;

(5) One end of the precision flow sensor is connected to the hydraulic pipeline, the other end is connected to the volume change acquisition system, and the volume change acquisition port on the volume change acquisition system is connected to the computer system through a data line;

(6) Connect the longitudinal wave transmitter, longitudinal wave receiver, shear wave transmitter and shear wave receiver to the acoustic wave acquisition system through a data cable, and connect the acoustic wave acquisition port on the acoustic wave acquisition system to the computer system through a data cable ;

(7) Start the pressure control system, inject liquid medium into the slurry cup, loosen the nut buckle on the pressurization and pressure relief ports, and tighten the nut buckle when the liquid medium flows out of the thread, at this time, the upper part of the slurry cup is full. liquid medium;

(8) Turn on the power supply of the temperature control system, set the temperature, pressure and time for heating and boosting according to the actual working conditions, and start the program. At this time, the temperature control system and the pressure control system will automatically increase the temperature and pressure according to the process of the program, and wait until it reaches the set point. The temperature and pressure control system will automatically keep the temperature and pressure at the same temperature and pressure to ensure the stable temperature and pressure environment of the cement slurry;

(9) When starting the heating and boosting procedure, start the acoustic wave acquisition system at the same time to monitor the real-time changes of longitudinal waves and shear waves during the heating and boosting stage and the curing stage of the cement slurry;

(10) After the temperature rise and pressure increase process is over, turn on the precision flow sensor, start the volume change acquisition system, monitor the volume change of the liquid medium in the slurry cup in real time, convert it into the volume change value of the cement slurry through the volume change acquisition system, and then pass the volume The volume change collection port on the change collection system transmits the real-time collection value to the computer system;

(11) After the experiment is over, save the volume change curve of the cement slurry, close the programs of the temperature control system, pressure control system, volume change acquisition system, and sound wave acquisition system. After the instrument cools down, remove the pressure in the slurry cup and remove it. Internal coupling temperature sensor, longitudinal wave transmitter, longitudinal wave receiver, shear wave transmitter, shear wave receiver, remove the top cover and bottom cover, remove the cement stone in the slurry cup, clean the slurry cup, close each control system, The power supply of the acquisition system and the computer system is completed, and the experiment is over.

Beneficial effects:

(1) The liquid medium of the present invention is in direct contact with the cement slurry, regardless of whether the cement slurry is in a liquid state, a plastic state or a solid state, the volume change of the cement slurry can be detected in real time to ensure the accuracy and continuity of the instrument detection.

(2) The present invention utilizes the action mechanism of longitudinal waves and shear waves, which is convenient for us to distinguish the liquid state, plastic state and solid state of the cement slurry. The combined analysis of the acoustic wave acquisition system and the volume change acquisition system can not only accurately measure the liquid state and plastic state of the cement slurry. The volume change of the three stages of state and solid state, and it is also convenient to monitor which stage the expansion agent mainly acts on the volume shrinkage of the cement slurry, which is of great significance for the evaluation and optimization of the expansion agent.

Description of drawings

Fig. 1 is the structural representation of the test device of the liquid-plastic-solid three-state volume change in a kind of oil well cement hydration process of the present invention;

2 is a schematic diagram of the test result of the volume change of the cement slurry containing the expansion agent 1 provided in the first embodiment of the present invention;

Fig. 3 is the schematic diagram of the volume change test result of the cement slurry containing expansion agent 2 provided by the second embodiment of the present invention;

FIG. 4 is a schematic diagram of the test result of the volume change of the cement slurry containing the expansion agent 3 provided in the third embodiment of the present invention.

Detailed ways

In order to make the purpose, technical solutions and advantages of the present invention clearer, the technical solutions in the present invention are described clearly and completely below. Obviously, the described embodiments are part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.

The function of the invention is not limited to the evaluation of the expansion agent, but is more aimed at the volume change of the cement slurry, which can realize continuous monitoring and at the same time distinguish the changes of each stage, and also provide technical support for the evaluation and modification of the cement slurry.

The invention provides a testing device and method for liquid-plastic-solid three-state volume change in the process of oil well cement hydration. Pressure and pressure relief port 6, bottom cover 7, internal temperature sensor 8, external temperature sensor 9, temperature control system 10, pressure sensor 11, pressure control system 12, precision flow sensor 13, volume change acquisition system 14, longitudinal wave emission It is composed of a device 15, a longitudinal wave receiver 16, a shear wave transmitter 17, a shear wave receiver 18, an acoustic wave acquisition system 19, a computer system 20 and the like.

The top cover 1 is fixed on the upper end face of the slurry cup through the upper thread of the slurry cup, which is convenient for disassembly and installation.

The liquid medium 2 is injected and released into the paddle cup by the pressure control system 12 through the pressurization and pressure relief port 6 .

The outer diameter of the cup wall 3 is D cm, the wall thickness is T cm, and the height is H cm. A heater 4 and an externally coupled temperature sensor 9 are installed outside.

The diameter of the cement slurry 5 is d cm, the height is h ₁ cm, and the upper end face is in direct contact with the liquid medium 2. The direct contact of the liquid medium 2 with the cement slurry will not affect the hydration reaction and later strength of the upper end face of the cement slurry, and regardless of the cement slurry. In liquid, plastic or solid state, the volume change of cement slurry can be detected in real time to ensure the accuracy of instrument detection. _The height of liquid medium ₂ is h ₂ cm, and the expansion height of cement slurry is h ₃ cm. _h3 .

The bottom cover 7 is fixed on the lower end face of the slurry cup through the lower thread of the slurry cup, which is convenient for disassembly and installation.

One end of the in-coupling temperature sensor 8 is installed on the bottom cover 7 through a sealing ring, and the other end is connected to the temperature control system 10 through a data cable.

The temperature control system 10 has four main connection ports, which are respectively connected with a heater 4 , an internal temperature sensor 8 , an external temperature sensor 9 , and a computer system 20 .

One end of the pressure sensor 11 is connected to the hydraulic pipeline, and the other end is connected to the computer system 20 .

The pressure control system 12 has the function of precise pressure control, and can keep the pressure in the slurry cup stable in real time.

One end of the precision flow sensor 13 is connected to the hydraulic pipeline, and the other end is connected to the volume change acquisition system 14 .

The volume change acquisition system 14 has two main connection ports, which are respectively connected with a precision flow sensor 13 and a computer system 20. The volume change acquisition system can continuously monitor the volume change in the whole process of cement slurry hydration and solidification.

One end of the longitudinal wave transmitter 15 is installed on the bottom cover 7 through a sealing ring, and the other end is connected to the acoustic wave acquisition system 19 through a data cable.

One end of the longitudinal wave receiver 16 is installed on the top cover 1 through a sealing ring, and the other end is connected to the acoustic wave acquisition system 19 through a data line. When the cement slurry is in a liquid state, the longitudinal wave value is relatively stable. When the cement slurry enters the plastic state of hydration and gelation, the longitudinal wave value begins to change, so as to distinguish the liquid state and the plastic state of the cement slurry.

One end of the shear wave transmitter 17 is installed on the bottom cover 7 through a sealing ring, and the other end is connected to the acoustic wave acquisition system 19 through a data cable.

One end of the shear wave receiver 18 is installed on the top cover 1 through a sealing ring, and the other end is connected to the acoustic wave acquisition system 19 through a data line. The main function of the shear wave is: the shear wave has a strong effect on solid objects. When the cement slurry is in the liquid and plastic state in the early stage, the shear wave does not transmit a signal in the cement slurry, and can only propagate along the cup wall to present a stable signal value, so as to reduce the shear wave. The shear wave can only distinguish the plastic state and the solid state of the cement paste in the properties of solid propagation. The combined analysis of longitudinal wave and shear wave is used to distinguish the volume changes of three stages of liquid, plastic and solid during the hydration process of cement slurry.

The acoustic wave acquisition system 19 has five main connection ports, which are respectively connected with a longitudinal wave transmitter 15, a longitudinal wave receiver 16, a shear wave transmitter 17, a shear wave receiver 18, a computer system 20, and an integrated acoustic wave acquisition system (19). ) and the data collected by the volume change collecting system (14) to measure the volume change of the cement slurry in three stages: liquid state, plastic state and solid state.

The computer system 20 can record the change process and current value of curves such as temperature, pressure, volume change, and sound wave in real time.

Another aspect of the present invention also provides a test method based on the above-mentioned test device, comprising the following steps in turn:

1. Install the bottom cover 7 on the lower end face of the slurry cup through the screw at the bottom of the slurry cup, and install the longitudinal wave transmitter 15, the shear wave transmitter 17, and the internal coupling temperature sensor 8 on the bottom cover 7 through the sealing ring. The cement slurry is in direct contact. For the convenience of disassembly, a layer of high temperature resistant lubricating oil can be applied to the surface.

2. Prepare the cement slurry of the corresponding system according to the formula requirements, then inject it into the h1 cm scale inside the slurry cup, install the top cover 1 on the upper end face of the slurry cup through the top thread of the slurry cup, and install the longitudinal wave receiver 16 and the shear wave receiver. 18 is installed on the top cover 1 through the sealing ring, both of which are in direct contact with the cement slurry.

3. Connect the in-coupling temperature sensor 8 and the external-coupling temperature sensor 9 to the temperature control system 10 through the data line, connect the heating pipeline at one end of the heater 4 to the temperature control system 10, and connect the temperature sensor on the temperature control system 10 The ports are connected to the computer system 20 through data lines.

4. One end of the pressure sensor 11 is connected to the hydraulic line, the other end is connected to the computer system 20, one end of the hydraulic line is connected to the pressure control system 12, and the other end is connected to the boost and pressure relief port 6 through a nut.

5. One end of the precision flow sensor 13 is connected to the hydraulic pipeline, the other end is connected to the volume change acquisition system 14, and the volume change acquisition port on the volume change acquisition system 14 is connected to the computer system 20 through a data line.

6. Connect the longitudinal wave transmitter 15, the longitudinal wave receiver 16, the shear wave transmitter 17, and the shear wave receiver 18 to the acoustic wave acquisition system 19 through the data cable, and connect the acoustic wave acquisition port on the acoustic wave acquisition system 19 through the data cable. connected to the computer system 20 .

7. Start the pressure control system 12, inject the liquid medium 2 into the slurry cup, loosen the nut buckle on the pressurization and pressure relief port 6, and tighten the nut buckle when the liquid medium flows out of the screw buckle. At this time, the slurry cup The upper part is filled with liquid medium 2.

8. Turn on the power supply of the temperature control system 10, set the temperature, pressure, and heating and boosting time according to the actual working conditions, and start the program. At this time, the temperature control system 10 and the pressure control system 12 will automatically increase the temperature and pressure according to the program process, and wait until the temperature rises to When the temperature and pressure are set, the temperature and pressure control system will automatically keep the temperature and pressure to keep the temperature and pressure of the cement slurry stable.

9. When starting the heating and boosting procedure, start the acoustic wave acquisition system 19 at the same time to monitor the real-time changes of longitudinal waves and shear waves during the heating and boosting stage and the curing stage of the cement slurry.

10. After the temperature rise and pressure rise process is over, turn on the precision flow sensor 13, start the volume change acquisition system 14, monitor the volume change of the liquid medium 2 in the slurry cup in real time, and convert it into the volume change value of the cement slurry through the volume change acquisition system 14, The real-time acquisition values are then transmitted to the computer system 20 through the volume change acquisition port on the volume change acquisition system 14 .

11. After the experiment is over, save the volume change curve of the cement slurry, close the programs of the temperature control system 10, the pressure control system 12, the volume change acquisition system 14, and the sound wave acquisition system 19. After the instrument has cooled down, remove the Pressure, remove the in-coupling temperature sensor 8, longitudinal wave transmitter 15, longitudinal wave receiver 16, shear wave transmitter 17, shear wave receiver 18, remove the top cover 1 and bottom cover 7, remove the cement stone in the cup , Clean the slurry cup, turn off the power of each control system, acquisition system, and computer system, and the experiment is over.

Example 1

The implementation process of the volume change test of cement slurry containing expansion agent 1 is as follows:

1. Install the bottom cover 7 on the lower end face of the slurry cup through the screw at the bottom of the slurry cup, and install the longitudinal wave transmitter 15, the shear wave transmitter 17, and the internal coupling temperature sensor 8 on the bottom cover 7 through the sealing ring. The cement slurry is in direct contact. For the convenience of disassembly, a layer of high temperature resistant lubricating oil can be applied to the surface.

2. Prepare a cement slurry system containing expansion agent 1 according to the formula requirements, then inject it into the h1 cm scale inside the slurry cup, install the top cover 1 on the upper end face of the slurry cup through the thread on the top of the slurry cup, install the longitudinal wave receiver 16, shear The wave receiver 18 is installed on the top cover 1 through a sealing ring, both of which are in direct contact with the cement slurry. For the convenience of disassembly, a layer of high temperature resistant lubricating oil can be respectively applied to the surface thereof.

3. Connect the in-coupling temperature sensor 8 and the external-coupling temperature sensor 9 to the temperature control system 10 through the data line, connect the heating pipeline at one end of the heater 4 to the temperature control system 10, and connect the temperature sensor on the temperature control system 10 The ports are connected to the computer system 20 through data lines.

4. One end of the pressure sensor 11 is connected to the hydraulic line, the other end is connected to the computer system 20, one end of the hydraulic line is connected to the pressure control system 12, and the other end is connected to the boost and pressure relief port 6 through a nut.

5. One end of the precision flow sensor 13 is connected to the hydraulic pipeline, the other end is connected to the volume change acquisition system 14, and the volume change acquisition port on the volume change acquisition system 14 is connected to the computer system 20 through a data line.

6. Connect the longitudinal wave transmitter 15, the longitudinal wave receiver 16, the shear wave transmitter 17, and the shear wave receiver 18 to the acoustic wave acquisition system 19 through the data cable, and connect the acoustic wave acquisition port on the acoustic wave acquisition system 19 through the data cable. connected to the computer system 20 .

7. Start the pressure control system 12, inject the liquid medium 2 into the slurry cup, loosen the nut buckle on the pressurization and pressure relief port 6, and tighten the nut buckle when the liquid medium flows out of the screw buckle. At this time, the slurry cup The upper part is filled with liquid medium 2.

8. Turn on the power supply of the temperature control system 10, set the temperature, pressure, and heating and boosting time according to the actual working conditions, and start the program. At this time, the temperature control system 10 and the pressure control system 12 will automatically increase the temperature and pressure according to the program process, and wait until the temperature rises to When the temperature and pressure are set, the temperature and pressure control system will automatically keep the temperature and pressure to keep the temperature and pressure of the cement slurry stable.

9. When starting the heating and boosting procedure, start the acoustic wave acquisition system 19 at the same time to ensure the real-time changes of longitudinal waves and shear waves during the heating and boosting stage and the curing stage of the cement slurry.

10. After the temperature rise and pressure rise process is over, turn on the precision flow sensor 13, start the volume change acquisition system 14, monitor the volume change of the liquid medium 2 in the slurry cup in real time, and convert it into the volume change value of the cement slurry through the volume change acquisition system 14, The real-time acquisition values are then transmitted to the computer system 20 through the volume change acquisition port on the volume change acquisition system 14 .

11. After the experiment is over, save the volume change curve of the cement slurry, close the programs of the temperature control system 10, the pressure control system 12, the volume change acquisition system 14, and the sound wave acquisition system 19. After the instrument has cooled down, remove the Pressure, remove the in-coupling temperature sensor 8, longitudinal wave transmitter 15, longitudinal wave receiver 16, shear wave transmitter 17, shear wave receiver 18, remove the top cover 1 and bottom cover 7, remove the cement stone in the cup , Clean the slurry cup, turn off the power of each control system, acquisition system, and computer system, and the experiment is over.

Embodiment 2

The implementation process of the volume change test of cement slurry containing expansion agent 2 is as follows:

1. Install the bottom cover 7 on the lower end face of the slurry cup through the screw at the bottom of the slurry cup, and install the longitudinal wave transmitter 15, the shear wave transmitter 17, and the internal coupling temperature sensor 8 on the bottom cover 7 through the sealing ring. The cement slurry is in direct contact. For the convenience of disassembly, a layer of high temperature resistant lubricating oil can be applied to the surface.

2. Prepare the cement slurry system containing expansion agent 2 according to the formula requirements, then inject it into the h1 cm scale inside the slurry cup, install the top cover 1 on the upper end face of the slurry cup through the thread on the top of the slurry cup, install the longitudinal wave receiver 16, shear The wave receiver 18 is installed on the top cover 1 through a sealing ring, both of which are in direct contact with the cement slurry. For the convenience of disassembly, a layer of high temperature resistant lubricating oil can be respectively applied to the surface thereof.

3. Connect the in-coupling temperature sensor 8 and the external-coupling temperature sensor 9 to the temperature control system 10 through the data line, connect the heating pipeline at one end of the heater 4 to the temperature control system 10, and connect the temperature sensor on the temperature control system 10 The ports are connected to the computer system 20 through data lines.

4. One end of the pressure sensor 11 is connected to the hydraulic line, the other end is connected to the computer system 20, one end of the hydraulic line is connected to the pressure control system 12, and the other end is connected to the boost and pressure relief port 6 through a nut.

5. One end of the precision flow sensor 13 is connected to the hydraulic pipeline, the other end is connected to the volume change acquisition system 14, and the volume change acquisition port on the volume change acquisition system 14 is connected to the computer system 20 through a data line.

6. Connect the longitudinal wave transmitter 15, the longitudinal wave receiver 16, the shear wave transmitter 17, and the shear wave receiver 18 to the acoustic wave acquisition system 19 through the data cable, and connect the acoustic wave acquisition port on the acoustic wave acquisition system 19 through the data cable. connected to the computer system 20 .

7. Start the pressure control system 12, inject the liquid medium 2 into the slurry cup, loosen the nut buckle on the pressurization and pressure relief port 6, and tighten the nut buckle when the liquid medium flows out of the screw buckle. At this time, the slurry cup The upper part is filled with liquid medium 2.

8. Turn on the power supply of the temperature control system 10, set the temperature, pressure, and heating and boosting time according to the actual working conditions, and start the program. At this time, the temperature control system 10 and the pressure control system 12 will automatically increase the temperature and pressure according to the program process, and wait until the temperature rises to When the temperature and pressure are set, the temperature and pressure control system will automatically keep the temperature and pressure to keep the temperature and pressure of the cement slurry stable.

9. When starting the heating and boosting procedure, start the acoustic wave acquisition system 19 at the same time to ensure the real-time changes of longitudinal waves and shear waves during the heating and boosting stage and the curing stage of the cement slurry.

10. After the temperature rise and pressure rise process is over, turn on the precision flow sensor 13, start the volume change acquisition system 14, monitor the volume change of the liquid medium 2 in the slurry cup in real time, and convert it into the volume change value of the cement slurry through the volume change acquisition system 14, The real-time acquisition values are then transmitted to the computer system 20 through the volume change acquisition port on the volume change acquisition system 14 .

11. After the experiment is over, save the volume change curve of the cement slurry, close the programs of the temperature control system 10, the pressure control system 12, the volume change acquisition system 14, and the sound wave acquisition system 19. After the instrument has cooled down, remove the Pressure, remove the in-coupling temperature sensor 8, longitudinal wave transmitter 15, longitudinal wave receiver 16, shear wave transmitter 17, shear wave receiver 18, remove the top cover 1 and bottom cover 7, remove the cement stone in the cup , Clean the slurry cup, turn off the power of each control system, acquisition system, and computer system, and the experiment is over.

Embodiment 3

The implementation process of the volume change test of cement slurry containing expansion agent 3 is as follows:

1. Install the bottom cover 7 on the lower end face of the slurry cup through the screw at the bottom of the slurry cup, and install the longitudinal wave transmitter 15, the shear wave transmitter 17, and the internal coupling temperature sensor 8 on the bottom cover 7 through the sealing ring. The cement slurry is in direct contact. For the convenience of disassembly, a layer of high temperature resistant lubricating oil can be applied to the surface.

2. Prepare the cement slurry system containing expansion agent 3 according to the formula requirements, then inject it into the h1 cm scale inside the slurry cup, install the top cover 1 on the upper end face of the slurry cup through the thread on the top of the slurry cup, and install the longitudinal wave receiver 16, shear The wave receiver 18 is installed on the top cover 1 through a sealing ring, both of which are in direct contact with the cement slurry. For the convenience of disassembly, a layer of high temperature resistant lubricating oil can be respectively applied to the surface thereof.

3. Connect the in-coupling temperature sensor 8 and the external-coupling temperature sensor 9 to the temperature control system 10 through the data line, connect the heating pipeline at one end of the heater 4 to the temperature control system 10, and connect the temperature sensor on the temperature control system 10 The ports are connected to the computer system 20 through data lines.

4. One end of the pressure sensor 11 is connected to the hydraulic line, the other end is connected to the computer system 20, one end of the hydraulic line is connected to the pressure control system 12, and the other end is connected to the boost and pressure relief port 6 through a nut.

5. One end of the precision flow sensor 13 is connected to the hydraulic pipeline, the other end is connected to the volume change acquisition system 14, and the volume change acquisition port on the volume change acquisition system 14 is connected to the computer system 20 through a data line.

6. Connect the longitudinal wave transmitter 15, the longitudinal wave receiver 16, the shear wave transmitter 17, and the shear wave receiver 18 to the acoustic wave acquisition system 19 through the data cable, and connect the acoustic wave acquisition port on the acoustic wave acquisition system 19 through the data cable. connected to the computer system 20 .

7. Start the pressure control system 12, inject the liquid medium 2 into the slurry cup, loosen the nut buckle on the pressurization and pressure relief port 6, and tighten the nut buckle when the liquid medium flows out of the screw buckle. At this time, the slurry cup The upper part is filled with liquid medium 2.

8. Turn on the power supply of the temperature control system 10, set the temperature, pressure, and heating and boosting time according to the actual working conditions, and start the program. At this time, the temperature control system 10 and the pressure control system 12 will automatically increase the temperature and pressure according to the program process, and wait until the temperature rises to When the temperature and pressure are set, the temperature and pressure control system will automatically keep the temperature and pressure to keep the temperature and pressure of the cement slurry stable.

9. When starting the heating and boosting procedure, start the acoustic wave acquisition system 19 at the same time to ensure the real-time changes of longitudinal waves and shear waves during the heating and boosting stage and the curing stage of the cement slurry.

10. After the temperature rise and pressure rise process is over, turn on the precision flow sensor 13, start the volume change acquisition system 14, monitor the volume change of the liquid medium 2 in the slurry cup in real time, and convert it into the volume change value of the cement slurry through the volume change acquisition system 14, The real-time acquisition values are then transmitted to the computer system 20 through the volume change acquisition port on the volume change acquisition system 14 .

11. After the experiment is over, save the volume change curve of the cement slurry, close the programs of the temperature control system 10, the pressure control system 12, the volume change acquisition system 14, and the sound wave acquisition system 19. After the instrument has cooled down, remove the Pressure, remove the in-coupling temperature sensor 8, longitudinal wave transmitter 15, longitudinal wave receiver 16, shear wave transmitter 17, shear wave receiver 18, remove the top cover 1 and bottom cover 7, remove the cement stone in the cup , Clean the slurry cup, turn off the power of each control system, acquisition system, computer system, and the experiment is over.

Table 1 List of experimental results

serial number temperature/℃ pressure/MPa Volume change rate/% The main action stage of the expansion agent Example 1 120 20.7 -3.60 liquid Embodiment 2 120 20.7 -1.20 plastic state Embodiment 3 120 20.7 -1.22 solid state/hardening stage

Remark:

Example 1 Formula: 400g Grade G cement + 90% weighting agent + 35% silica fume + 6% microsilica + 3% expansion agent 1 + 2% stabilizer + 3% dispersant + 1.5% defoamer + 6% reducer Water loss agent + 6% retarder + 70% water;

Example 2 Formula: 400g Grade G cement + 90% weighting agent + 35% silica fume + 6% microsilica + 3% expansion agent 2 + 2% stabilizer + 3% dispersant + 1.5% defoamer + 6% reducer Water loss agent + 6% retarder + 70% water;

Example 3 Formula: 400g Grade G cement + 90% weighting agent + 35% silica fume + 6% microsilica + 3% expansion agent 3 + 2% stabilizer + 3% dispersant + 1.5% defoamer + 6% reducer Water loss agent + 6% retarder + 70% water

Analysis of results:

Embodiment 1: It can be seen from the test chart of the experimental results (Fig. 2) that the volume shrinkage of the cement slurry of the expansion agent 1 has not been well improved, because the hydration reaction of the expansion material is too fast, and the slurry is in a liquid state. The expansion effect is mostly absorbed by the slurry, so the effect of the expansion agent 1 cannot be reflected, so this type of expansion agent is not suitable for the cement slurry of this system.

Embodiment 2: It can be seen from the test chart of the experimental results (Fig. 3) that the volume shrinkage of the cement slurry added with the expansion agent 2 has been improved. It can be seen from the longitudinal wave curve that when the cement slurry begins to enter the plastic state, the expansion material The hydration reaction began to occur, the volume of the cement slurry began to expand, the volume change rate curve began to rise, and then the reaction was rapid, and the volume change rate curve rose rapidly; it can be seen from the shear wave curve that when the cement slurry entered the solid state from the plastic state, The hydration reaction of the swelling material reaches the maximum, the volume expansion of the cement slurry also reaches the maximum, and the volume change rate curve rises to the maximum value. After that, the reaction of the swelling material gradually slows down, and the curve begins to decrease slowly, and then gradually becomes stable. This kind of expansion agent has a good expansion effect in the plastic stage of the cement slurry, and does not affect the development of the internal structural strength of the cement stone in the later stage. Therefore, the expansion agent 2 can meet the use of the cement slurry of this system.

Embodiment 3: It can be seen from the experimental result test diagram (Fig. 4) that although the volume shrinkage of the cement slurry of the expansion agent 3 has been well improved, the hydration reaction of the expansion material is too slow, as can be seen from the shear wave curve. , the reaction begins when the slurry forms the gel strength, which will have a certain destructive effect on the slurry structure. Although it has a good effect on the later shrinkage of the cement slurry, it has a negative effect on the integrity of the cement sheath. Seriously More cracks will also be formed during the time, which will affect the sealing ability of the cement sheath in the later stage, so the expansion agent 3 is not suitable for the cement slurry of this system.

Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, but not to limit them; although the present invention has been described in detail with reference to the foregoing embodiments, those of ordinary skill in the art should understand that it can still be Modifications are made to the technical solutions described in the foregoing embodiments, or some technical features thereof are equivalently replaced; and these modifications or replacements do not make the essence of the corresponding technical solutions depart from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims (6)

1. A test device for liquid-plastic-solid three-state volume change in a cement hydration process, characterized in that it comprises a sealed slurry cup (3) for containing cement slurry (5), on the sealed slurry cup (3) A shear wave collection device for collecting shear waves of cement slurry (5), a longitudinal wave collection device for collecting longitudinal waves of cement slurry (5), a pressure control system for controlling the pressure in the sealed slurry cup (3), and a A volume acquisition system for measuring the volume change of the cement slurry (5) in the sealed slurry cup (3), and a heating measuring device for heating the cement slurry (5); The shear wave acquisition device, the longitudinal wave acquisition device, the pressure control system, the volume acquisition system, and the heating measurement device are connected to the computer system; The shear wave acquisition device includes a shear wave transmitter (17), a shear wave receiver (18), and an acoustic wave acquisition system (19); the longitudinal wave acquisition device includes a longitudinal wave transmitter (15), a longitudinal wave receiver ( 16), a sound wave acquisition system (19); One ends of the shear wave transmitter (17) and the longitudinal wave transmitter (15) are respectively probed into the cement slurry, and the other ends are respectively connected to the sound wave acquisition system (19); The longitudinal wave receiver (16) and the shear wave receiver (18) are respectively installed on the top cover (1) of the sealed cup (3); the longitudinal wave transmitter (15) and the shear wave transmitter (17) are respectively Installed on the bottom cover (7) of the sealed paddle cup (3). 2. The test device for liquid-plastic-solid three-state volume change during cement hydration according to claim 1, wherein the shear wave transmitter (17), the shear wave receiver (18), the longitudinal wave The surfaces of the transmitter (15) and the longitudinal wave receiver (16) are respectively coated with a layer of high temperature resistant lubricating oil. 3. The testing device for liquid-plastic-solid three-state volume change during cement hydration according to claim 1, wherein the pressure control system comprises a pressurizing and venting device arranged on the sealed slurry cup (3). pressure port (6), pressure sensor (11), pressure control system (12), liquid medium (2) placed on the upper surface of the cement slurry in the sealed slurry cup (3); The pressurization and pressure relief port (6) is connected to a pressure control system (12) through a hydraulic pipeline, and the pressure control system (12) can control the flow into or out of the liquid medium (2) in the sealed cup (3) through the hydraulic pipeline The signal acquisition end of the pressure sensor (11) is connected to the pressure control system (12), and the signal output end of the pressure sensor (11) is connected to the computer system; The diameter of the cement slurry (5) is d cm, the height is h ₁ cm, and the upper end face is in direct contact with the liquid medium (2). Strength, liquid medium (2) height h ₂ cm, cement slurry expansion height h ₃ cm, satisfying h ₁

h ₂

_h3 . 4. The testing device for liquid-plastic-solid three-state volume change during cement hydration process according to claim 1, wherein the volume acquisition system comprises: a precision flow sensor (13) and a volume change acquisition system (14); The collection end of the precision flow sensor (13) is installed on the hydraulic pipeline for measuring the flow rate of the liquid medium passing through the hydraulic pipeline, and the signal output end thereof is connected to the volume change acquisition system (14), and the volume change acquisition system (14) Connect with computer system. 5. The testing device for liquid-plastic-solid three-state volume change during cement hydration according to claim 1, wherein the heating measurement device comprises: a heater (4), a heater (4) for measuring an externally coupled temperature sensor (9) for heating temperature, an internal coupled temperature sensor (8) for measuring the temperature of the cement slurry (5), and a temperature control system (10); The signal output terminals of the in-coupled temperature sensor (8) and the external-coupled temperature sensor (9) and the heater (4) are respectively connected to the temperature control system (10), and the signal output terminal of the temperature control system (10) is connected to the computer system connect. 6. a method for testing liquid-plastic-solid three-state volume change in a cement hydration process, characterized in that the volume change of liquid-plastic-solid three-state is tested by a testing device for liquid-plastic-solid three-state volume change in the cement hydration process; The testing device for liquid-plastic-solid three-state volume change during cement hydration includes: a top cover (1), a liquid medium (2), a sealed slurry cup (3), a heater (4), a cement slurry (5), a Pressure and pressure relief port (6), bottom cover (7), internal coupling temperature sensor (8), external coupling temperature sensor (9), temperature control system (10), pressure sensor (11), pressure control system (12) , precision flow sensor (13), volume change acquisition system (14), longitudinal wave transmitter (15), longitudinal wave receiver (16), shear wave transmitter (17), shear wave receiver (18), acoustic wave acquisition system (19), computer system (20); The test method specifically includes the following steps: Step 1: Install the bottom cover (7) on the lower end face of the slurry cup through the screw at the bottom of the slurry cup, and install the longitudinal wave transmitter (15), shear wave transmitter (17), and internal coupling temperature sensor (8) on the On the bottom cover (7), the three parts are in direct contact with the cement slurry. For the convenience of disassembly, a layer of high temperature resistant lubricating oil is respectively applied to the surface; Step 2: Prepare the cement slurry of the corresponding system according to the formula requirements, then inject it into the h ₁ cm scale inside the slurry cup, install the top cover (1) on the upper end face of the slurry cup through the thread on the top of the slurry cup, and install the longitudinal wave receiver (16) . The shear wave receiver (18) is installed on the top cover (1) through the sealing ring, both of which are in direct contact with the cement slurry. For the convenience of disassembly, a layer of high temperature resistant lubricating oil is respectively applied to its surface; Step 3: Connect the internal coupling temperature sensor (8) and the external coupling temperature sensor (9) to the temperature control system (10) through the data cable, and connect the heating pipeline at one end of the heater (4) to the temperature control system (10) on, connecting the temperature sensor port on the temperature control system (10) to the computer system (20) through a data cable; Step 4: Connect one end of the pressure sensor (11) to the pressure control system (12), and the other end to the computer system (20); one end of the hydraulic pipeline is connected to the pressure control system (12), and the other end is connected through a nut buckle On the boost and pressure relief ports (6); Step 5: Connect one end of the precision flow sensor (13) to the hydraulic pipeline, and the other end to the volume change acquisition system (14), and connect the volume change acquisition port on the volume change acquisition system (14) to the computer through a data cable on system (20); Step 6: Connect the longitudinal wave transmitter (15), the longitudinal wave receiver (16), the shear wave transmitter (17), and the shear wave receiver (18) to the acoustic wave acquisition system (19) through a data cable, and connect the acoustic wave The acoustic wave acquisition port on the acquisition system (19) is connected to the computer system (20) through a data line; Step 7: Start the pressure control system (12), inject the liquid medium (2) into the slurry cup, loosen the nut on the pressurization and pressure relief port (6), and tighten it when the liquid medium flows out of the thread The nut is buckled, and the upper part of the slurry cup is filled with liquid medium (2); Step 8: Turn on the power supply of the temperature control system (10), set the temperature, pressure and temperature rise and boost time according to the actual working conditions, and start the program. At this time, the temperature control system (10) and the pressure control system (12) will automatically follow the program progress. When the temperature and pressure rise to the set temperature and pressure value, the temperature and pressure control system will automatically keep the temperature and pressure to keep the temperature and pressure of the cement slurry stable; Step 9: When starting the heating and boosting procedure, simultaneously start the acoustic wave acquisition system (19) to monitor the real-time changes of longitudinal waves and shear waves during the heating and boosting stage and the curing stage of the cement slurry; Step 10: After the temperature rise and pressure rise process is over, turn on the precision flow sensor (13), start the volume change acquisition system (14), monitor the volume change of the liquid medium (2) in the slurry cup in real time, and use the volume change acquisition system (14) Converted into the volume change value of the cement slurry, and then transmit the real-time collection value to the computer system (20) through the volume change collection port on the volume change collection system (14); Combine the detection data of longitudinal waves and shear waves to measure the cement slurry The volume change in three stages of liquid, plastic and solid; Step 11: After the experiment is over, save the volume change curve of the cement slurry, close the programs of the temperature control system (10), the pressure control system (12), the volume change acquisition system (14), and the sound wave acquisition system (19), and wait until After the instrument is cooled down, remove the pressure in the cup, remove the in-coupling temperature sensor (8), longitudinal wave transmitter (15), longitudinal wave receiver (16), shear wave transmitter (17), shear wave receiver ( 18), remove the top cover (1) and bottom cover (7), remove the cement stone in the slurry cup, clean the slurry cup, turn off the power of each control system, acquisition system, and computer system, and the experiment is over.

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