Method and system for dynamically regulating and controlling sulfur form in pressure leaching process of copper sulfide slag
By using real-time monitoring and thermal shock intervention technology, the sulfur form in the pressure leaching process of copper sulfide slag is dynamically controlled, which solves the problem of dense sulfur film formation and improves the leaching efficiency of valuable metals as well as the stability and economy of the production process.
Patent Information
- Application Number
- CN202511946641.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-12-23
- Publication Date
- 2026-03-06
AI Technical Summary
During the pressure leaching process of copper sulfide slag, the generation and morphology control of elemental sulfur are difficult to effectively prevent the formation of a dense sulfur film, which leads to a decrease in the chemical reaction rate, affects the leaching efficiency of valuable metals, and increases energy consumption and cost.
By monitoring the turbidity and stratification potential of the reaction slurry in real time, the system identifies the initial passivation risk signals, generates thermal shock intervention commands, induces explosive nucleation to form a loose and porous sulfur layer, and performs macroscopic oxidation environment regulation in parallel to ensure the continuous driving force of the chemical reaction.
It enables early warning and timely intervention of passivation risks, reduces energy consumption, improves leaching efficiency and stability, reduces operational lag risks, and enhances the automation and intelligence level of the production process.
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Figure CN121610653A_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of hydrometallurgical technology and relates to a method and system for dynamic control of sulfur speciation during the pressure leaching of copper sulfide slag. Background Technology
[0002] A key technical challenge in the pressure leaching of copper sulfide slag lies in the formation and morphology control of elemental sulfur. Elemental sulfur generated during the leaching reaction easily crystallizes on the surface of unreacted slag particles, forming a dense physical film—a phenomenon known as passivation. This dense sulfur film isolates the leaching agent from the mineral particle core, causing a sharp decrease in the chemical reaction rate or even complete termination, ultimately severely impacting the leaching efficiency of valuable metals and resulting in waste of materials and energy. Effectively avoiding or eliminating this passivation film is a critical bottleneck in improving the economics of the entire hydrometallurgical process.
[0003] Currently, the industry commonly employs several traditional methods to address sulfur passivation. One method involves raising the operating temperature above the melting point of sulfur, causing the generated sulfur to exist in a liquid state, thus preventing the formation of a solid crystalline film. However, this method is extremely energy-intensive and places stringent demands on equipment. Another method involves adding chemical additives such as surfactants to alter the surface properties of sulfur, promoting its formation into a loose or hydrophilic morphology. However, this not only increases production costs but may also introduce impurities into subsequent solution purification and metal recovery processes, causing systemic problems. In addition, increasing the intensity of mechanical stirring is also a common approach, attempting to peel off the sulfur film through physical shear force. However, its effectiveness is limited, especially after the passivation layer has already formed. Simple mechanical energy is often insufficient to effectively break down the dense crystalline structure, and it consumes enormous amounts of energy.
[0004] The drawbacks of traditional methods are obvious. Whether it's ultra-high temperature leaching, adding chemical additives, or intensifying mechanical stirring, these methods are essentially passive or global intervention strategies, lacking the ability to perceive and precisely control the passivation process in real time. They often only take effect after passivation has already occurred or spread globally, making it difficult to prevent the formation of a dense sulfur film at its source. This results in high intervention costs, low efficiency, and significant side effects. These methods fail to achieve online, dynamic, and localized intervention in sulfur crystallization kinetics, lacking an intelligent solution that can precisely address passivation risks at their inception and collaboratively maintain the optimal chemical reaction environment. Summary of the Invention
[0005] In order to overcome the above-mentioned defects of the prior art and to achieve the above objectives, the present invention proposes the following technical solution: a method for dynamic control of sulfur form during the pressure leaching of copper sulfide slag, comprising: S1, collecting the turbidity value and stratification potential value of the reaction slurry, and generating a real-time state flow of dual parameters of the leaching process containing indirect physical form indicators and direct chemical environment indicators.
[0006] S2. Based on the real-time state flow of two parameters, the passivation risk bud signal is identified.
[0007] S3. In response to the initial signal of passivation risk, generate a thermal shock intervention command.
[0008] S4. Execute the thermal shock intervention command to induce explosive nucleation in a local area of the reactor, generating a loose and porous physical morphology.
[0009] S5. In parallel, macroscopic oxidation environment control parameters are generated based on the real-time state flow of two parameters.
[0010] S6. Implement macroscopic oxidation environment control parameters to conduct closed-loop feedback regulation of the main oxidant supply in order to maintain the continuous driving force of the metal leaching chemical reaction.
[0011] The second aspect of the present invention provides a dynamic control system for sulfur speciation during the pressure leaching of copper sulfide slag, comprising: a state flow acquisition module, which collects the turbidity value and stratification potential value of the reaction slurry, and generates a real-time state flow of two parameters of the leaching process, including indirect physical speciation indicators and direct chemical environment indicators.
[0012] The passivation risk identification module identifies the initial passivation risk signals based on a two-parameter real-time state flow.
[0013] The thermal shock intervention command generation module generates thermal shock intervention commands in response to the passivation risk bud signal.
[0014] The physical morphology intervention execution module executes the thermal shock intervention command, and generates a loose and porous physical morphology by inducing explosive nucleation in a local area of the reactor.
[0015] The macroscopic environmental parameter generation module generates macroscopic oxidation environment control parameters in parallel based on a two-parameter real-time state flow.
[0016] The chemical environment regulation module executes macroscopic oxidation environment control parameters and performs closed-loop feedback regulation of the main oxidant supply to maintain the continuous driving force of the metal leaching chemical reaction.
[0017] Compared with the prior art, the beneficial effects of the present invention are as follows: (1) By establishing a dual-parameter real-time monitoring system, the present invention can identify the signs of physical morphological changes caused by the ordered crystallization of elemental sulfur in advance, and realize early warning of passivation risk. It no longer relies on passive treatment after the passivation phenomenon occurs, but captures the physical budding signal before the irreversible dense sulfur film is formed, thereby advancing the intervention time to the initial stage of the problem, significantly improving the timeliness and effectiveness of intervention, and avoiding major losses caused by reaction stagnation.
[0018] (2) This invention introduces a physical field intervention method based on thermal shock, which fundamentally changes the crystallization mode of elemental sulfur by inducing explosive nucleation in local micro-regions within the reactor. Unlike traditional macroscopic and uniform intervention, this instantaneous and localized precise intervention can force the formation of a loose and porous sulfur layer, completely eliminating the physical basis for passivation. This direct control of crystallization kinetics is far more effective than traditional indirect methods such as mechanical stirring or chemical additives, achieving a solution to core technical problems with lower energy and material consumption.
[0019] (3) This invention combines instantaneous local intervention targeting the physical morphology with continuous overall regulation targeting the macroscopic chemical environment, forming a dual closed-loop protection mechanism. While addressing the risk of acute passivation through physical means, the system simultaneously adjusts key chemical parameters to ensure that the chemical driving force required for metal leaching is always maintained at an optimal level. This synergistic effect of physical and chemical regulation ensures that the leaching process maintains high stability and efficiency under any operating condition disturbance.
[0020] (4) By realizing the dynamic perception, accurate prediction and intelligent control of the key physicochemical states of the leaching process, this invention significantly improves the automation and intelligence level of the entire production process. It reduces the over-reliance on the experience of operators, reduces the risks caused by misjudgment and operational delays, and makes the entire leaching process more stable, efficient and economical, providing an effective technical approach for achieving refined management and maximizing benefits in hydrometallurgical processes. Attached Figure Description
[0021] To more clearly illustrate the technical solutions of the embodiments of the present invention, the accompanying drawings used in the description of the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.
[0022] Figure 1 This is a schematic diagram of the implementation steps of the method of the present invention.
[0023] Figure 2 This is a schematic diagram of the system module connections of the present invention. Detailed Implementation
[0024] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0025] Example 1: Please refer to Figure 1 As shown, the method for dynamically regulating sulfur forms during the pressure leaching of copper sulfide slag proposed by the present invention includes: S1. Collect the turbidity value and delamination potential value of the reaction slurry to generate a two-parameter real-time state stream of the leaching process that includes an indirect index of physical form and a direct index of chemical environment.
[0026] In a preferred embodiment, the step of collecting the turbidity value and delamination potential value of the reaction slurry to generate a two-parameter real-time state stream of the leaching process that includes an indirect index of physical form and a direct index of chemical environment includes: S1.1. Continuously collect the turbidity value of the reaction slurry through an on-line turbidimeter deployed on the external circulation pipeline of the leaching reactor.
[0027] S1.2. Synchronously collect the delamination potential value in the liquid phase of the reaction slurry through multiple redox potential sensors arranged vertically inside the leaching reactor.
[0028] S1.3. Combine the turbidity value and delamination potential value with time stamps aligned into a data sequence to generate a two-parameter real-time state stream.
[0029] Specifically, sensor deployment and data collection are carried out on a leaching reactor operating the pressure leaching process of copper sulfide slag. The leaching reactor is a closed container for chemical leaching reactions under high temperature and high pressure conditions, and its structure includes a reactor body and an external circulation pipeline for accommodating and circulating reaction materials.
[0030] The operation process is as follows: The first operation is to install an on-line turbidimeter on the external circulation pipeline supporting the leaching reactor. This on-line turbidimeter emits a beam of light with a specific wavelength through the reaction slurry flowing through the pipeline and measures the degree of light scattering by suspended particles, thereby continuously outputting a changing turbidity value in real time. This turbidity value is positively correlated with the concentration of suspended fine particles in the reaction slurry and, as an indirect index of physical form, reflects the dispersion and aggregation state of solid particles in the liquid phase. The indirect index of physical form refers to an index that indirectly infers the change trend of the target physical form (here, the crystal form of elemental sulfur) by measuring a physical quantity that is easy to monitor on-line (here, the turbidity value).
[0031] The on-line turbidimeter is a sensor device that can be installed on an industrial pipeline and continuously measure the turbidity of a fluid without sampling. Its core function is to emit a light source and detect the intensity of scattered light. The unit of the output turbidity value is usually NTU, and the setting is based on ensuring that its measurement range can cover the change range of particle concentration during the process from the initial dispersion of the reaction slurry to the formation of a sulfur film. Generally, a measurement range of 0 to 4000 NTU is selected.
[0032] The reaction slurry is a general term for the solid-liquid mixture in the leaching reactor, which includes unreacted copper sulfide slag, leaching solution, and solid products generated by the reaction.
[0033] The turbidity value is a physical quantity that characterizes the degree of turbidity of a liquid and is used to indirectly reflect the number and state of fine solid particles suspended in the reaction slurry.
[0034] The second operation involves installing three redox potential sensors inside the leaching reactor, along a vertical axis from top to bottom, at the upper, middle, and lower layers. These three sensors are set to synchronous acquisition mode, meaning they simultaneously measure the potential value of the reaction slurry liquid phase at their respective locations. These stratified potential values serve as direct indicators of the chemical environment, directly reflecting the driving force intensity and uniformity of the chemical reaction in different regions of the reactor. Direct indicators of the chemical environment refer to parameters that can directly measure and reflect the core characteristics of the chemical reaction environment (in this case, the redox atmosphere), namely, the stratified potential value.
[0035] The redox potential sensor is an electrochemical sensor that characterizes the relative strength of oxidizing or reducing properties of a reaction system by measuring the electrode potential. Its function is to provide a quantitative indicator of the driving force of the reaction, with the unit being millivolts (mV).
[0036] The layered potential value is a set of data collected synchronously by three redox potential sensors deployed in the upper, middle and lower layers of the reaction slurry liquid phase. It includes three independent potential readings to assess whether the chemical environment inside the reactor is evenly distributed in the vertical space.
[0037] Finally, continuous turbidity values from an online turbidimeter and stratified potential values from three redox potential sensors are aggregated through a data acquisition system. The system uses the time information (time stamp) inherent in each data point to align data from different sources. Specifically, using a common, high-frequency clock as a reference, a turbidity value and the three potential values (upper, middle, and lower) collected at each moment are combined into a single data unit. This data unit contains time information, turbidity information, and potential information at the three locations. These data units are continuously generated in chronological order, forming a two-parameter real-time state stream, providing the initial data foundation for subsequent analysis of the correlation between the chemical environment and physical state. The two-parameter real-time state stream is time-series, with each time point's data unit containing two different types of parameters: turbidity value and stratified potential value, used to dynamically describe the state of the reaction process.
[0038] For example, at a certain moment, the turbidity value of the reaction slurry collected by the online turbidimeter deployed on the external circulation pipeline is 850 NTU. Simultaneously, three redox potential sensors installed in the leaching reactor synchronously collect the stratification potential values in the liquid phase of the reaction slurry: upper layer 455 mV, middle layer 460 mV, and lower layer 458 mV. The data acquisition system adds the current timestamp, such as "time T," to these data and combines them into a data unit. This process continues at a frequency of once per second, and the continuously generated sequence of data units constitutes a two-parameter real-time state stream. At "time T+1 seconds," the newly generated data unit may contain a turbidity value of 845 NTU and stratification potential values of upper layer 456 mV, middle layer 461 mV, and lower layer 459 mV. This two-parameter real-time state stream completely records the dynamic changes of the turbidity value, an indirect indicator of physical morphology, and the stratification potential value, a direct indicator of the chemical environment.
[0039] S2. Based on the real-time state flow of two parameters, the passivation risk bud signal is identified.
[0040] In a preferred embodiment, the step of identifying passivation risk budding signals based on the two-parameter real-time state stream includes: S2.1, resolving a continuous turbidity value sequence from the two-parameter real-time state stream in real time.
[0041] S2.2 Calculate the rate of decrease of the turbidity value sequence over time.
[0042] S2.3. Compare the descent rate with the preset risk threshold rate. When the descent rate exceeds the risk threshold rate, generate a passivation risk bud signal.
[0043] In a further preferred embodiment, the preset risk threshold rate is dynamically adjusted according to the reaction stage of the leaching process, wherein the reaction stage includes the initial reaction stage and the middle and late reaction stages.
[0044] By introducing a risk threshold rate that varies with the reaction stage and combining it with monitoring the rate of turbidity decrease, the system can identify the nascent passivation risk signals at different reaction stages. This avoids misjudgments caused by drastic turbidity fluctuations due to material mixing in the early stages of the reaction, while also improving the detection sensitivity for the rapid sulfur film formation stage in the later stages of the reaction, ensuring the timeliness and necessity of physical intervention.
[0045] Specifically, upon receiving the two-parameter real-time state stream, the system activates a dedicated risk identification module. Its primary task is to extract a continuous sequence of turbidity values from the input two-parameter real-time state stream in real time. In practice, this risk identification module ignores the stratified potential values and only reads the turbidity value in each data unit in chronological order, forming a turbidity change curve that evolves over time.
[0046] The turbidity value sequence is a continuous data stream composed of single turbidity parameters extracted in chronological order from a two-parameter real-time state stream.
[0047] Next, the risk identification module uses a differential calculation method to analyze the turbidity value sequence, thereby obtaining its rate of decrease over time. The rate of decrease is a physical quantity that measures how quickly the turbidity value decreases over time, reflecting the speed at which suspended fine particles disappear from the reaction slurry or agglomerate and settle. For example, by calculating the difference between the turbidity value at the current moment and the value at the previous minute, and then dividing it by the time interval of one minute, a rate value representing the recent change in turbidity can be obtained.
[0048] Subsequently, the calculated turbidity decrease rate is compared in real time with a preset risk threshold rate. When the absolute value of the calculated actual turbidity decrease rate exceeds the risk threshold rate set for the current stage, the system determines that passivation risk is accumulating. This determination result is an internal logical state, signifying the confirmation of potential risk.
[0049] The risk threshold rate is a pre-set critical value used to determine whether the rate of turbidity decrease is abnormal, and it is dynamically adjusted according to the reaction stage. The setting is based on the analysis of a large amount of historical data at different leaching reaction stages. For example, in the early stage of the reaction, particle dissolution and breakage may cause turbidity fluctuations, at which time the risk threshold rate is set more leniently; while in the middle and later stages of the reaction, the turbidity should decrease slowly in a normal leaching process, at which time the risk threshold rate is set more strictly to capture any accelerated downward trend that indicates rapid sulfur layer encapsulation.
[0050] Finally, once the system determines that passivation risk is accumulating, it will immediately generate a clear signal indicating the nascent stage of passivation risk. This signal can be a digital flag or a specific data packet, serving as the trigger for subsequent intervention measures. Its core function is to capture early signs of physical morphology before the sulfur film forms a dense and irreversible structure.
[0051] For example, the system continuously receives a two-parameter real-time status stream. At "time T+60 seconds," the risk identification module parses and obtains the current turbidity value as 820 NTU. The module calculates the turbidity decrease rate over the past minute as (845 NTU - 820 NTU) / 1 minute, resulting in a decrease rate of 25 NTU / minute. Assuming the current stage is in the middle of the reaction, the system dynamically adjusts the risk threshold rate for this stage to 20 NTU / minute according to preset rules. Because the actual decrease rate of 25 NTU / minute exceeds the risk threshold rate of 20 NTU / minute, the system determines that passivation risk is accumulating. Based on this determination, the system immediately generates a high-level passivation risk budding signal and outputs it.
[0052] S3. In response to the initial signal of passivation risk, generate a thermal shock intervention command.
[0053] In a preferred embodiment, the step of generating a thermal shock intervention command in response to a passivation risk bud signal includes: S3.1, obtaining the signal strength by quantifying the specific difference between the rate of decrease of the turbidity value and the rate of decrease of the preset risk threshold; and obtaining the duration of the signal by quantifying the time elapsed from the start of the passivation risk bud signal to the current moment.
[0054] S3.2 Based on the signal strength and duration, match and determine a set of injection parameters in the preset intervention strategy library, including injection pressure, duration and number of applications.
[0055] S3.3 Encapsulate the injection parameters to generate thermal shock intervention commands.
[0056] Specifically, a dedicated instruction generation module continuously monitors the status of passivation risk budding signals. Upon receiving a passivation risk budding signal generated in the previous steps, this module is immediately activated, using the received signal as the trigger condition for subsequent operations. The instruction generation module then analyzes two key attributes of the passivation risk budding signal: signal strength and duration. Signal strength is quantified as the difference between the actual turbidity decrease rate and the risk threshold rate; a larger difference indicates faster risk accumulation and higher strength. Signal duration refers to the length of time elapsed from the signal's generation to the current moment.
[0057] Then, the instruction generation module accesses an internally stored library of preset intervention strategies. This library contains multiple intervention plans for different risk levels. Each plan specifies a set of thermal shock parameters, including injection pressure, duration, and number of applications. These parameters are based on extensive experimental data and operational experience, aiming to provide the optimal physical intervention plan for different levels of passivation risk. The system will then search the preset intervention strategy library based on the intensity and duration of the currently analyzed passivation risk budding signal, selecting the most suitable intervention strategy for the current risk situation.
[0058] The injection pressure refers to the ejection pressure of the cryogenic fluid during thermal shock, which determines the fluid's penetration power and range of influence.
[0059] The duration refers to the time from the start to the end of a single injection action, which controls the total energy input of a single intervention.
[0060] The number of actions refers to the number of times the spraying action needs to be performed in a complete intervention event, in order to deal with more stubborn or continuously accumulating passivation risks.
[0061] Finally, the system extracts the specific values of injection pressure, duration and number of applications from the selected strategy, and packages these parameters into a standard format data instruction. This instruction is the final generated thermal shock intervention instruction, which is used to issue operation commands to downstream execution equipment.
[0062] For example, the system generates a high-level passivation risk budding signal. Upon receiving this signal, the instruction generation module starts timing and analyzes its intensity. Assume the turbidity value decreases at a rate of 25 NTU / min, exceeding the risk threshold rate of 20 NTU / min (a total of 5 NTU / min); this represents the signal intensity. If the signal lasts for 90 seconds, the system uses "intensity 5 NTU / min, duration 90 seconds" as the query condition and matches it against a preset intervention strategy library. The found strategy is a moderate-intensity intervention, with parameters: injection pressure set to 2.5 MPa, duration set to 1.5 seconds, and number of applications set to 1. The system then extracts these parameters, encapsulates them to generate a thermal shock intervention instruction, with the instruction content being {injection pressure: 2.5, duration: 1.5, number of applications: 1}.
[0063] S4. Execute the thermal shock intervention command to induce explosive nucleation in a local area of the reactor, generating a loose and porous physical morphology.
[0064] In a preferred embodiment, the execution of the thermal shock intervention command, which induces explosive nucleation in a local area of the reactor to generate a loose and porous physical morphology, includes: S4.1, driving an instantaneous injection device connected to the lower part of the reactor.
[0065] S4.2. Using an instantaneous injection device, a low-temperature fluid with a temperature difference exceeding the specified temperature of the main body inside the reactor is injected into the reaction slurry to form an instantaneous local low-temperature zone around the nozzle.
[0066] S4.3. By utilizing the thermal shock caused by the instantaneous local low temperature zone, the dissolved sulfur is forced to form a large number of disordered sulfur crystal nuclei in an explosive nucleation manner, generating a loose and porous physical form.
[0067] Specifically, upon receiving the packaged thermal shock intervention command, the physical execution system immediately parses the command to obtain specific parameters such as injection pressure, duration, and number of applications. Based on these parameters, the system drives one or more instantaneous injection devices installed in the lower part of the leaching reactor to begin performing the physical intervention. The core component of these instantaneous injection devices is a high-speed switching valve, which can precisely control the start and stop of the injection action. Its core function is to create instantaneous, localized drastic changes in operating conditions, enabling the fluid to be injected into the reactor at high speed in a very short time.
[0068] Upon execution of the command, the instantaneous injection device rapidly opens the valve within milliseconds, forcefully injecting a pre-prepared cryogenic fluid—significantly colder than the main reactor fluid—into the high-temperature, high-pressure reaction slurry at the set injection pressure and duration. The cryogenic fluid is a fluid with a significantly lower temperature compared to the nearly 200°C working medium inside the reactor; it is typically ambient temperature process water or cooling water, serving as a medium for generating thermal shock. The injection of the cryogenic fluid creates a momentary, localized cryogenic zone within a very small area around the nozzle.
[0069] The significant temperature difference between the low-temperature fluid and the main body temperature of the reaction slurry refers to a huge difference between the temperature of the low-temperature fluid and the main body temperature of the reaction slurry, for example, a temperature difference exceeding 150 degrees Celsius, which is a prerequisite for generating effective thermal shock.
[0070] The instantaneous local low-temperature zone is a low-temperature region that forms near the nozzle at the instant the low-temperature fluid is injected, with a spatial range of extremely small size (micrometer to millimeter level) and an existence time of extremely short duration (millisecond level).
[0071] Within the instantaneous localized low-temperature zone, the temperature drops abruptly from the main temperature inside the vessel (e.g., 180 degrees Celsius) to near the temperature of the cryogenic fluid (e.g., 25 degrees Celsius). This dramatic temperature jump constitutes a strong thermal shock. Elemental sulfur, which normally exists in a dissolved state at high temperatures, experiences a sharp decrease in solubility within this instantaneous localized low-temperature zone, reaching an extremely high supersaturation. This extreme supersaturation prevents the dissolved sulfur from undergoing orderly molecular arrangement and slow crystal growth. Instead, it is forced to instantly overcome the energy barrier required for crystallization, simultaneously forming a massive number of tiny, disordered sulfur crystal nuclei within the micro-region through explosive nucleation.
[0072] The explosive nucleation is a crystallization method under extremely high supersaturation conditions where the nucleus generation rate is much greater than the crystal growth rate, characterized by the instantaneous generation of a large number of tiny nuclei.
[0073] The sulfur crystal nuclei that form rapidly aggregate, but due to the disorder of the formation process, they cannot form a dense crystalline layer. Instead, they form a loose and porous physical form that adheres to the surface of the slag particles. This form does not hinder the contact between the leachate and the slag, thus avoiding passivation.
[0074] The loose and porous physical morphology refers to a solid layer of elemental sulfur generated through explosive nucleation. Its internal structure is not dense, containing numerous pores and channels, which is completely different in physical structure from the dense sulfur film formed through ordered crystallization. This precise intervention in crystallization kinetics ensures that the generated elemental sulfur layer has high permeability, fundamentally solving the passivation problem. Its effect far exceeds that of traditional methods such as simple cooling or mechanical stirring.
[0075] For example, after receiving a thermal shock intervention command with the content {injection pressure: 2.5, duration: 1.5, number of applications: 1}, the system drives the instantaneous injection device located in the lower part of the reactor to perform one injection. This instantaneous injection device injects 25°C process water into the 180°C reaction slurry at a pressure of 2.5 MPa for 1.5 seconds. Near the nozzle, a sudden, localized low-temperature zone is formed. Within this zone, dissolved sulfur rapidly reaches extremely high supersaturation, followed by explosive nucleation, generating a large number of disordered sulfur crystal nuclei. These nuclei aggregate and form a loose, porous physical layer on the surface of the slag particles, effectively preventing subsequent passivation.
[0076] S5. In parallel, macroscopic oxidation environment control parameters are generated based on the real-time state flow of two parameters.
[0077] In a preferred embodiment, the step of generating macroscopic oxidation environment control parameters based on the two-parameter real-time state flow includes: S5.1, extracting the layered potential values from the two-parameter real-time state flow and calculating their average potential values.
[0078] S5.2 Compare the average potential value with the preset target leaching potential value and calculate the deviation between the two.
[0079] S5.3. The proportional-integral-derivative control algorithm is adopted. Based on the deviation, the historical accumulation of the deviation and the trend of change, macroscopic oxidation environment regulation parameters are generated. The comprehensive control effect of this algorithm is combined with closed-loop feedback regulation to ensure that the overall chemical environment can be maintained in the optimal state quickly and stably while performing physical intervention, thus realizing the synergistic effect of physical regulation and chemical regulation.
[0080] The closed-loop feedback regulation is an automatic control method that compares the average value of the actual output potential of the system with the target leaching potential value of the desired output, and uses the deviation between the two to adjust the oxidant flow rate input to the system, forming a closed control loop to achieve precise output control.
[0081] Specifically, while performing the aforementioned physical interventions, a separate chemical environment control module operates in parallel. This module also continuously receives the two-parameter real-time state stream generated in the first step, but it focuses on the direct indicators of the chemical environment. The primary operation is to extract the upper, middle, and lower layer redox potential values from each data unit. Next, the chemical environment control module performs an arithmetic average of these three potential values to calculate an average value that represents the overall macroscopic chemical reaction environment intensity of the entire reactor. For example, adding the upper layer (455mV), middle layer (460mV), and lower layer (458mV) and dividing by 3 yields an average potential value.
[0082] The system then compares this real-time calculated average potential with a pre-set target leaching potential. This target leaching potential is an optimal redox potential reference point pre-set based on the specific mineral leaching kinetics. It is set according to the center value of the potential range determined through small-scale and pilot-scale laboratory experiments, achieving the highest metal leaching rate while maintaining reasonable economic costs; for example, it might be set at 460mV. Through comparison, the system calculates the deviation between the actual value and the target value. This deviation reflects the degree and direction of deviation between the current chemical environment and the ideal state.
[0083] Finally, based on this deviation value, the system employs a proportional-integral-derivative (PID) control algorithm. This algorithm comprehensively considers the magnitude of the current deviation (proportional action), the accumulation of historical deviations (integral action), and the trend of deviation changes (derivative action), calculating a precise adjustment amount through a pre-defined mathematical logic. This adjustment amount is the final macroscopic oxidation environment control parameter, which will be used to precisely adjust the supply rate of the main oxidant to maintain efficient metal leaching.
[0084] The proportional-integral-derivative (PID) control algorithm is a classic closed-loop control strategy. By combining proportional, integral, and derivative control actions, it can rapidly, accurately, and stably regulate the controlled process. The formula for calculating the macroscopic oxidation environment control parameters is: In the formula, This represents the macroscopic oxidation environment control parameter generated at time t. Its unit can be the opening percentage of the control valve or the flow regulation signal. It is a specific control signal value, and its function is to guide the oxidant supply module on how to adjust its output flow. This represents the deviation between the average potential value at time t and the target leaching potential value, i.e. ; It is a proportional coefficient used to adjust the intensity of the control action. It is set based on the system response speed and stability requirements and is tuned through control engineering methods such as step response testing. It is the integral coefficient, used to eliminate the steady-state error of the system. The setting basis is also obtained through system tuning, and it aims to balance the speed of eliminating steady-state error and avoid system oscillation. These are differential coefficients used to predict the trend of deviation changes and intervene in advance to improve system stability. The basis for setting them is to suppress overshoot and oscillation through tuning.
[0085] For example, the system extracts the layered redox potential values at a certain moment from the two-parameter real-time state stream: 455mV for the upper layer, 460mV for the middle layer, and 458mV for the lower layer. The calculated average potential is (455+460+458) / 3≈457.7mV. Assuming the target leaching potential is set to 460mV, the current deviation... The value is 460mV - 457.7mV = 2.3mV. The proportional-integral-derivative (PID) control algorithm calculates a specific output value based on this deviation, the previous deviation history and rate of change, and the set control coefficients (e.g., Kp = 0.5, Ki = 0.1, Kd = 0.05). This output value is the macroscopic oxidation environment control parameter. For example, the calculation result indicates that the macroscopic oxidation environment control parameter should increase the flow rate by 2%.
[0086] S6. Implement macroscopic oxidation environment control parameters to conduct closed-loop feedback regulation of the main oxidant supply in order to maintain the continuous driving force of the metal leaching chemical reaction.
[0087] In a preferred embodiment, the step of executing macroscopic oxidation environment control parameters to perform closed-loop feedback regulation of the main oxidant supply in order to maintain the continuous driving force of the metal leaching chemical reaction includes: S6.1, loading the macroscopic oxidation environment control parameters into the controller of the main oxidant supply module.
[0088] S6.2 The controller adjusts the flow rate of the oxidant delivered to the reactor in real time according to the macro-oxidation environment control parameters. By using the average potential of the overall chemical environment in the reactor as feedback, the closed-loop feedback regulation of the oxidant flow rate is achieved, ensuring the stability of the macro-oxidation environment and creating a continuous and effective basic chemical condition for physical intervention. The two work together to ensure leaching efficiency.
[0089] Specifically, after receiving the macroscopic oxidation environment control parameters generated by the proportional-integral-derivative control algorithm, the controller of the main oxidant supply module immediately executes the adjustment action. First, these macroscopic oxidation environment control parameters are loaded into the controller's memory as explicit digital instructions.
[0090] The main oxidant supply module is a complete system responsible for supplying oxidant into the leaching reactor, and typically includes a gas source, pipelines, flow meters, regulating valves, and a controller.
[0091] The oxidant is a substance that gains electrons in a chemical reaction. In this process, it usually refers to oxygen or oxygen-enriched air, and its role is to provide the necessary oxidizing environment to decompose sulfide minerals.
[0092] The controller is a programmable electronic device with built-in logic that interprets the parameter and translates it into physical actions. It is responsible for receiving external instructions and controlling the execution elements within the module.
[0093] Subsequently, based on the applied macroscopic oxidation environment control parameters, the controller adjusts in real time the actuators connected to the main oxidant supply pipeline, typically a flow control valve or a metering pump driver. For example, if the macroscopic oxidation environment control parameters indicate a need for a 2% increase in flow rate, the controller sends a signal to the control valve to increase its opening by the corresponding percentage, or to increase the stroke frequency of the metering pump. Flow rate refers to the volume or mass of oxidant flowing through the pipeline per unit time and is a direct indicator of the oxidant supply rate.
[0094] In this way, the actual flow rate of the oxidant delivered to the leaching reactor is precisely altered. This adjustment process is a continuous closed-loop feedback; the system constantly collects potential values, calculates deviations, generates control parameters, and executes adjustments. This ensures that the overall redox potential within the reactor fluctuates within a small range around the set target leaching potential, remaining consistently stable. This stable, strongly oxidizing environment provides sufficient and continuous chemical reaction driving force for the decomposition of metal sulfides and the dissolution of metal ions in the copper sulfide slag, guaranteeing the high efficiency of the entire leaching process.
[0095] The driving force of the chemical reaction here specifically refers to the redox potential difference necessary to maintain the metal leaching reaction. A stable and sufficiently high potential is the core condition to ensure that the chemical reaction can continue in the desired direction.
[0096] For example, when the controller of the main oxidant supply module receives a macroscopic oxidation environment control parameter indicating a 2% increase in flow rate, the controller immediately sends an additional opening signal to the electrically operated regulating valve connected to the main oxidant pipeline. Assuming the regulating valve is currently open at 50%, upon receiving the signal, its opening is precisely adjusted to 52%, resulting in an increase in the flow rate of pure oxygen supplied to the reactor from 10.0 cubic meters per minute to 10.2 cubic meters per minute. The increased oxygen entering the reaction slurry raises the overall redox potential within the reactor. In the next detection, the average potential may rise to 459.5 mV, closer to the target leaching potential of 460 mV. Through this closed-loop feedback regulation, the system continuously stabilizes the overall redox potential within the reactor near the target leaching potential, thereby ensuring a continuous driving force for the metal leaching chemical reaction.
[0097] In a further preferred embodiment, steps S4 and S5 are executed in parallel: the physical intervention on passivation risk in step S4 and the feedback adjustment of the macroscopic oxidation environment in step S5 are executed in parallel, forming a dual protection mechanism.
[0098] The dual protection mechanism combines instantaneous, localized intervention for acute physical problems with continuous, holistic regulation for chronic chemical environments to ensure that while the physical morphology is corrected in a timely manner, the overall driving force of the chemical reaction is always maintained at the optimal level, thereby achieving a significant improvement in the overall efficiency and stability of the leaching process.
[0099] Example 2: Please refer to Figure 2 As shown, based on Embodiment 1, the second aspect of the present invention provides a dynamic control system for sulfur speciation during the pressure leaching of copper sulfide slag, comprising: a state flow acquisition module, a passivation risk identification module, a thermal shock intervention command generation module, a sulfur speciation intervention execution module, a macroscopic environmental parameter generation module, and a chemical environment adjustment execution module.
[0100] The state flow acquisition module is connected to the passivation risk identification module and the macroscopic environmental parameter generation module, respectively. The passivation risk identification module is connected to the thermal shock intervention command generation module. The thermal shock intervention command generation module is connected to the physical morphology intervention execution module. The macroscopic environmental parameter generation module is connected to the chemical environment regulation execution module.
[0101] The state flow acquisition module collects the turbidity value and stratification potential value of the reaction slurry, and generates a real-time state flow of the leaching process with two parameters, including indirect physical morphology indicators and direct chemical environment indicators.
[0102] The passivation risk identification module identifies passivation risk budding signals based on a two-parameter real-time state flow.
[0103] The thermal shock intervention command generation module generates a thermal shock intervention command in response to a passivation risk budding signal.
[0104] The physical morphology intervention execution module executes the thermal shock intervention command, and generates a loose and porous physical morphology by inducing explosive nucleation in a local area of the reactor.
[0105] The macroscopic environmental parameter generation module generates macroscopic oxidation environment control parameters in parallel based on a dual-parameter real-time state flow.
[0106] The chemical environment regulation execution module executes macroscopic oxidation environment control parameters and performs closed-loop feedback regulation of the main oxidant supply to maintain the continuous driving force of the metal leaching chemical reaction.
[0107] It should be noted that the formulas described above, through the principle of dimensional consistency and mathematical standardization methods (such as normalization, dimensionless parameter conversion, or unit system unification), can translate physical quantities with different properties into unitless standard values or superimposed parameters of the same dimension. This eliminates the interference of different dimensions on the computational logic, allowing the formulas to retain the original data distribution characteristics while possessing mathematical rationality and adaptability to objective laws. The descriptions are merely exemplary embodiments of the present invention and should not be construed as limiting the scope of the invention.
Claims
1. A method for dynamic regulation of sulfur form in the pressure leaching process of copper sulfide residue, characterized in that, The method comprises the following steps: S1, collecting the turbidity value and the stratification potential value of the reaction slurry, and generating a double-parameter real-time state stream of the leaching process containing indirect indicators of physical morphology and direct indicators of chemical environment; S2, identifying the passivation risk germination signal based on the double-parameter real-time state stream; S3, generating a thermal shock intervention instruction in response to the passivation risk germination signal; S4, executing the thermal shock intervention instruction to generate a loose and porous physical morphology by inducing explosive nucleation in a local area of the reaction kettle; S5, in parallel, generating macroscopic oxidation environment regulation parameters based on the double-parameter real-time state stream; S6, executing the macroscopic oxidation environment regulation parameters to perform closed-loop feedback regulation on the supply of the main oxidation agent to maintain the continuous driving force of the metal leaching chemical reaction.
2. The method according to claim 1, wherein the method is characterized in that, The method for collecting the turbidity value and the stratification potential value of the reaction slurry, and generating a double-parameter real-time state stream of the leaching process containing indirect indicators of physical morphology and direct indicators of chemical environment comprises the following steps: S1.1, continuously collecting the turbidity value of the reaction slurry through an online turbidity meter deployed on the external circulation pipeline of the leaching reaction kettle; S1.2, synchronously collecting the stratification potential value in the liquid phase of the reaction slurry through multiple oxidation-reduction potential sensors arranged in the vertical direction inside the leaching reaction kettle; S1.3, combining the time-stamped turbidity value and the stratification potential value into a data sequence to generate the double-parameter real-time state stream.
3. The method according to claim 1, wherein the method is characterized in that, The method for identifying the passivation risk germination signal based on the double-parameter real-time state stream comprises the following steps: S2.1, real-time analyzing the continuous turbidity value sequence from the double-parameter real-time state stream; S2.2, calculating the descending rate of the turbidity value sequence over time; 4. The method according to claim 3, wherein the method is characterized in that, S2.3, comparing the descending rate with a preset risk threshold rate, and generating the passivation risk germination signal when the descending rate exceeds the risk threshold rate. The preset risk threshold rate is dynamically adjusted according to the reaction stage of the leaching process, wherein the reaction stage includes the initial reaction stage and the middle and late reaction stage; 5. The method according to claim 3, wherein the method is characterized in that, By introducing the risk threshold rate varying with the reaction stage and combining the monitoring of the descending rate of the turbidity value, the passivation risk germination signal in different reaction stages is identified. The method for generating a thermal shock intervention instruction in response to the passivation risk germination signal comprises the following steps: S3.1, obtaining the intensity of the signal by quantifying the specific difference between the descending rate of the turbidity value and the preset risk threshold rate, and obtaining the duration of the signal by quantifying the time length elapsed since the generation of the passivation risk germination signal to the current time; 6. The method according to claim 1, wherein the method is characterized in that, S3.2, matching and determining a set of jet parameters, including jet pressure, duration and action times, in a preset intervention strategy library according to the intensity and duration of the signal; S3.3, encapsulating the jet parameters to generate the thermal shock intervention instruction. The method for executing the thermal shock intervention instruction to generate a loose and porous physical morphology by inducing explosive nucleation in a local area of the reaction kettle comprises the following steps: S4.1, driving a transient jet device connected to the lower part of the reaction kettle; S4.2, jetting a low-temperature fluid with a temperature difference exceeding a specified temperature difference from the main body temperature in the kettle into the reaction slurry through the transient jet device to form a transient local low-temperature zone around the nozzle. S4.3, the thermal shock caused by the transient local low temperature area forces the dissolved sulfur to form a large number of disordered sulfur nuclei in an explosive nucleation manner, generating a loose and porous physical form.
7. The method according to claim 1, wherein the method is characterized in that, The macro-oxidation environment regulation parameter based on the double-parameter real-time state flow includes: S5.1, extracting the hierarchical potential value from the double-parameter real-time state flow and calculating the potential average value; S5.2, comparing the potential average value with the preset target leaching potential value, and calculating the deviation therebetween; S5.3, adopting a proportional-integral-derivative control algorithm, generating a macro-oxidation environment regulation parameter based on the deviation, the historical accumulation of the deviation, and the change trend.
8. The method according to claim 7, wherein the method is characterized in that, The execution of the macro-oxidation environment regulation parameter includes: S6.1, loading the macro-oxidation environment regulation parameter to the controller of the main oxidation agent supply module; S6.2, the controller adjusts the oxidation agent flow rate delivered into the reactor in real time according to the macro-oxidation environment regulation parameter; and the closed-loop feedback regulation of the oxidation agent flow rate is realized by taking the potential average value reflecting the overall chemical environment in the reactor as feedback.
9. The method according to claim 1, wherein the method is characterized in that, The execution mode of steps S4 and S5: the physical form intervention of the passivation risk in step S4 and the feedback regulation of the macro-oxidation environment in step S5 are executed in parallel, constituting a double protection mechanism.
10. A system for dynamic control of sulfur form in the pressure leaching process of copper sulfide residues, characterized by, The state flow acquisition module collects the turbidity value and the hierarchical potential value of the reaction slurry, and generates a double-parameter real-time state flow of the leaching process containing indirect indicators of physical form and direct indicators of chemical environment; The passivation risk identification module identifies the passivation risk germination signal based on the double-parameter real-time state flow; The thermal shock intervention instruction generation module generates a thermal shock intervention instruction in response to the passivation risk germination signal; The physical form intervention execution module executes the thermal shock intervention instruction to generate a loose and porous physical form by inducing explosive nucleation in the local area of the reactor; The macro-environment parameter generation module, in parallel, generates a macro-oxidation environment regulation parameter based on the double-parameter real-time state flow; The chemical environment regulation execution module executes the macro-oxidation environment regulation parameter to perform closed-loop feedback regulation on the supply of the main oxidation agent, so as to maintain the sustained driving force of the metal leaching chemical reaction.