Experimental device for rapid determination of acid rock reaction

Abstract

The invention relates to the technical field of petroleum geology testing, in particular to an acid rock reaction rapid determination experiment device which comprises an acid storage tank, a preheating kettle, a gas pressurization unit, a reaction kettle, an intelligent control collection unit and an analysis unit. The acid storage tank sends acid liquor to the preheating kettle to preheat the acid liquor; the gas pressurization system pressurizes target pressure into the reaction kettle; a sampling sensing module in the intelligent control collection unit detects the amount of reaction liquid in a rotary sampler and the condensation time of a condenser, and a sampling control module determines a plurality of pressure lag time periods according to pressure data and the amount of the reaction liquid in a reaction kettle collected at a plurality of time points; therefore, the reaction stopping time of the reaction liquid of the control group, the condensation rate of the condenser and the pressurization rate of the gas pressurization unit are determined, and the acid rock reaction kinetic parameters are determined. The pressure is effectively and rapidly increased, constant-pressure liquid supplementing is achieved, operation is convenient, the automatic sampling efficiency is improved, and meanwhile the accuracy of test data is improved.

Description

Technical Field

[0001] The invention relates to the technical field of petroleum geological testing, in particular to an acid-rock reaction rapid determination experimental device. Background Art

[0002] Acid-rock reaction refers to the chemical reaction between acid and rock. The process of acid-rock reaction can be roughly described as: hydrogen ions (H+) in the acid diffuse to the rock surface; H+ is adsorbed on the rock surface and reacts chemically with the mineral components in the rock; the products generated by the reaction detach from the rock surface and leave the reaction area through mass transfer.

[0003] Chinese patent publication number: CN118294582A, discloses an acid-rock reaction kinetics experimental device and method, the experimental device includes: a reactor, an acid storage tank, a timed sampling system, a manual pump device and a gas cylinder. The method includes: during the acid-rock reaction, the volume and pressure of the acid liquid in the reactor gradually decrease. At this time, the manual pump device is used to increase the pressure and replenish the acid liquid in the reactor without stopping the experiment to ensure the continuity of the reaction.

[0004] It can be seen that the above technical solution has the following problems: when the pressure is increased in the reactor by a manual pump device, the pressurization speed is slow, but the acid-rock reaction speed is fast, resulting in inaccurate data tracking. Therefore, it is necessary to study an acid-rock reaction rapid determination experimental device that can quickly increase the pressure and achieve constant pressure fluid replenishment, improve the accuracy of the test data, and provide parameters and basis for acidization optimization design and acid system optimization. Summary of the invention

[0005] To this end, the present invention provides an acid-rock reaction rapid determination experimental device to overcome the problem that the acid-rock experimental device in the prior art has slow pressurization and fails to timely match the high speed of the acid-rock reaction, resulting in a lag in data tracking.

[0006] To achieve the above object, the present invention provides an acid-rock reaction rapid determination experimental device, comprising:

[0007] Acid storage tank, preheating kettle, gas pressurization unit, reactor, intelligent control collection unit and analysis unit;

[0008] The acid storage tank is connected to the preheating kettle, the acid storage tank is used to store acid solution and transport the acid solution to the preheating kettle, and the preheating kettle is used to preheat the acid solution;

[0009] The gas pressurizing unit is connected to the reactor to pressurize the reactor to a target pressure;

[0010] The intelligent control collection unit includes a condenser, a rotary sampler connected to the condenser for collecting reaction liquid, a sampling sensor module, and a sampling control module for judging whether the sampling is completed. The condenser is connected to the liquid outlet of the reactor. The reaction liquid in the reactor enters the rotary sampler after being condensed by the condenser. The sampling sensor module is used to detect the amount of reaction liquid in the rotary sampler and the condensation time of the condenser. The sampling control module is used to determine a number of pressure hysteresis time periods according to the pressure data in the reactor collected at a number of time points and the amount of reaction liquid, and determine the reaction stop timing of the control group reaction liquid and the condensation rate of the condenser based on the pressure hysteresis time period;

[0011] The analysis unit is connected to the intelligent control collection unit, and is used to adjust and determine the pressurization rate of the gas pressurization unit based on the duration of the pressure lag time period, and to determine the acid-rock reaction kinetic parameters based on the pressure lag time period, the test data of the reaction liquid samples of the control group reaction liquid, and the test data of the reaction liquid samples of the measurement group reaction liquid.

[0012] Furthermore, the control group is the reactor that performs acid-rock reaction under preset boosting conditions; and the measurement group is the reactor that performs acid-rock reaction under pressure-maintaining conditions.

[0013] Furthermore, the rotary sampler is provided with a plurality of cleaning ports, and the plurality of cleaning ports are used to realize automatic cleaning of a plurality of test tubes on the rotary sampler.

[0014] Further, the sampling control module determines a number of pressure hysteresis time periods, including:

[0015] Collecting pressure data and reaction liquid volume data in the control group reactor at the plurality of time points, and forming a first pressure curve and a first reaction liquid yield curve;

[0016] Collecting the pressure data and the reaction liquid volume data in the reaction kettle of the measurement group at the several time points, and forming a second pressure curve and a second reaction liquid yield curve;

[0017] determining a plurality of pressure mutation time points based on the first pressure curve and the second pressure curve;

[0018] Determining a plurality of response time points based on the first reaction liquid yield curve and the second reaction liquid yield curve;

[0019] The plurality of pressure hysteresis time periods are determined based on the pressure mutation time point and the plurality of response time points.

[0020] Furthermore, the sampling control module determines a number of pressure mutation time points, including:

[0021] Normalizing the first pressure curve and the second pressure curve;

[0022] At the same time point, determining the normalized pressure difference between the first pressure curve and the second pressure curve;

[0023] The pressure difference is compared with a preset pressure difference, and a pressure mutation time point is determined according to the comparison result.

[0024] Furthermore, the sampling control module determines a number of response time points, including:

[0025] At the same time point, determining the difference in reaction liquid yield between the first reaction liquid yield curve and the second reaction liquid yield curve;

[0026] The reaction solution yield difference is compared with a preset reaction solution yield difference, and a response time point is determined according to the comparison result.

[0027] Further, the sampling control module determines the plurality of pressure hysteresis time periods based on the plurality of pressure mutation time points and the plurality of response time points, including:

[0028] Matching the plurality of pressure mutation time points with the plurality of response time points;

[0029] The time difference between the pressure mutation time point and the response time point after matching is determined based on the matching results.

[0030] Furthermore, the sampling control module determines the reaction stopping time of the control group reaction solution based on the pressure hysteresis period, including:

[0031] Collecting the reaction solution of the control group at the cutoff time point of the pressure hysteresis period;

[0032] Stop collecting the reaction solution of the control group at the initial time point of the pressure hysteresis period.

[0033] Further, the sampling control module determines the condensation rate of the control group condenser based on the pressure hysteresis period, including:

[0034] If the time interval of a single pressure hysteresis period is less than or equal to a preset time interval, increasing the condensation rate of the condenser;

[0035] If the time interval of a single pressure hysteresis period is greater than the preset time interval, the condensing rate of the condenser is reduced.

[0036] Further, the sampling control module determines the pressurization rate of the gas pressurization unit based on the time adjustment of the pressure hysteresis time period, including:

[0037] If the time interval of a single pressure hysteresis period is greater than the preset time interval, the pressurization rate of the gas pressurization system is increased.

[0038] Furthermore, the interval durations of the multiple time points range from 5 minutes to 10 minutes.

[0039] Furthermore, the target pressure has a value range of 5 MPa to 10 MPa.

[0040] Furthermore, if the time interval of a single pressure hysteresis period is less than or equal to a preset time interval, there is no need to adjust the pressurization rate of the gas pressurization system.

[0041] Compared with the prior art, the beneficial effect of the present invention is that the acid-rock reaction rapid determination experimental device of the present invention can quickly increase the pressure and achieve constant pressure fluid replenishment by integrating the acid storage tank, preheating kettle, gas booster unit, reactor, intelligent control collection unit and analysis unit. At the same time, by setting the control group and the measurement group to determine the pressure lag time, the boost rate of the gas booster system and the condenser condensation time are dynamically adjusted based on the pressure lag time, so as to further optimize the experimental process, more accurately determine the acid-rock reaction kinetic parameters, improve the accuracy of the test data, and provide parameters and basis for the acidization optimization design and acid liquid system optimization.

[0042] Furthermore, the present invention constructs a first pressure curve to reflect the pressure change process in which the pressure rises rapidly and stabilizes at the target pressure under the action of the gas boosting system, and constructs a second pressure curve to reflect the natural pressure fluctuations of the acid-rock reaction without external boosting. Based on the first pressure curve and the second pressure curve, the influence of the boosting on the pressure dynamics in the reactor can be accurately identified, thereby determining the pressure lag time period, thereby further optimizing the experimental process, being able to more accurately determine the acid-rock reaction kinetic parameters, improving the accuracy of the test data, and providing parameters and basis for acidizing optimization design and acid liquid system optimization.

[0043] Furthermore, the present invention normalizes the first pressure curve and the second pressure curve to eliminate the difference in dimension or magnitude between the two, so that the pressure changes of the two can be directly compared at the same time point. Subsequently, the pressure difference between the two normalized curves is calculated and compared with the preset pressure difference to identify the time point when the pressure changes significantly, thereby further optimizing the experimental process, being able to more accurately determine the acid-rock reaction kinetic parameters, improving the accuracy of the test data, and providing parameters and basis for the acidization optimization design and the acid system optimization.

[0044] Furthermore, the present invention determines the reaction stopping timing of the control group reaction liquid based on the pressure hysteresis time period, and uses the pressure hysteresis phenomenon to accurately control the end time point and the start time point of collecting the reaction liquid during the reaction process, thereby ensuring that the collected reaction liquid fully reflects the final state of the reaction under the target pressure conditions, further optimizing the experimental process, being able to more accurately determine the acid-rock reaction kinetic parameters, and improving the accuracy of the test data, thus providing parameters and basis for acidizing optimization design and acid system optimization.

[0045] Furthermore, the present invention adjusts the working state of the condenser in real time to optimize the condensation efficiency by monitoring the time interval of the pressure hysteresis phenomenon, thereby further optimizing the experimental process, being able to more accurately determine the acid-rock reaction kinetic parameters, improving the accuracy of the test data, and providing parameters and basis for acidizing optimization design and acid liquid system optimization.

[0046] Furthermore, the present invention achieves efficient control of the pressure in the reactor by dynamically adjusting the pressurization rate of the gas pressurization system based on the length of the pressure lag time period, ensuring that the acid-rock reaction can be carried out efficiently at the target pressure, thereby further optimizing the experimental process, being able to more accurately determine the acid-rock reaction kinetic parameters, and improving the accuracy of test data, providing parameters and basis for acidizing optimization design and acid liquid system optimization. BRIEF DESCRIPTION OF THE DRAWINGS

[0047] Figure 1 It is a connection schematic diagram of the acid-rock reaction rapid determination experimental device of the present invention;

[0048] Figure 2 This is a schematic diagram of the structure of the acid-rock reaction rapid determination experimental device of the present invention;

[0049] Figure 3 A flow chart for determining a plurality of pressure hysteresis time periods for an embodiment of the present invention;

[0050] Figure 4 A flow chart of determining the timing of stopping a reaction according to an embodiment of the present invention;

[0051] In the figure: 1, acid storage tank; 2, preheating kettle; 3, gas booster unit; 4, reaction kettle; 5, intelligent control collection unit; 501, condenser; 502, rotary sampler; 503, sampling sensor module; 504, sampling control module; 6, analysis unit. DETAILED DESCRIPTION

[0052] In order to make the objects and advantages of the present invention more clearly understood, the present invention is further described below in conjunction with embodiments; it should be understood that the specific embodiments described herein are only used to explain the present invention and are not used to limit the present invention.

[0053] The preferred embodiments of the present invention are described below with reference to the accompanying drawings. It should be understood by those skilled in the art that these embodiments are only used to explain the technical principles of the present invention and are not intended to limit the protection scope of the present invention.

[0054] It should be noted that, in the description of the present invention, terms such as "up", "down", "left", "right", "inside" and "outside" indicating directions or positional relationships are based on the directions or positional relationships shown in the drawings. This is merely for the convenience of description and does not indicate or imply that the device or element must have a specific orientation, be constructed and operated in a specific orientation. Therefore, it cannot be understood as a limitation on the present invention.

[0055] In addition, it should be noted that in the description of the present invention, unless otherwise clearly specified and limited, the terms "installed", "connected", and "connected" should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection, or it can be indirectly connected through an intermediate medium, or it can be the internal communication of two components. For those skilled in the art, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0056] See also Figure 1 , Figure 2 As shown, Figure 1 This is a schematic diagram of the connection of the acid-rock reaction rapid determination experimental device of the present invention. Figure 2 The schematic diagram of the structure of the acid-rock reaction rapid determination experimental device of the present invention is shown in FIG. Specifically, the present invention provides an acid-rock reaction rapid determination experimental device, comprising: an acid storage tank 1, a preheating kettle 2, a gas booster unit 3, a reactor 4, an intelligent control collection unit 5, and an analysis unit 6;

[0057] The acid storage tank 1 is connected to the preheating kettle 2, the acid storage tank 1 is used to store the acid solution and transport the acid solution to the preheating kettle 2, and the preheating kettle 2 is used to preheat the acid solution;

[0058] The gas pressurizing unit 3 is connected to the reactor 4 to pressurize the reactor 4 to a target pressure;

[0059] The intelligent control collection unit 5 includes a condenser 501, a rotary sampler 502 connected to the condenser 501 for collecting reaction liquid, a sampling sensor module 503, and a sampling control module 504 for judging whether sampling is completed. The condenser 501 is connected to the liquid outlet of the reactor 4. The reaction liquid in the reactor 4 enters the rotary sampler 502 after being condensed by the condenser 501. The sampling sensor module 503 is used to detect the amount of reaction liquid in the rotary sampler 502 and the condensation time of the condenser 501. The sampling control module 504 is used to determine a number of pressure hysteresis time periods according to the pressure data in the reactor 4 collected at a number of time points and the amount of reaction liquid, and determine the reaction stop timing of the control group reaction liquid and the condensation rate of the condenser 501 based on the pressure hysteresis time period;

[0060] The analysis unit 6 is connected to the intelligent control collection unit 5, and is used to adjust and determine the pressurization rate of the gas pressurization unit 3 based on the duration of the pressure lag time period, and to determine the acid-rock reaction kinetic parameters based on the pressure lag time period, the test data of the reaction liquid sample of the control group reaction liquid, and the test data of the reaction liquid sample of the measurement group reaction liquid.

[0061] Specifically, the control group is the reactor 4 that performs acid-rock reaction under preset boosting conditions; the measurement group is the reactor 4 that performs acid-rock reaction under pressure-maintaining conditions.

[0062] It is understandable that the acid storage tank 1 is used to store the acid required for the experiment, such as hydrochloric acid, hydrofluoric acid, etc. These acidic solutions will react with the rock samples in the reactor 4 in the subsequent steps. The preheating kettle 2 preheats the acid to ensure that the temperature of the acid is uniform when it enters the reactor 4. The gas booster system is responsible for pressurizing the reactor 4 to reach the target pressure required for the experiment. The condenser 501 in the intelligent control collection unit 5 is used to condense the steam or gas generated during the reaction to ensure that only liquid reaction liquid enters the subsequent collection system. The amount of reaction liquid is the content of the reaction liquid in a single test tube.

[0063] It is understandable that, due to the effect of the gas boosting system, the pressure in the reactor 4 will gradually increase to the target pressure as the reaction proceeds, and during the acid-rock reaction, the volume of the acid solution will continue to decrease, and the pressure in the reactor 4 will also decrease. In order to stabilize the pressure in the reactor 4 at the target pressure, the gas boosting system will continue to increase the pressure to maintain the constant pressure condition in the reactor 4. At the same time, since the boosting speed of the gas boosting system has a certain delay relative to the acid-rock reaction speed, it will cause inaccurate data tracking. Therefore, based on the control group and the measurement group, the several pressure lag time periods are determined, and the several pressure lag time periods reflect the response lag time of the boosting system and the time required for the pressure balance in the reactor 4. Based on the several pressure lag time periods, the boosting rate of the gas boosting system is adjusted and determined, and the condensation rate of the condenser 501 is adjusted to determine the acid-rock reaction kinetic parameters.

[0064] In implementation, the intervals between the time points are in the range of 5 min to 10 min, preferably 7 min, and the target pressure is in the range of 5 MPa to 10 MPa, preferably 7 MPa. The time points and the target pressure ranges and preferred values ​​can be determined according to actual conditions, and will not be described in detail here.

[0065] The acid-rock reaction rapid determination experimental device of the present invention can rapidly increase pressure and realize constant pressure fluid replenishment by integrating an acid storage tank 1, a preheating kettle 2, a gas booster unit 3, a reactor 4, an intelligent control collection unit 5 and an analysis unit 6. At the same time, by setting a control group and a measurement group to determine the pressure lag time, the boost rate of the gas booster system and the condensation time of the condenser 501 are dynamically adjusted based on the pressure lag time, thereby further optimizing the experimental process, being able to more accurately determine the acid-rock reaction kinetic parameters, improving the accuracy of the test data, and providing parameters and basis for the acidization optimization design and the acid liquid system optimization.

[0066] Specifically, the rotary sampler 502 is provided with a plurality of cleaning ports, and the plurality of cleaning ports are used to realize automatic cleaning of a plurality of test tubes on the rotary sampler 502 .

[0067] It can be understood that a plurality of cleaning ports can be provided on the rotary sampler 502, and the plurality of cleaning ports are mainly used for a plurality of test tubes on the rotary sampler.

[0068] In implementation, there is no specific limitation on the number and position of the cleaning ports, the cleaning method, the pressure, flow rate and time of the cleaning. As long as the cleaning of the test tubes on the rotating sampler 502 can be achieved through the cleaning ports and the best cleaning effect can be achieved, no further details will be given here.

[0069] See also Figure 3, is a flow chart of determining a plurality of pressure hysteresis time periods according to an embodiment of the present invention. Specifically, the sampling control module determines a plurality of pressure hysteresis time periods, including:

[0070] Step S1, collecting pressure data and reaction liquid volume data in the control group reactor 4 at the aforementioned several time points, and forming a first pressure curve and a first reaction liquid yield curve;

[0071] Step S2, collecting the pressure data and the reaction liquid volume data in the reaction kettle 4 of the measurement group at the several time points, and forming a second pressure curve and a second reaction liquid yield curve;

[0072] Step S3, determining a plurality of pressure mutation time points based on the first pressure curve and the second pressure curve;

[0073] Step S4, determining a plurality of response time points based on the first reaction liquid yield curve and the second reaction liquid yield curve;

[0074] Step S5, determining the plurality of pressure hysteresis time periods based on the pressure mutation time point and the plurality of response time points.

[0075] It is understandable that the first pressure curve reflects that under the action of the gas supercharging system, the pressure in the reactor 4 rises rapidly and stabilizes at the target pressure. The first pressure curve is affected by the supercharging time and the acid-rock reaction process, and therefore has a rising phase (supercharging) and a stable phase (maintaining the target pressure). The second pressure curve reflects the natural change trend of the pressure in the reactor 4 when there is no external supercharging. Since there is no external supercharging, the second pressure curve will only fluctuate according to the acid-rock reaction process. The pressure hysteresis period is determined by the first pressure curve and the second pressure curve.

[0076] The present invention constructs a first pressure curve to reflect the pressure change process in which the pressure rises rapidly and stabilizes at the target pressure under the action of the gas boosting system, and constructs a second pressure curve to reflect the natural pressure fluctuation of the acid-rock reaction without external boosting. Based on the first pressure curve and the second pressure curve, the influence of the boosting on the pressure dynamics in the reactor 4 can be accurately identified, thereby determining the pressure lag time period, thereby further optimizing the experimental process, being able to more accurately determine the acid-rock reaction kinetic parameters, improving the accuracy of the test data, and providing parameters and basis for acidizing optimization design and acid liquid system optimization.

[0077] Specifically, the sampling control module determines several pressure mutation time points, including:

[0078] Normalizing the first pressure curve and the second pressure curve;

[0079] At the same time point, determining the normalized pressure difference between the first pressure curve and the second pressure curve;

[0080] The pressure difference is compared with a preset pressure difference, and a pressure mutation time point is determined according to the comparison result.

[0081] It can be understood that since the first pressure curve is obtained under pressurized conditions and the second pressure curve is obtained under unpressurized conditions, the first pressure curve and the second pressure curve are normalized, and the pressure difference between the first pressure curve and the second pressure curve at the same time point is determined. The pressure difference reflects the pressure difference in the reactor 4 during the acid-rock reaction process with or without pressurization. The preset pressure difference is used to determine whether the pressure in the reactor 4 changes significantly. Assuming that the pressure difference at a certain time point exceeds the preset pressure difference, it is considered that the pressure in the reactor 4 changes suddenly at this time point, thereby determining the time point of the pressure mutation.

[0082] In a specific embodiment, the first pressure curve P1(t) and the second pressure curve P2(t) are normalized to obtain normalized curves P'1(t) and P'2(t). The normalization formula is as follows:

[0083]

[0084]

[0085] Among them, P'1(t i ) is the first pressure curve after normalization i Pressure data at a time point, P1(t i ) is the first pressure curve t i Pressure data at a given time point, P 1min (t) is the minimum value of the pressure data in the first pressure curve, P 1max (t) is the maximum value of the pressure data in the first pressure curve, i = 1, 2, .., n, n is the number of pressure data. i ) is the normalized second pressure curve t i Pressure data at a given time point, P2(t i ) is the t in the second pressure curve i Pressure data at a given time point, P 2min (t) is the minimum value of the pressure data in the second pressure curve, P 2max (t) is the maximum value of the pressure data in the second pressure curve.

[0086] The formula for determining the pressure difference between the normalized first pressure curve and the second pressure curve at several reaction time points is as follows:

[0087] ΔP(t i)=|P1'(t i )-P2'(t i )| (3)

[0088] Among them, ΔP(t i ) is t i The pressure difference between the first pressure curve and the second pressure curve after normalization at a certain time point.

[0089] In implementation, the preset pressure difference has a value range of 0.5 MPa to 0.65 MPa. Preferably, the preset pressure difference is 0.55 MPa. The value range and preferred value of the preset pressure difference can be determined according to actual conditions and will not be elaborated here.

[0090] The present invention normalizes the first pressure curve and the second pressure curve to eliminate the difference in dimension or magnitude between the two, so that the pressure changes of the two can be directly compared at the same time point. Subsequently, the pressure difference between the two normalized curves is calculated and compared with the preset pressure difference to identify the time point when the pressure changes significantly, thereby further optimizing the experimental process, being able to more accurately determine the acid-rock reaction kinetic parameters, improving the accuracy of the test data, and providing parameters and basis for the acidization optimization design and the acid system optimization.

[0091] Specifically, the sampling control module determines several response time points, including:

[0092] At the same time point, determining the difference in reaction liquid yield between the first reaction liquid yield curve and the second reaction liquid yield curve;

[0093] The reaction solution yield difference is compared with a preset reaction solution yield difference, and a response time point is determined according to the comparison result. Specifically, the time point when the reaction solution yield difference is greater than the preset reaction solution yield difference is determined as the response time point.

[0094] t j At the time point, the reaction solution yield difference is calculated as follows:

[0095] ΔM(t j )=|M1(t j )-M2(t j )| (4)

[0096] Among them, M1(t j ) is t j The yield of the first reaction liquid at the time point, M2(t j ) is t j The output of the second reaction liquid at the time point, j is the number of response time points.

[0097] In implementation, the preset range of the reaction liquid yield difference is 5ml to 10ml. Preferably, the preset value of the reaction liquid yield is 6ml. The preset range and preferred value of the reaction liquid yield difference need to be adjusted according to actual conditions and will not be repeated here.

[0098] Specifically, the sampling control module determines the plurality of pressure hysteresis time periods based on the plurality of pressure mutation time points and the plurality of response time points, including:

[0099] Matching the plurality of pressure mutation time points with the plurality of response time points;

[0100] The time difference between the pressure mutation time point and the response time point after matching is determined based on the matching results.

[0101] It is understandable that the purpose of matching is to find the response time point of the acid-rock reaction after each pressure mutation time point. Each pressure mutation time point is matched with its nearest response time point. Once the pressure mutation time point and the response time point are successfully matched, the time difference between the two can be calculated. This time difference is the duration of the pressure lag time period. The pressure lag time period is of great significance for understanding reaction kinetics, optimizing reaction conditions, and evaluating the response speed of the reaction system.

[0102] The calculation formula for the duration (time difference) of the mth pressure hysteresis period is as follows:

[0103] Δt m =|t i -t j | (5)

[0104] Among them, t i is the i-th response time point, t j is the jth pressure mutation time point.

[0105] See also Figure 4 , is a flow chart of determining the reaction stopping time according to an embodiment of the present invention. Specifically, the sampling control module determines the reaction stopping time of the control group reaction solution based on the pressure hysteresis time period, including:

[0106] Collecting the reaction solution of the control group at the cutoff time point of the pressure hysteresis period;

[0107] Stop collecting the reaction solution of the control group at the initial time point of the pressure hysteresis period.

[0108] It is understandable that collecting the reaction liquid of the control group at the cut-off time point of the pressure hysteresis time period means that the pressure in the reactor 4 reaches the target pressure at this time. Collecting the reaction liquid at this time can ensure that the collected reaction liquid fully reflects the final state of the reaction under the target pressure condition, avoiding experimental errors caused by collecting too early or too late. At the same time, stopping collecting the reaction liquid of the control group at the initial time point of the pressure hysteresis time period means that the reaction liquid is not collected after the pressure hysteresis phenomenon begins to appear.

[0109] The present invention determines the reaction stopping timing of the reaction liquid of the control group based on the pressure hysteresis time period, and uses the pressure hysteresis phenomenon to accurately control the end time point and the start time point of collecting the reaction liquid during the reaction process, thereby ensuring that the collected reaction liquid fully reflects the final state of the reaction under the target pressure conditions, further optimizing the experimental process, being able to more accurately determine the acid-rock reaction kinetic parameters, and improving the accuracy of the test data, thus providing parameters and basis for the acidizing optimization design and the acid liquid system optimization.

[0110] Specifically, the sampling control module determines the condensation rate of the control group condenser 501 based on the pressure hysteresis period, including:

[0111] If the time interval of a single pressure hysteresis period is less than or equal to a preset time interval, increasing the condensation rate of the condenser 501;

[0112] If the time interval of a single pressure hysteresis period is greater than the preset time interval, the condensation rate of the condenser 501 is reduced.

[0113] It is understandable that when the time interval of a single pressure hysteresis time period is less than or equal to the preset time interval, it means that the pressure does not fluctuate significantly during the condensation process and there is no hysteresis phenomenon, so the condensation rate is increased to shorten the time of the entire condensation process. When the time interval of a single pressure hysteresis time period is greater than the preset time interval, it means that the pressure hysteresis time is too long at this time, which will also affect the reaction liquid yield, so the condensation rate of the condenser 501 is reduced.

[0114] The present invention adjusts the working state of the condenser 501 in real time by monitoring the time interval of the pressure hysteresis phenomenon to optimize the condensation efficiency, thereby further optimizing the experimental process, being able to more accurately determine the acid-rock reaction kinetic parameters, improving the accuracy of the test data, and providing parameters and basis for acidizing optimization design and acid liquid system optimization.

[0115] Specifically, the sampling control module determines the pressurization rate of the gas pressurization unit 3 based on the duration of the pressure hysteresis period, including:

[0116] If the time interval of a single pressure hysteresis period is less than or equal to the preset time interval, the gas pressurization system does not pressurize the reactor 4;

[0117] If the time interval of a single pressure hysteresis period is greater than the preset time interval, the pressurization rate of the gas pressurization system is increased.

[0118] It is understandable that if the time interval of a single pressure hysteresis time period is less than or equal to the preset time interval, it means that the pressure change in the reactor 4 has reached or is close to the constant pressure state (target pressure). At this time, the gas boosting system chooses not to boost the reactor 4. If the time interval of a single pressure hysteresis time period is greater than the preset time interval, it means that the boosting rate of the current gas boosting system is too slow. In order to ensure that the acid-rock reaction is carried out at the target pressure, the boosting rate of the gas boosting system is increased. By increasing the boosting rate, the required target pressure is reached faster. Preferably, the single increase value of the boosting rate is set to 10% to 30% of the boosting rate before adjustment.

[0119] The present invention realizes efficient control of the pressure in the reactor 4 by dynamically adjusting the pressurization rate of the gas pressurization system based on the length of the pressure lag time period, ensuring that the acid-rock reaction can be carried out efficiently at the target pressure, thereby further optimizing the experimental process, being able to more accurately determine the acid-rock reaction kinetic parameters, improving the accuracy of the test data, and providing parameters and basis for acidizing optimization design and acid liquid system optimization.

[0120] Embodiment 1:

[0121] a. Install the fixed rock sample on the rotating connecting rod and put it into reactor 4. Close the shutoff valve between preheating reactor 2 and reactor 4, add 500mL of acid solution into preheating reactor 2, set the test temperature, control the heating rate, which is not higher than 5℃ / min, and heat the preheating reactor 2, acid-rock reactor 4 and rock sample. When the temperature is about to reach the set temperature, increase the pressure through the gas booster system (control group), and the pressure in reactor 4 rises to 7MPa.

[0122] b. Same as step a, but after the preheating kettle 2, the acid-rock reaction kettle 4 and the rock sample are heated, the acid solution is directly flowed into the reaction kettle 4 for acid-rock reaction (measurement group).

[0123] c. Open the sampling valve at several reaction time points to take samples, collect parameters such as pressure and reaction liquid volume in the system in real time, and determine the pressure lag time period. Based on the test data of the pressure lag time period, reaction liquid samples of the control group reaction liquid, and reaction liquid samples of the measurement group reaction liquid, further determine the acid-rock reaction kinetic parameters.

[0124] So far, the technical solutions of the present invention have been described in conjunction with the preferred embodiments shown in the accompanying drawings. However, it is easy for those skilled in the art to understand that the protection scope of the present invention is obviously not limited to these specific embodiments. Without departing from the principle of the present invention, those skilled in the art can make equivalent changes or substitutions to the relevant technical features, and the technical solutions after these changes or substitutions will fall within the protection scope of the present invention.

Claims

1. An acid-rock reaction rapid determination experimental device, characterized in that: include: Acid storage tank, preheating kettle, gas pressurization unit, reactor, intelligent control collection unit and analysis unit; The acid storage tank is connected to the preheating kettle, the acid storage tank is used to store acid solution and transport the acid solution to the preheating kettle, and the preheating kettle is used to preheat the acid solution; The gas pressurizing unit is connected to the reactor to pressurize the reactor to a target pressure; The intelligent control collection unit includes a condenser, a rotary sampler connected to the condenser for collecting reaction liquid, a sampling sensor module, and a sampling control module for judging whether the sampling is completed. The condenser is connected to the liquid outlet of the reactor. The reaction liquid in the reactor enters the rotary sampler after being condensed by the condenser. The sampling sensor module is used to detect the amount of reaction liquid in the rotary sampler and the condensation time of the condenser. The sampling control module is used to determine a number of pressure hysteresis time periods according to the pressure data in the reactor collected at a number of time points and the amount of reaction liquid, and determine the reaction stop timing of the control group reaction liquid and the condensation rate of the condenser based on the pressure hysteresis time period; The analysis unit is connected to the intelligent control collection unit, and is used to adjust and determine the pressurization rate of the gas pressurization unit based on the duration of the pressure lag time period, and to determine the acid-rock reaction kinetic parameters based on the pressure lag time period, the test data of the reaction liquid samples of the control group reaction liquid, and the test data of the reaction liquid samples of the measurement group reaction liquid.

2. The acid-rock reaction rapid determination experimental device according to claim 1 is characterized in that: The control group is a reactor that performs an acid-rock reaction under a preset boosting condition; the measurement group is a reactor that performs an acid-rock reaction under a pressure-maintaining condition.

3. The acid-rock reaction rapid determination experimental device according to claim 1 is characterized in that: The rotary sampler is provided with a plurality of cleaning ports, and the plurality of cleaning ports are used for realizing automatic cleaning of a plurality of test tubes on the rotary sampler.

4. The acid-rock reaction rapid determination experimental device according to claim 1 is characterized in that: The sampling control module determines a number of pressure hysteresis time periods, including: Collecting pressure data and reaction liquid volume data in the control group reactor at the plurality of time points, and forming a first pressure curve and a first reaction liquid yield curve; Collecting the pressure data and the reaction liquid volume data in the reaction kettle of the measurement group at the several time points, and forming a second pressure curve and a second reaction liquid yield curve; determining a plurality of pressure mutation time points based on the first pressure curve and the second pressure curve; Determining a plurality of response time points based on the first reaction liquid yield curve and the second reaction liquid yield curve; The plurality of pressure hysteresis time periods are determined based on the pressure mutation time point and the plurality of response time points.

5. The acid-rock reaction rapid determination experimental device according to claim 4 is characterized in that: The sampling control module determines a number of pressure mutation time points, including: Normalizing the first pressure curve and the second pressure curve; At the same time point, determining the normalized pressure difference between the first pressure curve and the second pressure curve; The pressure difference is compared with a preset pressure difference, and a pressure mutation time point is determined according to the comparison result.

6. The acid-rock reaction rapid determination experimental device according to claim 5, characterized in that: The sampling control module determines a number of response time points, including: At the same time point, determining the difference in reaction liquid yield between the first reaction liquid yield curve and the second reaction liquid yield curve; The reaction solution yield difference is compared with a preset reaction solution yield difference, and a response time point is determined according to the comparison result.

7. The acid-rock reaction rapid determination experimental device according to any one of claims 4 to 6, characterized in that: The sampling control module determines the plurality of pressure hysteresis time periods based on the plurality of pressure mutation time points and the plurality of response time points, including: Matching the plurality of pressure mutation time points with the plurality of response time points; The time difference between the pressure mutation time point and the response time point after matching is determined based on the matching results.

8. The acid-rock reaction rapid determination experimental device according to claim 1, characterized in that: The sampling control module determines the reaction stop timing of the control group reaction solution based on the pressure hysteresis period, including: Collecting the reaction solution of the control group at the cutoff time point of the pressure hysteresis period; Stop collecting the reaction solution of the control group at the initial time point of the pressure hysteresis period.

9. The acid-rock reaction rapid determination experimental device according to claim 1, characterized in that: The sampling control module determines the condensation rate of the control group condenser based on the pressure hysteresis period, including: If the time interval of a single pressure hysteresis period is less than or equal to a preset time interval, increasing the condensation rate of the condenser; If the time interval of a single pressure hysteresis period is greater than the preset time interval, the condensing rate of the condenser is reduced.

10. The acid-rock reaction rapid determination experimental device according to claim 1, characterized in that: The sampling control module determines the pressurization rate of the gas pressurization unit based on the time length of the pressure hysteresis period, including: If the time interval of a single pressure hysteresis period is greater than the preset time interval, the pressurization rate of the gas pressurization system is increased.

11. The acid-rock reaction rapid determination experimental device according to claim 4, characterized in that: The interval lengths of the multiple time points range from 5 minutes to 10 minutes.

12. The acid-rock reaction rapid determination experimental device according to claim 1, characterized in that: The target pressure ranges from 5 MPa to 10 MPa.

13. The acid-rock reaction rapid determination experimental device according to claim 10, characterized in that: It also includes that if the time interval of a single pressure hysteresis period is less than or equal to a preset time interval, there is no need to adjust the pressurization rate of the gas pressurization system.

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