A rapid experimental apparatus for determining acid-rock reactions

The experimental device for rapid determination of acid-rock reaction, which integrates an acid storage tank, a preheating vessel, a gas pressurization unit, a reaction vessel, an intelligent control collection unit, and an analysis unit, solves the problem of inaccurate data caused by slow pressurization speed and achieves efficient and accurate determination of acid-rock reaction kinetic parameters.

CN119224263BActive Publication Date: 2025-11-14DAQING OILFIELD CO LTD +1
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Patent Information

Application Number
CN202411362479.3
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-09-27
Publication Date
2025-11-14
Estimated Expiration
2044-09-27

AI Technical Summary

Technical Problem

The existing acid-rock reaction experimental device has a slow pressurization rate, which cannot match the high speed of the acid-rock reaction in time, resulting in inaccurate data tracking.

Method used

Design an experimental device for rapid determination of acid-rock reaction, integrating an acid storage tank, a preheating vessel, a gas pressurization unit, a reaction vessel, an intelligent control collection unit, and an analysis unit. Determine the pressure lag time through a control group and a measurement group, dynamically adjust the pressurization rate of the gas pressurization unit and the condenser condensation time, and optimize the experimental process.

Benefits of technology

It enables rapid pressure increase and maintenance of constant pressure, improves the accuracy of test data, and provides parameters and basis for acidification optimization design and acid system selection.

✦ Generated by Eureka AI based on patent content.

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Abstract

This invention relates to the field of petroleum geological testing technology, and more particularly to an experimental device for rapid determination of acid-rock reaction, comprising: an acid storage tank, a preheating vessel, a gas pressurization unit, a reaction vessel, an intelligent control collection unit, and an analysis unit. The acid storage tank delivers acid to the preheating vessel for preheating; the gas pressurization system increases the pressure in the reaction vessel to a target pressure; the sampling sensor module in the intelligent control collection unit detects the volume of reaction liquid in the rotary sampler and the condensation time of the condenser; the sampling control module determines several pressure lag time periods based on the pressure data and reaction liquid volume collected in the reaction vessel at several time points, thereby determining the reaction cessation time of the control group reaction liquid, the condensation rate of the condenser, the pressurization rate of the gas pressurization unit, and the acid-rock reaction kinetic parameters. This invention effectively and rapidly increases pressure and achieves constant pressure replenishment, is easy to operate, improves automatic sampling efficiency, and enhances the accuracy of test data.
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Description

Technical Field

[0001] This invention relates to the field of petroleum geological testing technology, and in particular to an experimental device for rapid determination of acid rock reaction. Background Technology

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

[0003] Chinese Patent Publication No. CN118294582A discloses an experimental apparatus and method for acid-rock reaction kinetics. The experimental apparatus includes a reaction vessel, an acid storage tank, a timed sampling system, a manual pump device, and a gas cylinder. The method includes: during the acid-rock reaction, as the volume and pressure of the acid in the reaction vessel gradually decrease, the manual pump device is used to increase the pressure and replenish the acid in the reaction vessel without stopping the experiment, ensuring the continuity of the reaction.

[0004] Therefore, the above technical solution has the following problems: when increasing the pressure in the reactor using a manual pump, the pressurization rate is slow, but the acid-rock reaction rate is fast, leading to inaccurate data tracking. Therefore, it is necessary to study a rapid experimental device for measuring acid-rock reactions that can quickly increase pressure and achieve constant-pressure replenishment, improving the accuracy of test data, and providing parameters and basis for acidification optimization design and acid system selection. Summary of the Invention

[0005] To address this issue, the present invention provides a rapid experimental device for measuring acid-rock reactions, which overcomes the problem in the prior art where the acid-rock experimental device has slow pressurization and fails to match the high speed of the acid-rock reaction in time, resulting in a lag in data tracking.

[0006] To achieve the above objectives, the present invention provides an experimental apparatus for rapid determination of acid-rock reactions, comprising:

[0007] Acid storage tank, preheating kettle, gas pressurization unit, reaction kettle, 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 and transport the acid to the preheating kettle. The preheating kettle is used to preheat the acid.

[0009] The gas pressurization unit is connected to the reactor to pressurize the reactor to the target pressure.

[0010] The intelligent control collection unit includes a condenser, a rotary sampler connected to the condenser for collecting the reaction liquid, a sampling sensing module, and a sampling control module for determining whether sampling is complete. The condenser is connected to the liquid outlet of the reaction vessel. The reaction liquid in the reaction vessel is condensed by the condenser and then enters the rotary sampler. The sampling sensing 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 several pressure lag time periods based on the pressure data collected in the reaction vessel at several time points and the amount of reaction liquid, and to determine the reaction stop time of the control group reaction liquid and the condensation rate of the condenser based on the pressure lag time periods.

[0011] The analysis unit, which is connected to the intelligent control and collection unit, is used to 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 sample of the control group reaction liquid, and the test data of the reaction liquid sample of the measurement group reaction liquid.

[0012] Furthermore, the control group consists of the reactor undergoing acid-rock reaction under preset pressure conditions; the measurement group consists of the reactor undergoing acid-rock reaction under pressure-holding conditions.

[0013] Furthermore, the rotary sampler is provided with several cleaning ports, which are used to automatically clean several test tubes on the rotary sampler.

[0014] Furthermore, the sampling control module determines several pressure hysteresis time periods, including:

[0015] Pressure data and reaction liquid volume data in the control group reactor were collected at several time points, and a first pressure curve and a first reaction liquid production curve were generated.

[0016] The pressure data and reaction liquid volume data in the reactor group were collected at several time points, and a second pressure curve and a second reaction liquid production curve were generated.

[0017] Several pressure change time points are determined based on the first pressure curve and the second pressure curve;

[0018] Several response time points are determined based on the first reaction liquid yield curve and the second reaction liquid yield curve;

[0019] The pressure lag time periods are determined based on the pressure abrupt change time point and several response time points.

[0020] Furthermore, the sampling control module determines several pressure change time points, including:

[0021] The first pressure curve and the second pressure curve are normalized.

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

[0023] The pressure difference is compared with the preset pressure difference, and the pressure change time point is determined based on the comparison result.

[0024] Furthermore, the sampling control module determines several response time points, including:

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

[0026] The difference in the yield of the reaction solution is compared with the preset difference in the yield of the reaction solution, and the response time point is determined based on the comparison result.

[0027] Furthermore, the sampling control module determines the plurality of pressure lag time periods based on the plurality of pressure abrupt change time points and the plurality of response time points, including:

[0028] Match the aforementioned pressure mutation time points with the aforementioned 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 cessation timing of the control group reaction solution based on the pressure hysteresis time period, including:

[0031] The control group reaction solution was collected at the end of the pressure hysteresis period.

[0032] The collection of the control group reaction solution was stopped at the initial time point of the pressure hysteresis period.

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

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

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

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

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

[0038] Furthermore, the interval between the aforementioned time points ranges from 5 min to 10 min.

[0039] Furthermore, the target pressure ranges from 5 MPa to 10 MPa.

[0040] Furthermore, it also includes the option that if the time interval of a single pressure lag time period is less than or equal to a preset time interval, then there is no need to adjust the pressurization rate of the gas pressurization unit.

[0041] Compared with existing technologies, the beneficial effects of this invention are as follows: the rapid acid-rock reaction determination experimental device of this invention integrates an acid storage tank, a preheating vessel, a gas pressurization unit, a reaction vessel, an intelligent control collection unit, and an analysis unit, enabling it to rapidly increase pressure and achieve constant pressure replenishment. Simultaneously, by setting up a control group and a measurement group to determine the pressure lag time, and dynamically adjusting the pressurization rate of the gas pressurization unit and the condenser condensation time based on the pressure lag time, the experimental process is further optimized. This allows for more accurate determination of acid-rock reaction kinetic parameters, improves the accuracy of test data, and provides parameters and basis for acidification optimization design and acid system selection.

[0042] Furthermore, this invention constructs a first pressure curve to reflect the pressure change process of rapid pressure rise and stabilization at the target pressure under the action of the gas pressurization unit, and constructs a second pressure curve to reflect the natural pressure fluctuation of the acid-rock reaction without external pressurization. Based on the first and second pressure curves, the influence of pressurization on the pressure dynamics inside the reactor can be accurately identified, thereby determining the pressure lag time period, thus further optimizing the experimental process, more accurately determining the kinetic parameters of the acid-rock reaction, improving the accuracy of the test data, and providing parameters and basis for acidification optimization design and acid system selection.

[0043] Furthermore, this invention normalizes the first and second pressure curves, eliminating their differences in dimensions or magnitudes, allowing direct comparison of their pressure changes at the same time point. Subsequently, the pressure difference between the normalized two curves is calculated and compared with a preset pressure difference to identify the time points where significant pressure changes occur. This further optimizes the experimental procedure, enabling more accurate determination of acid-rock reaction kinetic parameters, improving the accuracy of test data, and providing parameters and basis for optimized acidification design and optimal acid system selection.

[0044] Furthermore, this invention determines the reaction cessation time of the control group reaction solution based on the pressure hysteresis time period, and uses the pressure hysteresis phenomenon to precisely control the end and start time points of the reaction process collection of the reaction solution, ensuring that the collected reaction solution fully reflects the final state of the reaction under the target pressure conditions, further optimizing the experimental process, enabling more accurate determination of acid-rock reaction kinetic parameters, improving the accuracy of test data, and providing parameters and basis for acidification optimization design and acid solution system selection.

[0045] Furthermore, this invention adjusts the working state of the condenser in real time by monitoring the time interval of pressure hysteresis to optimize condensation efficiency, thereby further optimizing the experimental process. It can more accurately determine the acid-rock reaction kinetic parameters, improve the accuracy of test data, and provide parameters and basis for acidification optimization design and acid system selection.

[0046] Furthermore, this invention achieves efficient control of the pressure inside the reactor by dynamically adjusting the pressurization rate of the gas pressurization unit based on the duration of the pressure lag time, ensuring that the acid-rock reaction can proceed efficiently under the target pressure. This further optimizes the experimental process, enables more accurate determination of the acid-rock reaction kinetic parameters, improves the accuracy of test data, and provides parameters and basis for acidification optimization design and acid system selection. Attached Figure Description

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

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

[0049] Figure 3 A flowchart for determining several pressure hysteresis time periods in an embodiment of the present invention;

[0050] Figure 4 A flowchart for determining the timing of reaction cessation in an embodiment of the present invention;

[0051] In the diagram: 1, acid storage tank; 2, preheating vessel; 3, gas pressurization unit; 4, reaction vessel; 5, intelligent control collection unit; 501, condenser; 502, rotary sampler; 503, sampling sensor module; 504, sampling control module; 6, analysis unit. Detailed Implementation

[0052] To make the objectives and advantages of the present invention clearer, the present invention will be further described below with reference to embodiments; it should be understood that the specific embodiments described herein are merely for explaining the present invention and are not intended to limit the present invention.

[0053] Preferred embodiments of the present invention will now be described with reference to the accompanying drawings. Those skilled in the art should understand that these embodiments are merely illustrative of the technical principles of the present invention and are not intended to limit the scope of protection of the present invention.

[0054] It should be noted that in the description of this invention, the terms "upper", "lower", "left", "right", "inner", "outer", etc., which indicate directions or positional relationships, are based on the directions or positional relationships shown in the accompanying drawings. This is only for the convenience of description and is not intended to indicate or imply that the device or element must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, it should not be construed as a limitation of this invention.

[0055] Furthermore, it should be noted that, in the description of this invention, unless otherwise explicitly specified and limited, the terms "installation," "connection," and "linking" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; and they can refer to the internal connection of two components. Those skilled in the art can understand the specific meaning of the above terms in this invention according to the specific circumstances.

[0056] Please see Figure 1 , Figure 2 As shown, Figure 1 This is a schematic diagram of the connection of the experimental apparatus for rapid determination of acid-rock reaction of the present invention. Figure 2 This is a schematic diagram of the experimental apparatus for rapid determination of acid-rock reaction according to the present invention. Specifically, the present invention provides an experimental apparatus for rapid determination of acid-rock reaction, comprising: an acid storage tank 1, a preheating vessel 2, a gas pressurization unit 3, a reaction vessel 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 acid and transport the acid to the preheating kettle 2. The preheating kettle 2 is used to preheat the acid.

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

[0059] The intelligent control collection unit 5 includes a condenser 501, a rotary sampler 502 connected to the condenser 501 for collecting the reaction liquid, a sampling sensor module 503, and a sampling control module 504 for determining whether sampling is complete. The condenser 501 is connected to the outlet of the reaction vessel 4. The reaction liquid in the reaction vessel 4 is condensed by the condenser 501 and then enters the rotary sampler 502. 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 several pressure lag time periods based on the pressure data collected in the reaction vessel 4 at several time points and the amount of reaction liquid, and to determine the reaction stop time of the control group reaction liquid and the condensation rate of the condenser 501 based on the pressure lag time periods.

[0060] The analysis unit 6, which is connected to the intelligent control and collection unit 5, is used to 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 reaction vessel 4 undergoing acid-rock reaction under a preset pressurization condition; the measurement group is the reaction vessel 4 undergoing acid-rock reaction under a pressure-holding condition.

[0062] Understandably, the acid storage tank 1 is used to store the acid solutions required for the experiment, such as hydrochloric acid and hydrofluoric acid, which will react with the rock samples in the reaction vessel 4 in subsequent steps. The preheating vessel 2 preheats the acid solutions to ensure uniform temperature when they enter the reaction vessel 4. The gas pressurization unit is responsible for pressurizing the reaction vessel 4 to reach the target pressure required for the experiment. The condenser 501 in the intelligent collection unit 5 is used to condense the vapor or gas generated during the reaction, ensuring that only liquid reaction solution enters the subsequent collection system. The amount of reaction solution is the content of reaction solution in a single test tube.

[0063] Understandably, due to the action of the gas pressurization unit, the pressure inside reactor 4 will gradually increase to the target pressure as the reaction proceeds. Furthermore, during the acid-rock reaction, the acid volume continuously decreases, and the pressure inside reactor 4 also decreases. To stabilize the pressure in reactor 4 at the target pressure, the gas pressurization unit continuously increases the pressure to maintain constant pressure conditions. However, because the pressurization rate of the gas pressurization unit is somewhat delayed relative to the acid-rock reaction rate, it can lead to inaccurate data tracking. Therefore, several pressure lag time periods are determined based on the control and measurement groups. These pressure lag time periods reflect the response lag time of the pressurization system and the time required for pressure equilibrium within reactor 4. Based on these pressure lag time periods, the pressurization rate of the gas pressurization unit is adjusted, and the condensation rate of the condenser 501 is also adjusted to determine the acid-rock reaction kinetic parameters.

[0064] In implementation, the interval between the specified time points ranges from 5 to 10 minutes, preferably 7 minutes. The target pressure ranges from 5 MPa to 10 MPa, preferably 7 MPa. The range and preferred values ​​of the specified time points and target pressure can be determined according to actual conditions, and will not be elaborated here.

[0065] The rapid acid-rock reaction determination experimental device of the present invention integrates an acid storage tank 1, a preheating vessel 2, a gas pressurization unit 3, a reaction vessel 4, an intelligent control collection unit 5, and an analysis unit 6, enabling rapid pressure increase and constant-pressure liquid replenishment. Simultaneously, by setting up a control group and a measurement group to determine the pressure lag time, and based on the pressure lag time, the pressurization rate of the gas pressurization unit and the condensation time of the condenser 501 are dynamically adjusted, thereby further optimizing the experimental process. This allows for more accurate determination of acid-rock reaction kinetic parameters, improves the accuracy of test data, and provides parameters and basis for acidification optimization design and acid system selection.

[0066] Specifically, the rotary sampler 502 is provided with several cleaning ports, which are used to automatically clean several test tubes on the rotary sampler 502.

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

[0068] In practice, there are no specific limitations on the number and location of the cleaning ports, the cleaning method, the cleaning pressure, flow rate, and time. As long as the cleaning ports can be used to clean the test tubes on the rotary sampler 502 and achieve the best cleaning effect, it is acceptable. Further details are omitted here.

[0069] Please see Figure 3This is a flowchart illustrating the determination of several pressure hysteresis time periods in an embodiment of the present invention. Specifically, the sampling control module determines several pressure hysteresis time periods, including:

[0070] Step S1: Collect pressure data and reaction liquid volume data in the control group reactor 4 at several time points, and form a first pressure curve and a first reaction liquid production curve;

[0071] Step S2: Collect pressure data and reaction liquid volume data in the reactor 4 at several time points, and form a second pressure curve and a second reaction liquid production curve;

[0072] Step S3: Determine several pressure change time points based on the first pressure curve and the second pressure curve;

[0073] Step S4: Determine several response time points based on the first reaction liquid yield curve and the second reaction liquid yield curve;

[0074] Step S5: Determine the plurality of pressure lag time periods based on the pressure abrupt change time points and the plurality of response time points.

[0075] Understandably, the first pressure curve reflects the rapid rise and stabilization of pressure within reactor 4 under the action of the gas pressurization unit. This first pressure curve is affected by the pressurization time and the acid-rock reaction process, thus exhibiting a rising phase (pressurization) and a stabilizing phase (maintaining the target pressure). The second pressure curve reflects the natural pressure change trend within reactor 4 without external pressurization. Since there is no external pressurization, the second pressure curve will only fluctuate according to the acid-rock reaction process. The pressure lag time period is determined using both the first and second pressure curves.

[0076] This invention constructs a first pressure curve to reflect the pressure change process of rapid pressure rise and stabilization at the target pressure under the action of the gas pressurization unit, and constructs a second pressure curve to reflect the natural pressure fluctuation of the acid-rock reaction without external pressurization. Based on the first and second pressure curves, the influence of pressurization on the pressure dynamics inside the reactor 4 can be accurately identified, thereby determining the pressure lag time period, further optimizing the experimental process, more accurately determining the kinetic parameters of the acid-rock reaction, improving the accuracy of the test data, and providing parameters and basis for acidification optimization design and acid system selection.

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

[0078] The first pressure curve and the second pressure curve are normalized.

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

[0080] The pressure difference is compared with the preset pressure difference, and the pressure change time point is determined based on the comparison result.

[0081] It is understandable 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 reactor 4 during the acid-rock reaction process with and without pressurization. The preset pressure difference value is used to determine whether the pressure in reactor 4 has changed significantly. If the pressure difference value at a certain time point exceeds the preset pressure difference value, it is considered that the pressure in reactor 4 has changed abruptly at that time point, thereby determining the time point of pressure change.

[0082] In one specific embodiment, the first pressure curve Second pressure curve Normalization is performed to obtain the normalized curve. and The normalization formula is as follows:

[0083] (1)

[0084] (2)

[0085] in, For the first pressure curve after normalization Stress data at specific points in time. For the first pressure curve Stress data at specific points in time. This represents the minimum pressure value in the first pressure curve. This represents the maximum pressure value in the first pressure curve. , This represents the number of pressure data points. For the normalized second pressure curve Stress data at specific points in time. For the second pressure curve Stress data at specific points in time. This represents the minimum pressure value in the second pressure curve. This represents the maximum pressure data in the second pressure curve.

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

[0087] (3)

[0088] in, for The pressure difference between the first and second pressure curves after normalization at a given time point.

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

[0090] This invention normalizes the first and second pressure curves, eliminating their differences in dimensions or magnitudes, allowing direct comparison of pressure changes at the same time point. Subsequently, the pressure difference between the normalized curves is calculated and compared with a preset pressure difference to identify the time points where significant pressure changes occur. This further optimizes the experimental procedure, enabling more accurate determination of acid-rock reaction kinetic parameters, improving the accuracy of test data, and providing parameters and basis for optimized acidification design and optimal acid system selection.

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

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

[0093] The difference in reaction liquid yield is compared with a preset difference in reaction liquid yield, and the response time point is determined based on the comparison result. Specifically, the time point when the difference in reaction liquid yield is greater than the preset difference in reaction liquid yield is determined as the response time point.

[0094] The formula for calculating the difference in reaction liquid yield at a given time point is as follows:

[0095] =| (4)

[0096] in, for Yield of the first reaction solution at the specified time point for The yield of the second reaction liquid at time point j, where j is the number of response time points.

[0097] In practice, the preset reaction liquid yield difference ranges from 5ml to 10ml. Preferably, the preset reaction liquid yield difference is 6ml. The range and preferred value of the preset reaction liquid yield difference need to be adjusted according to the actual situation, which will not be elaborated here.

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

[0099] Match the aforementioned pressure mutation time points with the aforementioned 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] Understandably, the purpose of matching is to find the corresponding response time of the acid-rock reaction after each pressure abrupt change. Each pressure abrupt change time is matched with its nearest response time. Once a match is successfully found, the time difference between the two can be calculated; this time difference is the duration of the pressure lag period. The pressure lag period is crucial for understanding reaction kinetics, optimizing reaction conditions, and evaluating the response rate of the reaction system.

[0102] The formula for calculating the duration (time difference) of the m-th pressure lag time period is as follows:

[0103] | (5)

[0104] in, For the i-th response time point, For the first A stress mutation time point.

[0105] Please see Figure 4 This is a flowchart illustrating the process of determining the reaction cessation timing in an embodiment of the present invention. Specifically, the sampling control module determines the reaction cessation timing of the control group reaction solution based on the pressure hysteresis time period, including:

[0106] The control group reaction solution was collected at the end of the pressure hysteresis period.

[0107] The collection of the control group reaction solution was stopped at the initial time point of the pressure hysteresis period.

[0108] It is understandable that collecting the control group reaction solution at the end of the pressure lag period means that the pressure inside reactor 4 has reached the target pressure. Collecting the reaction solution at this point ensures that the collected solution fully reflects the final state of the reaction under the target pressure conditions, avoiding experimental errors caused by collecting too early or too late. Conversely, stopping the collection of the control group reaction solution at the beginning of the pressure lag period means that no reaction solution is collected after the pressure lag phenomenon begins to appear.

[0109] This invention determines the reaction cessation time of the control group reaction solution based on the pressure hysteresis time period. It utilizes the pressure hysteresis phenomenon to precisely control the end and start times of reaction solution collection, ensuring that the collected reaction solution fully reflects the final state of the reaction under the target pressure conditions. This further optimizes the experimental process, enabling more accurate determination of acid-rock reaction kinetic parameters, improving the accuracy of test data, and providing parameters and basis for acidification optimization design and acid system selection.

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

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

[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] Understandably, when the time interval of a single pressure lag time is less than or equal to the preset time interval, it indicates that the pressure fluctuation during condensation is not significant and there is no lag phenomenon. Therefore, the condensation rate is increased, and the overall condensation process time is shortened. When the time interval of a single pressure lag time is greater than the preset time interval, it indicates that the pressure lag time is too long, which will also affect the yield of the reaction liquid. Therefore, the condensation rate of the condenser 501 is reduced.

[0114] This invention adjusts the working state of condenser 501 in real time by monitoring the time interval of pressure hysteresis to optimize condensation efficiency, thereby further optimizing the experimental process. It can more accurately determine the acid-rock reaction kinetic parameters, improve the accuracy of test data, and provide parameters and basis for acidification optimization design and acid system selection.

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

[0116] If the time interval of a single pressure lag time period is less than or equal to the preset time interval, the gas pressurization unit will not pressurize the reactor 4.

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

[0118] Understandably, if the time interval of a single pressure lag period is less than or equal to the preset time interval, it indicates that the pressure change inside reactor 4 has reached or is close to a constant pressure state (target pressure). At this time, the gas pressurization unit will not pressurize reactor 4. If the time interval of a single pressure lag period is greater than the preset time interval, it indicates that the current pressurization rate of the gas pressurization unit is too slow. To ensure that the acid-rock reaction proceeds at the target pressure, the pressurization rate of the gas pressurization unit is increased. By increasing the pressurization rate, the required target pressure can be reached more quickly. Preferably, the single increase in the pressurization rate is set to 10% to 30% of the original pressurization rate.

[0119] This invention achieves efficient control of the pressure inside reactor 4 by dynamically adjusting the pressurization rate of the gas pressurization unit based on the duration of the pressure lag time. This ensures that the acid-rock reaction can proceed efficiently under the target pressure, thereby further optimizing the experimental process, enabling more accurate determination of the acid-rock reaction kinetic parameters, improving the accuracy of test data, and providing parameters and basis for acidification optimization design and acid system selection. Example 1:

[0120] a. Attach the fixed rock sample to the rotating connecting rod and place it into reactor 4. Close the shut-off valve between preheating vessel 2 and reactor 4. Add 500 mL of acid solution to preheating vessel 2, set the test temperature, and control the heating rate, ensuring the heating rate does not exceed 5℃ / min. Heat preheating vessel 2, acid-rock reactor 4, and the rock sample. When the temperature is about to reach the set temperature, pressurize using the gas pressurization unit (control group), raising the pressure in reactor 4 to 7 MPa.

[0121] b. Same as step a, but after heating the preheating vessel 2, the acid-rock reaction vessel 4 and the rock sample, directly flow the acid into the reaction vessel 4 to carry out the acid-rock reaction (measurement group).

[0122] c. At several reaction time points, open the sampling valve 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 experimental data of the pressure lag time period, the reaction liquid sample of the control group, and the reaction liquid sample of the measurement group, further determine the acid-rock reaction kinetic parameters.

[0123] The technical solution of the present invention has been described above with reference to the preferred embodiments shown in the accompanying drawings. However, it will be readily understood by those skilled in the art that the scope of protection of the present invention is obviously not limited to these specific embodiments. Without departing from the principles 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 all fall within the scope of protection of the present invention.

Claims

1. A rapid experimental apparatus for determining acid-rock reactions, characterized in that, include: Acid storage tank, preheating kettle, gas pressurization unit, reaction kettle, 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 and transport the acid to the preheating kettle. The preheating kettle is used to preheat the acid. The gas pressurization unit is connected to the reactor to pressurize the reactor to the target pressure; The intelligent control collection unit includes a condenser, a rotary sampler connected to the condenser for collecting the reaction liquid, a sampling sensing module, and a sampling control module for determining whether sampling is complete. The condenser is connected to the outlet of the reaction vessel. The reaction liquid in the reaction vessel is condensed by the condenser and then enters the rotary sampler. The sampling sensing 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 several pressure lag time periods based on the pressure data collected in the reaction vessel at several time points and the amount of reaction liquid, and to determine the reaction cessation timing of the control group reaction liquid and the condensation rate of the condenser based on the pressure lag time periods. The sampling control module determines several pressure lag time periods, including... Pressure data and reaction liquid volume data in the control group reactor were collected at several time points, and a first pressure curve and a first reaction liquid production curve were generated. The pressure data and reaction liquid volume data in the reactor group were collected at several time points, and a second pressure curve and a second reaction liquid production curve were generated. Based on the first pressure curve and the second pressure curve, several pressure change time points are determined, and the time point corresponding to the pressure difference exceeding the preset pressure difference value is determined as the pressure change time point. Based on the first reaction liquid production curve and the second reaction liquid production curve, several response time points are determined, and the time point when the reaction liquid production difference is greater than the preset reaction liquid production difference is determined as the response time point. The timing for stopping the reaction includes: collecting the control group reaction solution at the end of the pressure hysteresis period; and stopping the collection of the control group reaction solution at the beginning of the pressure hysteresis period. The pressure lag time periods are determined based on the pressure abrupt change time points and the several response time points. The analysis unit, which is connected to the intelligent control collection unit, is used to 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 sample of the control group reaction liquid, and the test data of the reaction liquid sample of the measurement group reaction liquid. The control group consisted of the reactor undergoing acid-rock reaction under preset pressure conditions; the measurement group consisted of the reactor undergoing acid-rock reaction under pressure-holding conditions.

2. The experimental apparatus for rapid determination of acid-rock reaction according to claim 1, characterized in that, The rotary sampler is provided with several cleaning ports, which are used to automatically clean several test tubes on the rotary sampler.

3. The experimental apparatus for rapid determination of acid-rock reaction according to claim 2, characterized in that, The sampling control module determines several pressure change time points, including: The first pressure curve and the second pressure curve are normalized. At the same point in time, determine the pressure difference between the normalized first pressure curve and the second pressure curve; The pressure difference is compared with the preset pressure difference, and the pressure change time point is determined based on the comparison result.

4. The experimental apparatus for rapid determination of acid-rock reaction according to claim 3, characterized in that, The sampling control module determines several response time points, including: At the same time point, determine the difference in reaction liquid yield between the first reaction liquid yield curve and the second reaction liquid yield curve; The difference in the yield of the reaction solution is compared with the preset difference in the yield of the reaction solution, and the response time point is determined based on the comparison result.

5. The experimental apparatus for rapid determination of acid-rock reaction according to any one of claims 3 or 4, characterized in that, The sampling control module determines the pressure lag time periods based on the plurality of pressure abrupt change time points and the plurality of response time points, including: Match the aforementioned pressure mutation time points with the aforementioned 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.

6. The experimental apparatus for rapid determination of acid-rock reaction 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 time period, including: If the time interval of a single pressure hysteresis period is less than or equal to a preset time interval, the condenser condensation rate is increased. If the time interval of a single pressure hysteresis period is greater than the preset time interval, the condenser condensation rate is reduced.

7. The experimental apparatus for rapid determination of acid-rock reaction according to claim 6, characterized in that, The sampling control module determines the pressurization rate of the gas pressurization unit based on the duration of the pressure hysteresis time period, including: If the time interval of a single pressure lag time period is greater than the preset time interval, the pressurization rate of the gas pressurization unit is increased.

8. The experimental apparatus for rapid determination of acid-rock reaction according to claim 1, characterized in that, The interval between the specified time points ranges from 5 min to 10 min.

9. The experimental apparatus for rapid determination of acid-rock reaction according to claim 1, characterized in that, The target pressure ranges from 5 MPa to 10 MPa.

10. The experimental apparatus for rapid determination of acid-rock reaction according to claim 7, characterized in that, It also includes the option that if the time interval of a single pressure lag time period is less than or equal to a preset time interval, then there is no need to adjust the pressurization rate of the gas pressurization unit.

Citation Information

Patent Citations

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