Production control method for preparing high-purity copper sulfate based on etching waste liquid

CN122652929BActive Publication Date: 2026-10-09广东中耀环境科技有限公司
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Patent Information

Application Number
CN202611152075.0
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2026-07-31
Publication Date
2026-10-09
Estimated Expiration
2046-07-31

AI Technical Summary

Technical Problem

[0006]有鉴于此,本发明实施例提供了基于蚀刻废液制备高纯度硫酸铜的生产控制方法,用以解决现有技术中硫酸铜产品纯度和品质稳定性差的问题

Benefits of technology

本发明实施例提供的基于蚀刻废液制备高纯度硫酸铜的生产控制方法,实现了硫酸铜产品质量稳定可控,硫酸铜纯度稳定在99.9%以上,杂质含量≤5ppm,高纯品批次占比可达98%以上。全流程自动化显著提升生产效率,单批次生产周期缩短至10~12小时,相较传统工艺缩短约20%,劳动强度降低约60%。安全性和连续性得到增强,分段式酸化及管道双监控设计可防止反应失控及设备故障,生产故障率降低约80%,连续运行时间可达72小时以上。全过程数据实时存档,支持产品质量追溯,满足高端电镀及电子材料行业对供应链透明度的要求,同时辅料投加精准化和自动化控制减少资源浪费,实现节水约15%、节电约20%的节能效果,从而显著提升工艺稳定性、安全性及经济性。

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Abstract

The application discloses a production control method for preparing high-purity copper sulfate based on etching waste liquid, and relates to the technical field of waste liquid treatment. The method realizes automatic control of the whole process by introducing a distributed control module into each process link of pretreatment, neutralization, ammonia conversion, beating, acidification, filtration and crystallization of the etching waste liquid, realizes real-time collection, dynamic adjustment and data storage of process control parameters, thereby effectively reducing impurity content fluctuation, improving product purity stability, stabilizing copper sulfate purity at more than 99.9%, and enabling high-purity product batch ratio to reach more than 98%. Meanwhile, the whole-process automation significantly improves production efficiency, greatly shortens the production cycle of a single batch, and enhances safety and continuity. Meanwhile, accurate and automatic control of auxiliary material addition reduces resource waste, and the energy-saving effect is remarkable.
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Description

Technical Field

[0001] This invention relates to the field of waste liquid treatment technology, and in particular to a production control method for preparing high-purity copper sulfate based on etching waste liquid. Background Technology

[0002] In the existing industrial production process of electroplating-grade copper sulfate, etching waste liquid is usually used as copper-containing raw material. The process involves pretreatment, neutralization, ammonia conversion, pulping, acidification, filtration, crystallization, centrifugation, and drying to achieve copper resource recovery. While this process is relatively mature, the concentration of copper ions, impurity content, pH, and Baumé degree vary among different sources and batches of etching waste liquid. Current production processes still heavily rely on operators' experience to adjust auxiliary material dosages, material ratios, stirring times, and reaction temperatures, which can easily lead to fluctuations in reaction conditions between different batches, affecting the purity and crystal quality of the copper sulfate product.

[0003] To improve the automation level of copper sulfate preparation from waste etching solution, patent CN117383739B, entitled "An Apparatus and Method for Preparing Copper Sulfate from Waste Etching Solution," discloses an integrated and automated device that integrates multiple processing steps, including filtration, heating and concentration, quantitative acid addition, stirring reaction, precipitation separation, and drying. This technical solution reduces manual handling and feeding operations through appropriate conveying mechanisms, reaction devices, and control structures, thereby improving the continuity of the single preparation process and the degree of equipment integration.

[0004] However, the aforementioned technical solutions primarily focus on the structural combination of various processing devices, quantitative material delivery, and automatic operation under preset processes. Their control methods are typically based on pre-set feed amounts, operating times, or process sequences. Further improvements are needed to address the variations in the state of raw materials in different batches during industrial production, as well as the parameter transfer, dynamic adjustment, and operational coordination between processes such as pretreatment, neutralization, ammonia conversion, filtration, pulping, acidification, hot filtration, and crystallization. For example, while existing automatic feeding devices can add auxiliary materials according to set amounts, the preset feed amount may not match the current raw material state when the copper ion concentration, impurity content, or pH of the etching waste liquid changes. Existing systems typically cannot automatically correct the auxiliary material feed amount, material ratio, and reaction time of subsequent processes based on the detection results of preceding processes. They also struggle to continuously adjust the feeding process based on real-time changes in temperature, pH, Baumé degree, or material weight during the reaction process, relying more on fixed set values ​​for feeding and failing to achieve adaptive feeding based on the actual state of the materials.

[0005] Furthermore, each process typically operates with separate equipment or control units, meaning that the testing and operational data generated in the previous process are not effectively transferred to the next. For example, the copper content, impurity status, and actual consumption of auxiliary materials determined in the neutralization process may not be directly used to calculate the ammonia-containing material requirements for the ammonia-to-chemicals process; the filter cake weight obtained in the filtration process may not be sufficient to determine the pulping water consumption based on the filter cake liquid content; and the actual pulp concentration formed during pulping may not be directly sufficient to determine the total amount and dosage rate of sulfuric acid required for acidification. Due to the lack of a unified parameter correlation model between processes, production personnel still need to resample, recalculate, or adjust based on experience when switching processes, limiting further improvements in the automation level of the entire production line. Simultaneously, raw material testing data, auxiliary material dosage records, equipment operating parameters, process testing results, and finished product quality data in the existing production process are usually recorded separately by different positions or different equipment, with inconsistent data formats and recording methods. Some data is still stored in manually filled-out paper records or separate electronic spreadsheets. There is a lack of unified batch identification and correspondence between raw material information, production process parameters, and finished product testing results from different batches. When finished products have quality problems such as unqualified purity, high impurity content, abnormal crystal size, or high moisture content, it is difficult to quickly determine whether the abnormality is caused by raw material fluctuations, auxiliary material addition deviations, abnormal reaction temperature, decreased filtration efficiency, or unreasonable crystallization parameters. This results in low efficiency in tracing quality abnormalities, which is not conducive to quality abnormality tracing and continuous process optimization. Summary of the Invention

[0006] In view of this, embodiments of the present invention provide a production control method for preparing high-purity copper sulfate based on etching waste liquid, in order to solve the problem of poor purity and quality stability of copper sulfate products in the prior art.

[0007] This invention provides a production control method for preparing high-purity copper sulfate based on etching waste liquid, the method comprising: The etching waste liquid is transported to the pretreatment tank. The transmitter module of the pretreatment tank is controlled to obtain the first state parameter of the etching waste liquid. The distributed control module is driven to calculate and control the amount of auxiliary material added according to the first state parameter of the etching waste liquid until the etching waste liquid reaches the preset treatment state and then the addition of auxiliary material is stopped. The pretreated material is conveyed to the neutralization tank through a conveying device. The transmitter module of the neutralization tank collects the second state parameters of the material in the neutralization tank in real time. The distributed control module is driven to control the feed rate and stirring state of the alkaline etching waste liquid according to the second state parameters. After the reaction system reaches the preset reaction state, the alkaline copper pressure filter is controlled to filter and obtain alkaline copper filter cake. The alkali copper filter cake is transported to the ammonia transfer tank. The weighing module of the ammonia transfer tank is controlled to obtain the first weight parameter of the alkali copper filter cake. The distributed control module is driven to control the amount of ammonia water added and the stirring time according to the first weight parameter. After the ammonia transfer reaction is completed, the copper hydroxide filter press is controlled to perform a second filter press to obtain the copper hydroxide filter cake. The copper hydroxide filter cake is conveyed to the pulping tank. The second weight parameter of the copper hydroxide filter cake is obtained by the weighing module of the pulping tank. The distributed control module is driven to control the amount of water or copper sulfate mother liquor added and the stirring time according to the second weight parameter, so that the solid material forms a slurry. The slurry is transported to the acidification tank. The feeding speed and amount of the slurry and acidic materials are controlled by the distributed control module. The third state parameters of the reactants are acquired in real time by the transmitter module of the acidification tank. The acidification reaction is judged to be completed based on the third state parameters. The acidified filtrate is obtained by filtering the material after the acidification reaction through a hot filtration pipe. The acidified filtrate is transported to a crystallization tank, and the cooling rate and crystallization time are controlled by the distributed control module. After crystallization, the product is centrifuged and dried to obtain copper sulfate.

[0008] Preferably, before the etching waste liquid is transported to the pretreatment tank, the method further includes: registering the source and detecting the components of the etching waste liquid, and inputting the source registration data and component detection data into the distributed control module.

[0009] Preferably, the step of conveying the etching waste liquid to the pretreatment tank, controlling the transmitter module of the pretreatment tank to acquire the first state parameter of the etching waste liquid, and driving the distributed control module to calculate and control the amount of auxiliary material added based on the first state parameter of the etching waste liquid, until the etching waste liquid reaches the preset treatment state and the addition of auxiliary material is stopped, includes: After the etching waste liquid is transported to the pretreatment tank, the first state parameter of the etching waste liquid is collected in real time through the transmitter module of the pretreatment tank. The first state parameter includes at least one or more of the following: metal ion concentration parameter, Baumé parameter and pH parameter. The first state parameter is input into the distributed control module, which then obtains the target dosage of the auxiliary material based on a preset dosage determination rule; wherein the auxiliary material includes phosphoric acid and ammonia. The auxiliary material dosing device is controlled to add phosphoric acid and ammonia water into the pretreatment tank according to the target dosing amount, and the actuator is controlled to adjust the valve opening to achieve dynamic dosing; During the dosing process, the transmitter module continuously collects and updates the first status parameter in real time, and the distributed control module dynamically corrects the target dosing amount based on the real-time collection and update results. When the removal of metal ion impurities meets the standards and the Baume degree of acidic etching waste liquid reaches 30-40°Bé and the pH is 1.0-2.0, and the Baume degree of alkaline etching waste liquid reaches 13-25°Bé and the pH is 8-10, the auxiliary material addition device is controlled to stop adding auxiliary materials.

[0010] Preferably, the pretreated material is conveyed to a neutralization tank via a conveying device. A transmitter module in the neutralization tank collects the second state parameters of the material in the tank in real time. This drives the distributed control module to control the feed rate and stirring state of the alkaline etching waste liquid according to the second state parameters. After the reaction system reaches a preset reaction state, the alkaline copper pressure filter is controlled to perform pressure filtration to obtain an alkaline copper filter cake. The pretreated materials are fed into the neutralization tank according to a preset ratio; The transmitter module of the neutralization tank collects the second state parameters of the material in the neutralization tank in real time, including temperature, pH and liquid level parameters, and inputs the collection results into the distributed control module. The distributed control module controls the feed rate of alkaline etching waste liquid based on the temperature, pH and liquid level parameters, and adjusts the speed or frequency conversion operation parameters of the stirring device at the same time. The reaction system is controlled to react within a pH range of 4.0 to 6.0, a temperature range of 55 to 75°C, and a stirring frequency range of 35 to 40 Hz. When the reaction system reaches the preset reaction state, the distributed control module controls the alkali copper pressure filtration device to start, and the reaction product is pressure filtered to obtain alkali copper filter cake.

[0011] Preferably, the process of conveying the alkali copper filter cake to the ammonia transfer tank, controlling the weighing module of the ammonia transfer tank to obtain the first weight parameter of the alkali copper filter cake, driving the distributed control module to control the ammonia water addition amount and the stirring time according to the first weight parameter, and controlling the copper hydroxide filter press to perform a second filter press after the ammonia transfer reaction is completed to obtain the copper hydroxide filter cake includes: After the alkali copper filter cake is transported to the ammonia transfer tank, the first weight parameter of the alkali copper filter cake is obtained in real time through the weighing module of the ammonia transfer tank, and the first weight parameter is input into the distributed control module. The distributed control module calculates the ammonia dosage based on the weight parameters and the preset dosage ratio, and controls the ammonia dosing device to add ammonia to the ammonia transfer tank; wherein the preset dosage ratio is: by mass, the ratio of alkali copper filter cake to ammonia is 1:1.2 to 1.8. Control the stirring device of the ammonia transfer tank to run for 5 to 15 minutes; When the distributed control module determines that the ammonia conversion reaction is complete, it controls the copper hydroxide filter press to start, and filters the ammonia conversion reaction product to obtain copper hydroxide filter cake.

[0012] Preferably, the step of conveying the copper hydroxide filter cake to a pulping tank, obtaining a second weight parameter of the copper hydroxide filter cake through a weighing module in the pulping tank, and driving the distributed control module to control the addition amount of water or copper sulfate mother liquor and the stirring maintenance time according to the second weight parameter, so that the solid material forms a slurry, includes: The copper hydroxide filter cake is conveyed to the pulping tank, and the second weight parameter of the copper hydroxide filter cake is obtained in real time through the weighing module of the pulping tank, and the second weight parameter is input into the distributed control module. The distributed control module is driven to determine the amount of water or copper sulfate mother liquor to be added based on the second weight parameter, and controls the liquid addition device to add water or copper sulfate mother liquor into the pulping tank. The distributed control module is driven to determine the stirring duration based on the second weight parameter; The stirring device of the pulping tank is controlled to operate for the stirring duration; Determine whether the uniformity of the slurry meets the requirements. If it does not meet the requirements, drive the distributed control module to determine the corrected stirring time based on the stirring maintenance time, the second weight parameter, and the amount of water or copper sulfate mother liquor added. The stirring device of the pulping tank is controlled to operate for the corrected stirring time to obtain a slurry with the required uniformity.

[0013] Preferably, the step of conveying the slurry to the acidification tank, controlling the feeding speed and amount of the slurry and acidic materials through the distributed control module, and acquiring the third state parameters of the reactants in real time, and determining whether the acidification reaction is complete based on the third state parameters, includes: After the slurry is transported to the acidification tank, the distributed control module is driven to control the feeding speed and amount of the slurry and acidic material according to the preset control program. The acidic material is added in a segmented mode of fast addition followed by slow addition. The acidic material is concentrated sulfuric acid. The copper sulfate mother liquor is added by controlling the liquid dosing device to adjust the slurry specific gravity to the preset specific gravity range; The acidification reaction conditions are controlled within the range of temperature 85-95℃ and pH value 0.5-2.0, and the third state parameters of the reactants in the acidification tank are collected in real time, including the Baumé parameter. The collected third state parameters are then input into the distributed control module. When the Baume parameter reaches 40±3°Bé, the distributed control module is driven to stop feeding the acidic material and determine that the acidification reaction is complete.

[0014] Preferably, the step of filtering the material after the acidification reaction through a hot filtration pipe to obtain the acidified filtrate includes: A constant temperature control module and a pressure monitoring module are installed in the heat filtration pipeline. The constant temperature control module is used to maintain the material in the pipeline at a preset temperature. The pressure monitoring module is used to detect the pressure parameters inside the pipeline. When the acidified material passes through the hot filtration pipe, the constant temperature control module and the air pressure monitoring module respectively collect the pipe temperature parameters and air pressure parameters of the hot filtration pipe in real time, and input the collected parameters into the distributed control module. The distributed control module determines the pipeline's operating status based on the temperature and pressure parameters. When the pipeline temperature parameter is lower than a preset threshold, it controls the heating device to start for heating compensation. When the pressure parameter changes abnormally, it controls the alarm device to start.

[0015] Preferably, the acidified filtrate is transported to a crystallization tank, and the cooling rate and crystallization time are controlled by the distributed control module. After crystallization, the product is centrifuged and dried to obtain copper sulfate. The acidified filtrate is transported to a crystallization tank, and the third weight parameter and the fourth state parameter of the acidified filtrate are obtained by the weighing module and the transmitter module of the crystallization tank, respectively, wherein the fourth state parameter includes at least the temperature parameter and the Baumé parameter. The distributed control module determines the cooling rate and crystallization time based on the third weight parameter and the fourth state parameter, and then controls the acidified filtrate to crystallize. After crystallization, the material is automatically fed into a centrifuge to obtain copper sulfate crystals. The copper sulfate crystals are then transported to a drying device by a belt conveyor to dry them and obtain the finished copper sulfate product. The finished copper sulfate product is loaded into a packaging container using an automatic feeding device.

[0016] In summary, the beneficial effects of the present invention are as follows: The production control method for preparing high-purity copper sulfate based on etching waste liquid provided in this invention achieves stable and controllable copper sulfate product quality, with copper sulfate purity consistently above 99.9%, impurity content ≤5ppm, and high-purity batch ratio reaching over 98%. Full-process automation significantly improves production efficiency, shortening the single-batch production cycle to 10-12 hours, approximately 20% shorter than traditional processes, and reducing labor intensity by approximately 60%. Safety and continuity are enhanced; the segmented acidification and dual-monitoring pipeline design prevents reaction runaway and equipment failure, reducing the production failure rate by approximately 80%, and allowing continuous operation for over 72 hours. Real-time data archiving throughout the process supports product quality traceability, meeting the supply chain transparency requirements of the high-end electroplating and electronic materials industries. Simultaneously, precise and automated control of auxiliary material addition reduces resource waste, achieving energy savings of approximately 15% water and 20% electricity, thereby significantly improving process stability, safety, and economy. Attached Figure Description

[0017] To more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the embodiments of the present invention will be briefly introduced below. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort, and these are all within the protection scope of the present invention.

[0018] Figure 1 This is a schematic flowchart of a production control method for preparing high-purity copper sulfate based on etching waste liquid, according to an embodiment of the present invention.

[0019] Figure 2 This is a flowchart illustrating the preprocessing procedure according to an embodiment of the present invention.

[0020] Figure 3 This is a flowchart illustrating the neutralization process in an embodiment of the present invention.

[0021] Figure 4 This is a schematic flowchart of the ammonia conversion process according to an embodiment of the present invention.

[0022] Figure 5 This is a schematic flowchart of the pulping process according to an embodiment of the present invention.

[0023] Figure 6 This is a schematic flowchart of the acidification process according to an embodiment of the present invention.

[0024] Figure 7 This is a flowchart illustrating the filtering process according to an embodiment of the present invention.

[0025] Figure 8 This is a schematic flowchart of the crystallization and drying process according to an embodiment of the present invention. Detailed Implementation

[0026] The features and exemplary embodiments of various aspects of the present invention will now be described in detail. To make the objectives, technical solutions, and advantages of the present invention clearer, the present invention will be further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are only configured to explain the present invention and are not configured to limit the present invention. For those skilled in the art, the present invention can be practiced without some of these specific details. The following description of the embodiments is merely intended to provide a better understanding of the present invention by illustrating examples of the invention.

[0027] It should be noted that, in this document, relational terms such as "first" and "second" are used merely to distinguish one entity or operation from another, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Furthermore, the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such a process, method, article, or apparatus. Without further limitations, an element defined by the phrase "comprising..." does not exclude the presence of additional identical elements in the process, method, article, or apparatus that includes said element.

[0028] Example 1 Please see Figure 1 This invention provides a production control method for preparing high-purity copper sulfate based on etching waste liquid. This method is applicable to the production of high-purity copper sulfate products, especially for the industrial-scale production of electroplating-grade and electronic-grade copper sulfate. The specific steps of the production control method for preparing high-purity copper sulfate based on etching waste liquid are as follows: S1: The etching waste liquid is transported to the pretreatment tank. The transmitter module of the pretreatment tank is controlled to obtain the first state parameter of the etching waste liquid. The distributed control module is driven to calculate and control the amount of auxiliary material added according to the first state parameter of the etching waste liquid until the etching waste liquid reaches the preset treatment state and then the addition of auxiliary material is stopped. S2: The pretreated material is conveyed to the neutralization tank through the conveying device. The second state parameters of the material in the neutralization tank are collected in real time by the transmitter module of the neutralization tank. The distributed control module is driven to control the feed rate and stirring state of the alkaline etching waste liquid according to the second state parameters. After the reaction system reaches the preset reaction state, the alkaline copper pressure filter is controlled to filter and obtain alkaline copper filter cake. S3: The alkali copper filter cake is transported to the ammonia transfer tank. The weighing module of the ammonia transfer tank is controlled to obtain the first weight parameter of the alkali copper filter cake. The distributed control module is driven to control the amount of ammonia water added and the stirring time according to the first weight parameter. After the ammonia transfer reaction is completed, the copper hydroxide filter press is controlled to perform a second filter press to obtain the copper hydroxide filter cake. S4: The copper hydroxide filter cake is conveyed to the pulping tank. The second weight parameter of the copper hydroxide filter cake is obtained through the weighing module of the pulping tank. The distributed control module is driven to control the amount of water or copper sulfate mother liquor added and the stirring time according to the second weight parameter so that the solid material forms a slurry. S5: The slurry is transported to the acidification tank. The feeding speed and amount of the slurry and acidic materials are controlled by the distributed control module. The third state parameters of the reactants are obtained in real time by the transmitter module of the acidification tank. The acidification reaction is judged to be completed based on the third state parameters. S6: The material after the acidification reaction is completed is filtered through a hot filtration pipe to obtain acidified filtrate; S7: The acidified filtrate is transported to a crystallization tank, and the cooling rate and crystallization time are controlled by the distributed control module. After crystallization, the product is centrifuged and dried to obtain copper sulfate.

[0029] Specifically, the etching waste liquid is first transported to a pretreatment tank. A transmitter module installed on the pretreatment tank acquires the first state parameters of the etching waste liquid and transmits these parameters to a distributed control module. The distributed control module calculates the amount of auxiliary materials to be added based on a preset dosing model and drives the execution unit to perform precise dosing, effectively removing impurities from the etching waste liquid until it reaches a preset treatment state, at which point the dosing operation stops. Subsequently, the pretreated material is transported to a neutralization tank via a conveying device. A transmitter module in the neutralization tank collects the second state parameters of the material inside the tank in real time and transmits them to the neutralization tank. The second state parameter is fed back to the distributed control module. Based on the real-time collected second state parameter, the distributed control module adjusts the feed rate and stirring state of the alkaline etching waste liquid to stabilize the reaction system in the preset reaction state. After the reaction reaches the target, the module automatically controls the alkali copper filter press to perform a filter operation, obtaining an alkali copper filter cake. The alkali copper filter cake is transferred to an ammonia transfer tank via a conveying device. The first weight parameter of the alkali copper filter cake is obtained through the weighing module of the ammonia transfer tank. The distributed control module calculates and controls the ammonia dosage and stirring time based on the first weight parameter to ensure the ammonia transfer reaction proceeds fully. After the reaction is completed, the copper hydroxide filter press is driven for further processing. Secondary filtration yields copper hydroxide filter cake. The copper hydroxide filter cake is then conveyed to a slurry tank, where a weighing module obtains a second weight parameter. A distributed control module controls the addition of water or copper sulfate mother liquor based on this second weight parameter, and also controls the stirring time to ensure uniform dispersion of the solid material into a slurry. After slurry formation, the slurry is conveyed to an acidification tank. During acidification, the distributed control module controls the feeding rate and quantity of the slurry and acidic materials. Simultaneously, a transmitter module acquires a third state parameter in real time and uses this parameter to judge and adjust the reaction process, ensuring that pre-conditioning is met. The acidification reaction is confirmed to be complete when the judgment condition is set. After the acidification reaction is completed, the material is filtered through a hot filtration pipeline. The hot filtration pipeline is maintained in a stable operating state under the monitoring of the distributed control module to avoid crystallization or blockage of the material in the pipeline, thereby obtaining acidified filtrate. Finally, the acidified filtrate is transported to a crystallization tank. The distributed control module adjusts the cooling rate and controls the crystallization time according to the preset crystallization control program, so that crystals precipitate according to the predetermined growth conditions. After crystallization, the material is automatically transported to a centrifuge for solid-liquid separation, and then to a drying device for drying, finally obtaining copper sulfate product. Through the coordinated control of the above steps, this method realizes the recycling of copper resources in etching waste liquid, and introduces a distributed control module for full-process automation control in each process link such as pretreatment, neutralization, ammonia conversion, pulping, acidification, filtration and crystallization. It realizes real-time acquisition, dynamic adjustment and data storage of process control parameters, thereby effectively reducing the fluctuation of impurity content and improving the purity stability of the product.

[0030] The copper sulfate product prepared by this method has high purity and low impurity content, making it suitable for applications such as printed circuit board electroplating, precision electronic component manufacturing, metal surface treatment, and electronic chemicals. It also exhibits good adaptability to applications with high requirements for copper ion purity and trace impurity control. Furthermore, this method is applicable to continuous or batch production modes and can be automated and upgraded based on existing chemical production lines, demonstrating strong industrial application value and engineering feasibility.

[0031] In one embodiment, before conveying the etching waste liquid to the pretreatment tank, the method further includes: registering the source and detecting the components of the etching waste liquid, and inputting the source registration data and component detection data into the distributed control module.

[0032] Before the etching waste liquid is transported to the pretreatment tank, its source is registered and its components are analyzed. Specifically, upon entering the plant, the source information of the etching waste liquid is registered through an information entry terminal, including basic data such as the supplier, batch number, transportation time, and storage status, forming a corresponding batch identifier. Simultaneously, the batch of etching waste liquid undergoes component analysis to obtain data such as the content of major metal ions, acid-base properties, and concentration characterization parameters. The source registration data and component analysis data are transmitted via a data interface to a distributed control module for storage and archiving. Based on the component analysis data, the distributed control module automatically matches the corresponding pretreatment parameter model, providing initial data support for subsequent auxiliary material dosage calculations and process parameter settings. By establishing a database linking source and component information before pretreatment, the corresponding management of raw material batches and production parameters is achieved. This improves the targeting and accuracy of auxiliary material addition and provides a complete data chain support for subsequent product quality traceability, thereby enhancing the controllability and traceability of the production process.

[0033] Please see Figure 2 In one embodiment, the step of conveying the etching waste liquid to a pretreatment tank, controlling the transmitter module of the pretreatment tank to acquire the first state parameter of the etching waste liquid, and driving the distributed control module to calculate and control the amount of auxiliary material added based on the first state parameter of the etching waste liquid, until the etching waste liquid reaches a preset treatment state and then the addition of auxiliary material is stopped, includes: S11: After the etching waste liquid is transported to the pretreatment tank, the first state parameter of the etching waste liquid is collected in real time through the transmitter module of the pretreatment tank. The first state parameter includes at least one or more of the following: metal ion concentration parameter, Baumé parameter and pH parameter. S12: The first state parameter is input into the distributed control module, which then obtains the target dosage of the auxiliary material based on a preset dosage determination rule; wherein the auxiliary material includes phosphoric acid and ammonia. S13: Control the auxiliary material addition device to add phosphoric acid and ammonia water into the pretreatment tank according to the target addition amount, and control the actuator to adjust the valve opening to achieve dynamic addition; S14: During the dosing process, the first status parameter is continuously collected and updated in real time through the transmitter module, and the target dosing amount is dynamically corrected by the distributed control module based on the real-time collection and update results; S15: When the removal of metal ion impurities meets the standard and the Baume degree of acidic etching waste liquid reaches 30-40°Bé and the pH is 1.0-2.0, and the Baume degree of alkaline etching waste liquid reaches 13-25°Bé and the pH is 8-10, the auxiliary material addition device is controlled to stop adding auxiliary materials.

[0034] Specifically, the etching waste liquid is first introduced into a pretreatment tank via a transfer pump. The pretreatment tank is integrated with a transmitter module for real-time online monitoring of key initial state parameters of the waste liquid. This transmitter module may include an online metal ion concentration analyzer, pH transmitter, temperature transmitter, density transmitter, or Baumé transmitter. The online metal ion concentration analyzer detects changes in the concentration of copper ions and impurity metal ions; the pH transmitter detects the acidity or alkalinity of the system; the density transmitter or Baumé transmitter acquires the concentration characterization parameters of the waste liquid; and the temperature transmitter helps determine the stability of the reaction environment. All of these transmitters transmit the collected real-time data to a distributed control module. Based on preset dosage rules, the distributed control module automatically calculates the target dosages of phosphoric acid and ammonia and sends control commands to the auxiliary material dosing device. The auxiliary material dosing device adjusts the opening of corresponding valves via actuators to achieve continuous and adjustable precise dosing. During the dosing process, the transmitter module continuously collects real-time data on the metal ion concentration, Baume degree, and pH parameters of the waste liquid in the pretreatment tank. The distributed control module dynamically corrects the dosage of auxiliary materials based on the latest data, forming a closed-loop regulation mechanism to avoid over- or under-dosing caused by intermittent manual dosing. When the detection results show that the removal of metal ion impurities has reached the preset standard, and for acidic etching waste liquid, the Baume degree reaches 30–40°Bé and the pH is controlled within the range of 1.0–2.0; or for alkaline etching waste liquid, the Baume degree reaches 13–25°Bé and the pH is controlled within the range of 8–10, the distributed control module determines that the pretreatment has reached the preset treatment state and immediately issues a stop command to the auxiliary material dosing device to terminate the dosing of phosphoric acid and ammonia. Through the above-mentioned collaborative control methods of online monitoring, model calculation, dynamic correction, and automatic stop, quantitative control and fine adjustment of key first-state parameters in the pretreatment stage are achieved. This not only improves the stability of metal ion impurity removal but also ensures that the acidity, alkalinity, and concentration characterization parameters of the waste liquid are within a reasonable range. At the same time, it enhances the automation level and operational safety of the entire production process.

[0035] Please see Figure 3 In one embodiment, the pretreated material is conveyed to a neutralization tank via a conveying device. A transmitter module in the neutralization tank collects second state parameters of the material in the tank in real time. This data drives the distributed control module to control the feed rate and stirring state of the alkaline etching waste liquid based on the second state parameters. After the reaction system reaches a preset reaction state, the alkaline copper pressure filter is controlled to perform pressure filtration to obtain an alkaline copper filter cake. S21: Input the pretreated material into the neutralization tank according to the preset ratio; S22: The transmitter module of the neutralization tank collects the second state parameters of the material in the neutralization tank in real time, wherein the second state parameters include temperature parameters, pH parameters and liquid level parameters, and inputs the collection results into the distributed control module; S23: Drive the distributed control module to control the feed rate of alkaline etching waste liquid based on the temperature parameter, pH parameter and liquid level parameter, and at the same time adjust the speed or frequency conversion operation parameter of the stirring device; S24: Control the reaction system to react within the range of pH 4.0 to 6.0 and temperature 55 to 75°C. When the reaction system reaches the preset reaction state, the distributed control module controls the alkali copper pressure filter to start and filter the reaction product to obtain alkali copper filter cake.

[0036] Specifically, the pre-treated material is continuously fed into the neutralization tank via a quantitative conveying module according to a preset ratio, which can be determined based on production conditions. The quantitative conveying module can employ a metering pump or a mass flow control device to ensure a stable and controllable flow rate of material entering the neutralization tank. The neutralization tank is equipped with a transmitter module for real-time online monitoring of the second state parameters of the reaction system within the tank. These second state parameters include temperature, pH, and liquid level. The temperature parameter is acquired by a temperature transmitter, the pH parameter by a pH sensor, and the liquid level parameter by a level gauge. The collected real-time data is transmitted to a distributed control module, which analyzes and processes the data and compares it with a preset control range.

[0037] During the neutralization reaction, the distributed control module automatically adjusts the feed rate of the alkaline etching waste liquid based on real-time temperature, pH, and liquid level parameters. When the pH value is too low, the input flow rate of the alkaline etching waste liquid is appropriately increased; when the pH value approaches the upper limit, the feed rate is reduced or suspended, thereby stabilizing the reaction system within the control range of pH 4.0–6.0. ​​Simultaneously, the distributed control module monitors the reaction heat based on temperature parameters fed back from the temperature transmitter, maintaining the reaction system temperature within the range of 55–75℃. If the temperature is too high, it can be adjusted by reducing the feed rate or linking the cooling device; if the temperature is too low, it can be promoted by increasing the feed rate or adjusting the stirring intensity to accelerate the reaction and exothermicly. Furthermore, the distributed control module also controls the operation of the stirring device, adjusting the frequency of the stirrer's frequency converter to maintain stable operation within the range of 35–40Hz, thereby enhancing the uniformity of material mixing, improving reaction mass transfer efficiency, and preventing localized pH or temperature deviations.

[0038] Throughout the neutralization process, temperature, pH, and liquid level parameters are continuously fed back to the distributed control module, forming a closed-loop control system. When the detection results show that the pH of the reaction system is stable within the range of 4.0–6.0, the temperature is maintained within the range of 55–75°C, and the liquid level is within the safe operating range and maintained for a certain period, the distributed control module determines that the reaction has reached the preset reaction state. It then automatically sends a start command to the alkali copper filter press, initiating the filter press program to perform solid-liquid separation on the generated alkali copper precipitate, obtaining an alkali copper filter cake. Through this linkage control method, the feed rate and stirring state during the neutralization stage are automatically adjusted, ensuring stable and controllable reaction conditions, improving the consistency of alkali copper formation and subsequent filter press efficiency, and avoiding parameter fluctuations and product quality instability caused by manual operation.

[0039] Please see Figure 4 In one embodiment, the process of conveying the alkali copper filter cake to an ammonia transfer tank, controlling the weighing module of the ammonia transfer tank to obtain a first weight parameter of the alkali copper filter cake, driving the distributed control module to control the ammonia water addition amount and the stirring time according to the first weight parameter, and controlling the copper hydroxide filter press to perform a second filter press after the ammonia transfer reaction is completed to obtain copper hydroxide filter cake includes: S31: After the alkali copper filter cake is transported to the ammonia transfer tank, the first weight parameter of the alkali copper filter cake is obtained in real time through the weighing module of the ammonia transfer tank, and the first weight parameter is input into the distributed control module; S32: The distributed control module calculates the ammonia dosage based on the weight parameters and the preset dosage ratio, and controls the ammonia dosing device to add ammonia to the ammonia transfer tank; wherein the preset dosage ratio is: by mass, the ratio of alkali copper filter cake to ammonia is 1:1.2~1.8; S33: Control the stirring device of the ammonia transfer tank to run for 5 to 15 minutes; S34: When the distributed control module determines that the ammonia conversion reaction is complete, it controls the copper hydroxide filter press to start and filter the ammonia conversion reaction product to obtain copper hydroxide filter cake.

[0040] Specifically, the alkali copper filter cake obtained from neutralization and pressure filtration is transferred to an ammonia transfer tank via a conveying device. A weighing module is installed at the bottom or on the supporting structure of the ammonia transfer tank to monitor the mass of the alkali copper filter cake entering the tank in real time. After obtaining the first weight parameter of the alkali copper filter cake, the weighing module transmits this parameter to a distributed control module for processing. The distributed control module automatically calculates the target dosage of ammonia water based on the first weight parameter and a preset dosage ratio. The dosage ratio of alkali copper filter cake to ammonia water, by mass, is 1:1.2 to 1.8, preferably 1:1.5. After calculation, the distributed control module sends a control command to the ammonia water dosing device, adjusting the actuator to control the valve opening or the metering pump flow rate, ensuring that ammonia water is accurately added to the ammonia transfer tank according to the calculated value, thus avoiding proportional errors caused by manual estimation. During the ammonia water dosing process, the distributed control module simultaneously controls the stirring device in the ammonia transfer tank to start operation, ensuring thorough mixing and contact of the materials and promoting the reaction between the alkali copper and ammonia water. The stirring time is controlled within the range of 5–15 minutes to ensure sufficient mass transfer and uniform reaction within the system. During stirring, a second state parameter can be used for auxiliary judgment. When the preset reaction time is reached and the reaction completion criteria are met, the distributed control module confirms the completion of the ammonia-to-filter conversion reaction. Subsequently, the distributed control module sends a start command to the copper hydroxide filter press, transporting the material obtained from the ammonia-to-filter conversion reaction to the filter press for solid-liquid separation, obtaining copper hydroxide filter cake. Through weighing feedback and proportional calculation, precise and standardized control of the auxiliary material addition during the ammonia-to-filter conversion stage is achieved, ensuring consistent reaction conditions for each batch, avoiding incomplete reaction or impurity residue due to excessive or insufficient addition, and improving the stability of the copper hydroxide filter cake quality.

[0041] Please see Figure 5 In one embodiment, the step of conveying the copper hydroxide filter cake to a pulping tank, obtaining a second weight parameter of the copper hydroxide filter cake through a weighing module in the pulping tank, and driving the distributed control module to control the addition amount of water or copper sulfate mother liquor and the stirring duration according to the second weight parameter, so that the solid material forms a slurry, includes: S41: The copper hydroxide filter cake is conveyed to the pulping tank, and the second weight parameter of the copper hydroxide filter cake is obtained in real time through the weighing module of the pulping tank, and the second weight parameter is input into the distributed control module; S42: Drive the distributed control module to determine the amount of water or copper sulfate mother liquor to be added according to the second weight parameter, and control the liquid adding device to add water or copper sulfate mother liquor into the pulping tank; S43: Drive the distributed control module to determine the stirring duration based on the second weight parameter; S44: Control the stirring device of the pulping tank to operate for the stirring duration; S45: Determine whether the uniformity of the slurry meets the requirements. If it does not meet the requirements, drive the distributed control module to determine the corrected stirring time based on the stirring maintenance time and the second weight parameter, and the amount of water or copper sulfate mother liquor added. S46: Control the stirring device of the pulping tank to operate the corrected stirring time to obtain a slurry with the required uniformity.

[0042] Specifically, the copper hydroxide filter cake obtained from ammonia-to-pressure filtration is transferred to a pulping tank via a conveying device. A weighing module is installed at the bottom or on the supporting structure of the pulping tank to collect a second weight parameter of the copper hydroxide filter cake entering the tank in real time. This second weight data is transmitted in real time to a distributed control module. The distributed control module calculates the target dosage of water or copper sulfate mother liquor based on this second weight parameter to ensure that the final concentration and specific gravity of the slurry meet the preset process requirements. During the dosing process, the distributed control module sends control commands to the liquid dosing device, adjusting the actuator to control the valve opening or the metering pump flow rate, accurately adding water or copper sulfate mother liquor according to the calculated dosage. This avoids deviations caused by human estimation and ensures the consistency of the composition of each batch of slurry. Simultaneously with the liquid dosing, the distributed control module also calculates the required stirring time based on the filter cake weight parameter and controls the stirring device in the pulping tank to start, maintaining the preset speed and running time, ensuring that the copper hydroxide filter cake is fully mixed with the water or copper sulfate mother liquor to form a homogeneous slurry. During the mixing process, the distributed control module monitors the slurry's uniformity. If the slurry fails to reach the predetermined uniformity, the control module recalculates and corrects the mixing time based on weight parameters, liquid dosage, and the original mixing time, and instructs the mixing device to continue operating until the slurry's uniformity meets the process requirements. This embodiment employs a closed-loop control model of weight feedback—liquid dosage calculation—mixing time control—uniformity correction, ensuring that the slurry's concentration, specific gravity, and uniformity remain consistent across different batches. This avoids incomplete reaction or product quality fluctuations due to slurry inhomogeneity, thereby improving the stability and controllability of the entire high-purity copper sulfate production process.

[0043] Please see Figure 6 In one embodiment, the process of conveying the slurry to the acidification tank, controlling the feeding rate and amount of the slurry and acidic materials through the distributed control module, and acquiring the third state parameters of the reactants in real time, and determining whether the acidification reaction is complete based on the third state parameters, includes: S51: After the slurry is transported to the acidification tank, the distributed control module is driven to control the feeding speed and amount of the slurry and acidic material according to the preset control program. The acidic material is added in a segmented mode of fast addition followed by slow addition. The acidic material is concentrated sulfuric acid. S52: Control the addition of copper sulfate mother liquor by the liquid dosing device to adjust the slurry specific gravity to the preset specific gravity range; S53: Control the acidification reaction conditions within the range of temperature 85-95℃ and pH value 0.5-2.0, and collect the third state parameters of the reaction materials in the acidification tank in real time, wherein the third state parameters include the Baumé parameter, and input the collected third state parameters into the distributed control module; S54: When the Baume parameter reaches 40±3°Bé, the distributed control module is driven to control the acidic material to stop feeding and determine that the acidification reaction is complete.

[0044] Specifically, the homogeneous slurry obtained from the pulping tank is transferred to the acidification tank via a conveying device. The acidification tank is also equipped with a liquid dosing device, temperature transmitter, pH sensor, and Baume transmitter. The distributed control module precisely controls the feeding rate and quantity of the slurry and acidic materials according to a preset control program. The acidic materials, primarily concentrated sulfuric acid, are added in stages. Initially, a rapid addition quickly reaches the reaction initiation conditions, followed by a slower, continuous addition to stabilize the heat release, thus avoiding adverse effects on the reaction system and equipment from intense exothermic reactions. Simultaneously with the addition of the acidic materials, the distributed control module also controls the liquid dosing device to add copper sulfate mother liquor, adjusting the slurry specific gravity to maintain it within a preset range of 1.0–2.0, preferably 1.5, ensuring suitable material concentration and flowability for the acidification reaction. During the acidification process, the distributed control module controls the transmitter module to collect the third-state parameters of the reactants in the acidification tank in real time, including temperature, pH value, and Baume degree. These parameters are then dynamically analyzed and processed to determine the progress of the acidification reaction. By controlling the temperature and pH, the reaction system can be kept stable within the range of 85–95℃ and pH 0.5–2.0, effectively regulating the reaction rate and the risk of side reactions.

[0045] When the Baumé degree parameter reaches the preset range, preferably 40±3°Bé, and the reaction conditions are deemed to meet the design requirements in conjunction with temperature and pH values, the distributed control module automatically stops the acid material feeding device and simultaneously locks the slurry flow rate, marking the completion of the acidification reaction. Throughout the process, the distributed control module uses closed-loop control to continuously monitor and automatically adjust the feeding amount, feed rate, and slurry specific gravity, ensuring that each batch of slurry undergoes a full reaction in the acidification process. This also reduces human error, lowers safety risks, and ensures the consistency and stability of product quality. This control method not only improves the automation and controllability of the acidification process but also helps to increase the yield and purity of copper sulfate.

[0046] In one embodiment, the process of conveying the slurry to the acidification tank, controlling the feeding rate and quantity of the slurry and acidic materials through the distributed control module, and acquiring the third state parameters of the reactants in real time, and determining whether the acidification reaction is complete based on the third state parameters, includes: S501: Obtain the preceding feeding parameters, which include one or more of the following: the amount of auxiliary materials added in the pretreatment stage, the amount of alkaline etching waste liquid fed in the neutralization stage, the amount of ammonia water added in the ammonia conversion stage, and the amount of water or copper sulfate mother liquor added in the pulping stage. Specifically, before the slurry enters the acidification process, the distributed control module reads the feeding data corresponding to the current batch of material from the production records of each preceding process. These preceding feeding parameters reflect the degree of chemical treatment and changes in material composition that the current batch of copper-containing material undergoes before entering the acidification process. Specifically, the amount of auxiliary materials added during the pretreatment stage characterizes the removal of impurities and changes in the acid-base state of the etching waste liquid; the amount of alkaline etching waste liquid fed during the neutralization stage reflects the neutralization ratio between acidic and alkaline materials and the amount of alkali copper generated; the amount of ammonia added during the ammonia conversion stage reflects the reaction ratio during the conversion of alkali copper to copper hydroxide; and the amount of water or copper sulfate mother liquor added during the pulping stage reflects the dilution degree, copper content, and initial specific gravity of the slurry. The distributed control module can associate these parameters according to batch identifiers, enabling acidification control to no longer rely solely on single-point detection results of the current process, but to determine the basic reaction requirements of the current batch by combining the actual processing of the material in the preceding processes, thereby improving the targeting of acidification parameter settings.

[0047] S502: Drive the distributed control module to determine the initial acidification control parameters according to the preceding feeding parameters. The initial acidification control parameters include the initial target dosage of concentrated sulfuric acid, the initial first acceleration rate, the initial second acceleration rate, and the initial stage switching conditions, wherein the initial first acceleration rate is greater than the initial second acceleration rate. Specifically, the distributed control module determines the initial acidification control parameters for the current batch of material based on the preceding feed parameters and the pre-established correspondence between the feed parameters and acidification requirements. The initial target dosage of concentrated sulfuric acid is determined based on the amount of copper hydroxide formed in the preceding treatment, the degree of material dilution, and the amount of concentrated sulfuric acid required that may remain. The initial first acceleration rate is used for rapid acid addition in the early stage of the acidification reaction to allow the system to enter the effective reaction zone as quickly as possible. The initial second acceleration rate is used for slow acid addition in the later stage of the reaction to reduce the risk of excessive acid addition and violent exothermic reactions near the reaction endpoint. The initial stage switching condition is used to determine the timing for switching from the rapid addition stage to the slow addition stage.

[0048] S503: Obtain the actual material parameters of the material to be acidified, wherein the actual material parameters include one or more of the following: copper hydroxide filter cake weight parameter, filter cake moisture content, slurry specific gravity parameter, slurry initial pH parameter, slurry initial temperature parameter, and slurry uniformity parameter; Specifically, after determining the initial acidification control parameters, the actual state of the material to be acidified is further obtained to eliminate potential deviations between the previous feeding records and the actual state of the material. The copper hydroxide filter cake weight parameter characterizes the main copper-containing solids involved in the acidification reaction; the filter cake moisture content determines the ratio of actual solid matter to water carried in the filter cake, avoiding overestimation of the acidified material amount based solely on the total weight of the filter cake; the slurry specific gravity parameter reflects the overall concentration of solid and liquid components in the slurry; the initial slurry pH parameter characterizes the acid-base state of the material before acidification begins; the initial slurry temperature parameter assesses the initial thermal state of the material and its subsequent heat release tolerance; and the slurry homogeneity parameter reflects whether copper hydroxide is uniformly dispersed in the slurry. By obtaining these parameters, the actual acidification status of the current batch of material can be accurately grasped, avoiding the direct application of the same acid feeding parameters due to differences in filter cake moisture content, slurry concentration, or temperature.

[0049] S504: Determine the acidification correction parameters based on the actual material parameters, and correct the initial acidification control parameters based on the acidification correction parameters to obtain the target acidification control parameters. The target acidification control parameters include the target dosage of concentrated sulfuric acid, the first acceleration rate, the second acceleration rate, and the stage switching conditions. Specifically, the distributed control module compares the actual material parameters with the corresponding baseline material state, determines the acidification correction parameters based on the comparison results, and uses these parameters to adjust the initial target dosage of concentrated sulfuric acid, the initial first acceleration rate, the initial second acceleration rate, and the initial stage switching conditions. For example, when the actual solid content of the copper hydroxide filter cake is large or the slurry concentration is high, the target dosage of concentrated sulfuric acid can be increased accordingly; when the filter cake moisture content is high or the slurry specific gravity is low, the acid dosage requirement can be reduced according to the actual effective material quantity; when the initial slurry temperature is high, the first acceleration rate can be reduced or the second addition stage can be entered earlier to control the reaction temperature rise; when the slurry uniformity is poor, the high-speed acid addition can be delayed or stirring can be maintained first to ensure that the concentrated sulfuric acid can fully contact the slurry. The resulting target acidification control parameters take into account both the preceding production process and the current actual material state, which can reduce problems such as insufficient acidification, excessive concentrated sulfuric acid, and temperature runaway caused by fixed acid addition parameters.

[0050] S505: The slurry is transported to the acidification tank, and the liquid dosing device is controlled to add copper sulfate mother liquor to adjust the specific gravity of the slurry to a preset specific gravity range; Specifically, the pulped material is transported to the acidification tank via a pump and pipeline, and the amount of slurry entering the tank is determined by a level detector or metering device. Before the concentrated sulfuric acid is added, the distributed control module controls the liquid dosing device to add copper sulfate mother liquor to the acidification tank, adjusting the slurry's fluidity, concentration, and specific gravity using the copper sulfate mother liquor. The copper sulfate mother liquor can be derived from the recycled mother liquor separated after crystallization, and it itself contains a certain concentration of copper sulfate, thus preventing the introduction of impurities unrelated to the product system when adjusting the slurry's specific gravity. The slurry specific gravity can be continuously monitored during the dosing process, and the addition of copper sulfate mother liquor is stopped once the slurry specific gravity enters the preset range. By adjusting the slurry to a suitable specific gravity before acidification, copper hydroxide can maintain a good dispersion and flow state in the liquid phase, reducing uneven mixing caused by excessive local material viscosity, which is beneficial for the uniform diffusion and stable reaction of the subsequent concentrated sulfuric acid.

[0051] S506: Control the concentrated sulfuric acid to be added according to the first addition acceleration rate, and when the stage switching condition is met, reduce the concentrated sulfuric acid addition acceleration rate from the first addition acceleration rate to the second addition acceleration rate; Specifically, after the slurry specific gravity is adjusted and stirring is maintained, the distributed control module starts the concentrated sulfuric acid metering pump or adjusts the concentrated sulfuric acid dosing valve to add concentrated sulfuric acid to the acidification tank at a first dosing acceleration rate. The first dosing acceleration rate is a relatively high rate, mainly used in the early stages of the acidification reaction. At this point, the slurry still contains a significant amount of copper hydroxide to be acidified, and the added concentrated sulfuric acid can be consumed quickly, thus improving the acid dosing efficiency within the allowable temperature range. During the dosing process, the distributed control module continuously tracks the cumulative amount of concentrated sulfuric acid added and, in conjunction with the temperature, pH value, Baumé degree, and rate of change of the reactants, determines whether the stage switching conditions are met. These stage switching conditions may include one or more of the following: the cumulative dosing reaches a preset ratio, the pH value drops to a preset switching range, the temperature reaches a preset switching temperature, the temperature rise rate exceeds a preset value, or the Baumé degree approaches a preset range. When the stage switching conditions are met, the distributed control module reduces the operating frequency of the metering pump or decreases the opening of the dosing valve, adjusting the concentrated sulfuric acid dosing acceleration rate from the first to the second dosing acceleration rate. The second addition acceleration rate is lower than the first addition acceleration rate. It is used for slow acid replenishment in the later stage of the acidification reaction, so that the subsequently added concentrated sulfuric acid can fully diffuse and react with the remaining copper hydroxide. This reduces the local acid excess, rapid temperature rise and excessive pH drop caused by the reaction approaching the endpoint, thus balancing acidification efficiency and endpoint control accuracy.

[0052] S507: During the addition of concentrated sulfuric acid, the third state parameters of the reactants in the acidification tank are collected in real time. The third state parameters include temperature, pH and Baume degree. Specifically, during the addition of concentrated sulfuric acid and the acidification reaction, temperature transmitters, pH transmitters, and Baumé transmitters installed in the acidification tank continuously collect the temperature, pH, and Baumé parameters of the reactants and send the results to the distributed control module. The temperature parameter characterizes the heat generated by the reaction of concentrated sulfuric acid with the slurry and the thermal state of the reaction system; the pH parameter reflects the process of the slurry gradually transforming from an alkaline or weakly acidic system to an acidic system; and the Baumé parameter characterizes the changes in the concentration of the reaction solution and the density of the system after the formation of copper sulfate. The distributed control module can filter, analyze trends, and determine the validity of the continuously collected data, reducing the impact of material stirring, bubbles, or instantaneous fluctuations in sensors on the control results. By simultaneously monitoring multiple state parameters, the acidification process can be characterized from different aspects such as reaction temperature, degree of acidification, and material concentration, avoiding the need to judge the reaction state solely based on a single pH value or a fixed acid addition time.

[0053] S508: Dynamically correct the remaining dosage of concentrated sulfuric acid and the current dosage rate based on the third state parameter; Specifically, the distributed control module adjusts the amount of concentrated sulfuric acid yet to be added and the current dosing rate in real time based on the current value of the third state parameter and its trend over time. The remaining dosage is the basic remaining amount obtained by subtracting the cumulative actual dosage from the target dosage of concentrated sulfuric acid, and is further adjusted according to changes in pH, Baume degree, and temperature. When the pH decreases slowly and the Baume degree has not yet approached the target range, the current dosing rate can be appropriately increased within the safe temperature range; when the temperature rises too quickly, approaches the upper temperature limit, or the pH value rapidly approaches the lower target limit, the dosing rate can be reduced, dosing can be paused, or the remaining dosage can be reduced; when the Baume degree is close to the target value but the pH value has not yet met the requirements, concentrated sulfuric acid can continue to be added at a lower rate. By adjusting the remaining dosage and the current dosing rate online, the actual dosing process of concentrated sulfuric acid can be matched with the state of the reactants, avoiding over-dosing, under-dosing, or violent exothermic reactions caused by mechanically adding according to a predetermined target value.

[0054] S509: When the temperature of the reactants is between 85 and 95°C, the pH value is between 0.5 and 2.0, and the Baume degree parameter reaches 40 ± 3°Bé, the distributed control module is driven to stop the addition of concentrated sulfuric acid, and the acidification reaction is determined to be complete.

[0055] Specifically, when real-time monitoring results indicate that the temperature of the reactants is between 85 and 95°C, the pH value is between 0.5 and 2.0, and the Baume degree reaches 40 ± 3°Bé, the distributed control module determines that the current reaction system simultaneously meets the acidification completion conditions in terms of temperature, acidity, and concentration. Specifically, a temperature of 85–95°C indicates that the reaction system is maintained within a suitable reaction and material dissolution temperature range; a pH value of 0.5–2.0 indicates that copper hydroxide has been essentially acidified, and the system has the acidity required for subsequent copper sulfate preparation; and a Baume degree of 40 ± 3°Bé indicates that the concentration of the reaction solution is within the preset range. When all the above conditions are met simultaneously, the distributed control module closes the concentrated sulfuric acid dosing valve or stops the metering pump, and records the actual concentrated sulfuric acid dosage, acidification time, and reaction endpoint parameters, simultaneously determining that the acidification reaction is complete. This multi-parameter joint determination method avoids premature or delayed termination due to local fluctuations in a single detection parameter, improving the reliability of acidification endpoint determination and ensuring that subsequent hot filtration and crystallization processes obtain stable acidified materials.

[0056] In one embodiment, the step of driving the distributed control module to determine the initial acidification control parameters based on the preceding feed parameters includes: S5021: Determine the baseline amount of copper-based material to be acidified based on the amount of alkaline etching waste liquid fed during the neutralization stage and the amount of ammonia added during the ammonia conversion stage. Specifically, the distributed control module reads the alkaline etching waste liquid feed rate recorded during the neutralization stage and the ammonia dosage recorded during the ammonia conversion stage for the current production batch, and determines the baseline quantity of the copper-based material to be acidified based on the aforementioned preceding feed data. This baseline quantity characterizes the amount of copper-containing material formed after neutralization, pressure filtration, and ammonia conversion, which theoretically needs to react with concentrated sulfuric acid during the acidification stage. The feed rates of the acidic and alkaline etching waste liquids reflect the scale of copper-containing raw materials entering the neutralization system, while the ammonia dosage further reflects the processing scale of the neutralized alkaline copper during the ammonia conversion stage. The distributed control module can convert the feed data from different processes into a copper-based material characterization quantity based on the preset copper content, effective conversion ratio, or historically calibrated feed correspondence of each material.

[0057] S5022: Based on the feed amount of the alkaline etching waste liquid and the amount of ammonia added, determine the residual alkaline load parameter corresponding to the copper-based material to be acidified. The residual alkaline load parameter is used to characterize the additional consumption of acidic materials by the copper-based material to be acidified during the acidification stage. Specifically, the distributed control module reads the alkaline etching waste liquid feed rate recorded during the neutralization stage and the ammonia water addition rate recorded during the ammonia conversion stage for the current production batch, and determines the residual alkaline load parameter corresponding to the copper-based material to be acidified based on the aforementioned preceding feed data. The residual alkaline load parameter characterizes the degree of additional consumption of concentrated sulfuric acid by the residual alkaline components in the copper-based material to be acidified after neutralization, pressure filtration, and ammonia conversion. The alkaline etching waste liquid feed rate reflects the scale of alkaline components entering the neutralization system, and the ammonia water addition rate reflects the scale of ammonia-containing alkaline components introduced during the ammonia conversion process. Even after reaction and pressure filtration, these alkaline components may still partially remain in the alkaline copper filter cake, copper hydroxide filter cake, or slurry. The distributed control module can convert the corresponding feed rates into a unified residual alkaline load characterization value based on the preset effective alkalinity of the alkaline etching waste liquid and ammonia water, the consumption ratio of the preceding reaction, and the pressure filtration separation ratio. Therefore, when determining the concentrated sulfuric acid addition requirement, the additional acid consumption caused by residual alkaline components can be considered, avoiding insufficient acidification caused by determining the acid addition amount solely based on the amount of copper-based materials.

[0058] S5023: Determine the slurry dilution parameters based on the amount of water or copper sulfate mother liquor added during the pulping stage. The slurry dilution parameters are used to characterize the concentration and flow state of the copper-based material to be acidified before entering the acidification tank. Specifically, the distributed control module reads the amount of water or copper sulfate mother liquor added during the pulping stage of the current production batch and determines the slurry dilution parameters based on this amount. These slurry dilution parameters characterize the solid-liquid ratio, concentration, and flow state of the slurry formed after pulping the copper hydroxide filter cake before entering the acidification tank. Specifically, with roughly the same amount of copper-based material to be acidified, a larger amount of water or copper sulfate mother liquor added generally results in a thinner slurry with relatively low viscosity and good flowability; conversely, a smaller amount of water or copper sulfate mother liquor added generally results in a thicker slurry with relatively high viscosity and potentially slower diffusion of concentrated sulfuric acid. The distributed control module can determine the dilution level of the current batch slurry based on the type and amount of added liquid and the corresponding baseline amount of copper-based material to be acidified, and convert this into slurry dilution parameters that can be used for subsequent acid dosing control. This allows the concentrated sulfuric acid dosing rate and stage switching conditions to match the actual concentration and flow state of the slurry, reducing the risk of localized accumulation of concentrated sulfuric acid and concentrated release of reaction heat.

[0059] S5024: Determine the initial target dosage of concentrated sulfuric acid based on the baseline amount of the copper-based material to be acidified and the residual alkaline load parameters; Specifically, the distributed control module determines the initial target dosage of concentrated sulfuric acid for the current production batch based on the baseline quantity of the copper-based material to be acidified and the residual alkaline load parameter. The initial target dosage of concentrated sulfuric acid characterizes the total amount of concentrated sulfuric acid required to complete the acidification reaction of the current batch of copper-based material without dynamic correction based on real-time state parameters of the acidification process. Specifically, the baseline quantity of the copper-based material to be acidified reflects the amount of basic acid required to convert copper-containing alkaline materials such as copper hydroxide into copper sulfate, while the residual alkaline load parameter reflects the additional amount of compensating acid required to compensate for the residual alkaline components in the material. The distributed control module can first determine the basic dosage based on the baseline quantity of the copper-based material to be acidified and the preset acidification ratio, and then adjust the basic dosage according to the residual alkaline load parameter to obtain the initial target dosage of concentrated sulfuric acid.

[0060] S5025: Based on the initial target dosage of concentrated sulfuric acid, the residual alkaline load parameter, and the slurry dilution parameter, determine the initial dosing acceleration rate parameter, which includes an initial first dosing acceleration rate and an initial second dosing acceleration rate, wherein the initial first dosing acceleration rate is greater than the initial second dosing acceleration rate; Specifically, the distributed control module determines the initial sulfuric acid dosing acceleration parameter based on the initial target dosage of concentrated sulfuric acid for the current production batch, the residual alkaline load parameter, and the slurry dilution parameter. This initial acceleration parameter includes an initial first acceleration rate for the pre-acidification stage and an initial second acceleration rate for the post-acidification stage. Specifically, the initial target dosage of concentrated sulfuric acid reflects the overall acid dosage scale of the current batch; the residual alkaline load parameter reflects the consumption capacity of the pre-acidification materials for concentrated sulfuric acid; and the slurry dilution parameter reflects the diffusion conditions and heat dispersion conditions of the concentrated sulfuric acid after it enters the slurry. In the pre-acidification stage, there is a large amount of copper-based material to be acidified and residual alkaline components, resulting in a relatively strong consumption capacity of the system for concentrated sulfuric acid; therefore, a larger initial first acceleration rate can be used. In the post-acidification stage, the reactants gradually approach the target acidification state, and the system's consumption rate of concentrated sulfuric acid decreases; therefore, an initial second acceleration rate lower than the initial first acceleration rate is used. Therefore, by using a staged addition method that proceeds quickly at first and then slowly, both acidification efficiency and endpoint control precision can be balanced, while reducing the risk of excessive addition of concentrated sulfuric acid and localized violent exothermic reactions in the later stages of the reaction.

[0061] S5026: Determine the initial stage switching conditions based on the residual alkaline load parameters and the slurry dilution parameters. The initial stage switching conditions are used to control the switching of concentrated sulfuric acid from the initial first dosing acceleration rate to the initial second dosing acceleration rate.

[0062] Specifically, the distributed control module determines the initial stage switching conditions for switching concentrated sulfuric acid from the initial first acceleration rate to the initial second acceleration rate based on the residual alkaline load parameters and slurry dilution parameters corresponding to the current production batch. These initial stage switching conditions define the timing of the end of the rapid addition phase in the pre-acidification stage and may include one or more of the following: cumulative concentrated sulfuric acid dosage, the proportion of the cumulative dosage to the initial target dosage, the duration of the first acceleration rate, and changes in the state of the reactants. Specifically, when the residual alkaline load parameter is large, it indicates that the pre-acidification material has a relatively strong capacity to consume concentrated sulfuric acid, allowing for a corresponding increase in the cumulative dosage to enter the second addition stage or an extension of the first acceleration rate maintenance time. When the slurry dilution is low, the concentration is high, or the fluidity is poor, the diffusion and mixing speed of concentrated sulfuric acid in the slurry is relatively slow, allowing for earlier fulfillment of the stage switching conditions to reduce the risk of localized accumulation of concentrated sulfuric acid. Therefore, the timing of different acid addition rate switching can be determined based on the alkalinity load and slurry state of the current batch of materials, avoiding the use of fixed addition time or fixed cumulative addition amount for switching between different batches, and improving the matching degree between the segmented acid addition process and the actual material state.

[0063] In one embodiment, determining acidification correction parameters based on the actual material parameters and correcting the initial acidification control parameters based on the acidification correction parameters includes: S5041: Obtain the actual material parameters of the material to be acidified, wherein the actual material parameters include one or more of the following: actual weight of copper hydroxide filter cake, filter cake moisture content, slurry specific gravity parameter, slurry initial pH parameter, slurry initial temperature parameter, and slurry uniformity parameter; Specifically, before the material to be acidified enters the acidification tank, the distributed control module acquires the actual weight of the copper hydroxide filter cake, filter cake moisture content, slurry specific gravity parameter, slurry initial pH parameter, slurry initial temperature parameter, and slurry uniformity parameter corresponding to the current production batch. The actual weight of the copper hydroxide filter cake can be obtained by a weighing module installed on the pulping tank or material conveying device; the filter cake moisture content can be obtained by a moisture content detection device, or determined based on the weight of the material before and after filtration and the amount of filtrate discharged; the slurry specific gravity parameter, slurry initial pH parameter, and slurry initial temperature parameter can be collected by a specific gravity transmitter, pH transmitter, and temperature transmitter, respectively; the slurry uniformity parameter can be determined based on the differences between the specific gravity, solid content, or concentration detection results at different detection locations of the slurry. The above actual material parameters are used to characterize the actual copper content, residual acid-base state, concentration, thermal state, and mixing state of the material to be acidified, in order to eliminate the deviation between the previous feeding record and the current actual state of the material, so as to facilitate the correction of the initial acidification control parameters.

[0064] S5042: Based on the actual weight of the copper hydroxide filter cake and the moisture content of the filter cake, determine the actual amount of copper-based material to be acidified, and based on the deviation between the actual amount of copper-based material to be acidified and the reference amount of copper-based material to be acidified, determine the dosage correction parameter; Specifically, the distributed control module determines the actual amount of copper-based material to be acidified in the current production batch by deducting the weight corresponding to the moisture content of the copper hydroxide filter cake from its actual weight and moisture content. This actual amount of copper-based material to be acidified characterizes the scale of the actual effective solid material in the copper hydroxide filter cake, preventing the miscalculation of moisture carried by the filter cake as reactant when directly determining the acid dosage based on the total weight of the filter cake. Subsequently, the distributed control module compares the actual amount of copper-based material to be acidified with the baseline amount determined based on the previous feeding parameters to obtain the material quantity deviation between the two, and determines the dosage correction parameter based on the material quantity deviation. When the actual amount of copper-based material to be acidified is greater than the baseline amount, the dosage correction parameter is used to increase the estimated dosage of concentrated sulfuric acid; when the actual amount of copper-based material to be acidified is less than the baseline amount, the dosage correction parameter is used to decrease the estimated dosage of concentrated sulfuric acid. Therefore, the initial acid dosage formed by the previous process data can be corrected by using the actual weighing and moisture content test results, thereby improving the accuracy of the total concentrated sulfuric acid control.

[0065] S5043: Determine the acid consumption correction parameter based on the initial pH parameter and residual alkaline load parameter of the slurry. The acid consumption correction parameter is used to characterize the compensation addition requirement of concentrated sulfuric acid for the material to be acidified. Specifically, the distributed control module determines the acid consumption correction parameters for the current production batch based on the initial pH parameter of the slurry to be acidified and the aforementioned residual alkaline load parameter. The initial pH parameter of the slurry directly reflects the actual acid-base state of the slurry when it enters the acidification stage, while the residual alkaline load parameter reflects the potential additional acid consumption calculated based on the amount of alkaline etching waste liquid fed and the amount of ammonia added. The distributed control module can compare the actually measured initial pH parameter of the slurry with the estimated acid-base state corresponding to the residual alkaline load parameter, and determine the amount of concentrated sulfuric acid that needs to be increased or decreased based on the comparison results. When the initial pH of the slurry is higher than the baseline state or the residual alkaline load is large, it indicates that the material to be acidified has a high additional demand for concentrated sulfuric acid, and the acid consumption correction parameters for increasing the amount of acid added can be determined; when the initial pH of the slurry is lower than the baseline state or the actual alkalinity is less than the estimated value, the acid consumption correction parameters for reducing the amount of acid added can be determined. Thus, the calculation results of the preceding process can be combined with the actual pH detection results before acidification, reducing the impact of residual alkaline component estimation errors on the acidification endpoint.

[0066] S5044: Based on the slurry specific gravity parameter, slurry initial temperature parameter, and slurry uniformity parameter, determine the acceleration rate correction parameter, which is used to correct the initial first acceleration rate and the initial second acceleration rate. Specifically, the distributed control module determines the acceleration rate correction parameter corresponding to the current production batch based on the slurry specific gravity parameter, the slurry initial temperature parameter, and the slurry uniformity parameter. The slurry specific gravity parameter characterizes the slurry concentration and flow resistance; the slurry initial temperature parameter characterizes the thermal state of the reaction system before the addition of concentrated sulfuric acid; and the slurry uniformity parameter characterizes the dispersion degree of copper hydroxide solid in the liquid phase. Specifically, when the slurry specific gravity is high and the slurry uniformity is poor, the diffusion and mixing speed of concentrated sulfuric acid in the slurry is relatively slow, easily leading to excessively high local acid concentration and concentrated local heat release. Therefore, the acceleration rate correction parameter can be used to reduce the initial first acceleration rate and the initial second acceleration rate. When the initial slurry temperature is close to the upper limit of the allowable temperature for the acidification reaction, the corresponding acceleration rate can also be reduced to slow down the release of reaction heat per unit time. When the slurry specific gravity is within a suitable range, the uniformity is good, and the initial temperature is low, the acceleration rate can be maintained or appropriately increased within a safe range. This ensures that the actual addition rate of concentrated sulfuric acid matches the mass transfer conditions, thermal state, and mixing state of the slurry.

[0067] S5045: Determine the stage switching correction parameter based on the slurry specific gravity parameter, the slurry initial temperature parameter, and the acid consumption correction parameter. The stage switching correction parameter is used to correct the initial stage switching conditions. Specifically, the distributed control module determines the stage switching correction parameters corresponding to the transition from a rapid addition stage to a slow addition stage of concentrated sulfuric acid based on the slurry specific gravity parameter, the slurry initial temperature parameter, and the acid consumption correction parameter. The slurry specific gravity parameter reflects the diffusion conditions of concentrated sulfuric acid in the slurry, the slurry initial temperature parameter reflects the ability of the acidification system to continue absorbing reaction heat, and the acid consumption correction parameter reflects the increase or decrease in concentrated sulfuric acid demand for the current batch relative to the initial estimate. When the slurry specific gravity is high or the initial temperature is high, to avoid local overheating caused by excessively long rapid acid addition duration, the rapid addition stage can be ended earlier using the stage switching correction parameters. When the acid consumption correction parameters indicate a large additional acid demand from the current material, and the slurry flow and temperature conditions permit, the stage switching can be appropriately delayed to improve the efficiency of the initial acidification stage. The stage switching correction parameters can be used to adjust the cumulative concentrated sulfuric acid addition threshold, the cumulative addition ratio threshold, the rapid addition duration, or the reaction state threshold, so that the stage switching timing is adapted to the current material concentration, temperature, and actual acid consumption demand.

[0068] S5046: Based on the dosage correction parameter and the acid consumption correction parameter, the initial target dosage of concentrated sulfuric acid is corrected to obtain the target dosage of concentrated sulfuric acid; Specifically, the distributed control module corrects the initial target dosage of concentrated sulfuric acid determined based on the preceding feed parameters using dosage correction parameters and acid consumption correction parameters, thus obtaining the actual target dosage of concentrated sulfuric acid used in the current production batch. The dosage correction parameter compensates for the deviation between the actual amount of copper-based material to be acidified and the baseline amount, while the acid consumption correction parameter compensates for the deviation between the actual pH state of the slurry and the estimated residual alkalinity load from the preceding process. The distributed control module can add or subtract these two types of corrections to the initial target dosage of concentrated sulfuric acid to obtain the final target dosage. When the actual amount of copper-based material is large and the slurry alkalinity is high, the target dosage of concentrated sulfuric acid increases accordingly; when the actual amount of copper-based material is small or the slurry already has a low initial pH, the target dosage of concentrated sulfuric acid decreases accordingly. Therefore, the total acid dosage can be corrected from both the effective amount of copper-containing material and the actual additional acid consumption demand, reducing the problems of insufficient acidification or excessive concentrated sulfuric acid.

[0069] S5047: Based on the acceleration rate correction parameter and the stage switching correction parameter, the initial first acceleration rate, the initial second acceleration rate, and the initial stage switching condition are corrected to obtain the first acceleration rate, the second acceleration rate, and the stage switching condition.

[0070] Specifically, the distributed control module adjusts the initial first and second acceleration rates based on the acceleration rate correction parameters, and adjusts the initial stage switching conditions based on the stage switching correction parameters, resulting in the first acceleration rate, second acceleration rate, and stage switching conditions used for the current production batch. The first acceleration rate is used for rapid acid addition in the initial stage of the acidification reaction, the second acceleration rate is used for slow acid addition in the later stage, and the stage switching conditions determine the timing for switching from the first acceleration rate to the second acceleration rate. During the correction process, the distributed control module can perform correlation verification between the two acceleration rates and the switching conditions, ensuring that the corrected first acceleration rate is still greater than the second acceleration rate, and that the sum of the expected addition amounts for the rapid and slow addition stages matches the target addition amount of concentrated sulfuric acid. For example, when the initial slurry temperature is high or the uniformity is poor, both acceleration rates can be reduced simultaneously and the stage switching can be performed earlier; when the slurry has good fluidity and a large additional acid consumption requirement, a higher first acceleration rate can be maintained and the switching can be delayed. This leads to a segmented acid dosing control scheme that corresponds to the actual material state of the current batch, improving acidification efficiency while reducing the risk of localized intense heat release and excessive acid dosing.

[0071] In one embodiment, the dynamic correction of the remaining dosage of concentrated sulfuric acid and the current dosage rate based on the third state parameter includes: S5081: During the addition of concentrated sulfuric acid, the third state parameters of the reactants in the acidification tank and the cumulative amount of concentrated sulfuric acid added are obtained according to a preset sampling cycle. The third state parameters include temperature parameters, pH parameters and Baume degree parameters. Specifically, during the addition of concentrated sulfuric acid to the acidification tank at either a first or second acceleration rate, the distributed control module reads the temperature, pH, and Baume parameters of the reactants in the acidification tank according to a preset sampling period, and simultaneously acquires the cumulative amount of concentrated sulfuric acid added as recorded by the concentrated sulfuric acid dosing device. The temperature parameter characterizes the thermal state of the reaction between concentrated sulfuric acid and the copper-based material to be acidified; the pH parameter characterizes the acidity of the reactants and the acidification process; the Baume parameter characterizes the concentration state of the reactants; and the cumulative amount of concentrated sulfuric acid added characterizes the total amount of concentrated sulfuric acid added from the start of the acidification reaction in this batch to the current sampling time. The distributed control module can store the above parameters according to the batch identifier and sampling time of the current production batch to form an acidification state parameter sequence. This allows for continuous acquisition of the thermal state, acidity state, concentration state, and actual acid addition progress of the reactants during the concentrated sulfuric acid addition process, facilitating subsequent assessment of reaction risk, endpoint proximity, and dynamic correction of the acid addition process.

[0072] S5082: Determine the rate of temperature rise, rate of pH change, and trend of Baumé change based on the temperature, pH, and Baumé parameters within adjacent sampling periods, respectively. Specifically, the distributed control module acquires the temperature, pH, and Baume parameters corresponding to the current and previous sampling periods, and determines the temperature rise rate, pH change rate, and Baume change trend based on the parameter differences and time intervals between adjacent sampling periods. The temperature rise rate characterizes the degree of temperature increase of the reactants per unit time, reflecting the intensity of heat release under the current concentrated sulfuric acid addition conditions. The pH change rate characterizes the degree of pH change of the reactants per unit time, and can be expressed as the ratio of pH decrease to the sampling time interval to reflect the rate of acidity increase. The Baume change trend characterizes the direction and magnitude of change in reactant concentration as concentrated sulfuric acid is continuously added, and can include states such as Baume increase, stabilization, or abnormal decrease. The distributed control module can also perform smoothing processing based on parameter change results from multiple consecutive sampling periods to reduce instantaneous misjudgments caused by stirring fluctuations or detection noise. Therefore, the dynamic characteristics of reaction parameters changing over time can be further obtained from the state parameters at a single moment, improving the accuracy of judging the development trend of the acidification reaction.

[0073] S5083: Determine the acidification reaction risk status based on the temperature parameters, temperature rise rate, pH parameters, and pH change rate. The acidification reaction risk status is used to characterize the exothermic risk and acidity change risk when concentrated sulfuric acid is continuously added. Specifically, the distributed control module compares the current temperature parameter and temperature rise rate with the corresponding temperature control range and preset temperature rise rate threshold, respectively. Simultaneously, it compares the current pH parameter and pH change rate with the corresponding acidity control range and preset pH change rate threshold, respectively. Based on the comparison results, it determines the acidification reaction risk status. This acidification reaction risk status characterizes the likelihood of the reactants experiencing excessively high temperature, excessively rapid temperature rise, excessively rapid acidity decrease, or localized excess of concentrated sulfuric acid under continued concentrated sulfuric acid addition. For example, when the current temperature has not yet exceeded the upper temperature limit but the temperature rise rate is high, it indicates that the reactants may rapidly approach or exceed the allowable temperature in subsequent sampling periods, thus posing a potential exothermic risk. When the pH value drops rapidly or is already close to the target pH lower limit, it indicates that continuing to maintain the current addition rate may lead to excessively high acidity in the reactants, thus posing an acidity change risk. The distributed control module can classify the acidification reaction risk status into normal, warning, and high-risk states, or convert it into continuously changing risk characterization values. Therefore, it can identify the reaction runaway trend before the temperature or pH parameter truly exceeds the allowable range, enabling early reduction of the addition rate or suspension of concentrated sulfuric acid addition.

[0074] S5084: Based on the Baumé parameter, the Baumé variation trend, and the cumulative amount of concentrated sulfuric acid added, determine the acidification approach state, which is used to characterize the degree to which the reactants approach the target acidification endpoint; Specifically, the distributed control module determines the acidification approach state of the current reactants based on the difference between the current Baumé parameter and the target Baumé range, the Baumé trend within the continuous sampling period, and the proportion of the cumulative concentrated sulfuric acid dosage to the target dosage. This acidification approach state comprehensively characterizes the degree of proximity of the current acidification reaction to the target endpoint. The current Baumé parameter reflects whether the reactants are approaching the target range of 40±3°Bé; the Baumé trend reflects whether the concentration of the reactants is still changing significantly or has gradually stabilized; and the cumulative concentrated sulfuric acid dosage reflects the degree of completion of the predetermined acid dosing task. When the difference between the Baumé parameter and the target range is large and the cumulative dosage is small, the acidification reaction can be determined to be far from the endpoint. When the Baumé parameter enters the vicinity of the target Baumé range, the Baumé change gradually slows down, and the cumulative dosage is close to the target dosage, the acidification reaction can be determined to be near the endpoint. This avoids judging the reaction progress solely based on the cumulative acid dosage or a single Baumé parameter, improving the reliability of the determination of the degree of proximity to the acidification endpoint.

[0075] S5085: Based on the target dosage of concentrated sulfuric acid, the cumulative dosage of concentrated sulfuric acid, the acidification reaction risk status, and the acidification near-state, determine the remaining dosage correction parameter, and correct the remaining dosage of concentrated sulfuric acid based on the remaining dosage correction parameter; Specifically, the distributed control module determines the basic remaining dosage at the current moment based on the difference between the target dosage and the cumulative dosage of concentrated sulfuric acid, and determines the remaining dosage correction parameter in conjunction with the acidification reaction risk status and the acidification approach status. The remaining dosage correction parameter is used to increase, decrease, or maintain the basic remaining dosage calculated directly from the target dosage. When the acidification reaction risk is low and the acidification approach status indicates that the reactants are still significantly far from the target endpoint, the basic remaining dosage can be maintained, or a relatively large subsequent dosage space can be reserved within the allowable range. When the acidification reaction risk increases, or the acidification approach status indicates that the Baumé degree is approaching the target range, the remaining dosage can be reduced to decrease the possibility of subsequent excessive acid addition. When the Baumé degree has entered the vicinity of the target Baumé degree and the pH parameter is also close to the target range, the remaining dosage can be limited to a value suitable for a small-scale acid replenishment at the end. Therefore, the remaining acid addition task can be continuously updated according to the actual state of the reactants, avoiding the concentrated sulfuric acid dosing device mechanically executing the target dosage amount determined before the start of acidification.

[0076] S5086: Determine the acceleration rate correction parameter based on the acidification reaction risk state and the acidification near state, and correct the current acceleration rate of concentrated sulfuric acid based on the acceleration rate correction parameter; wherein, when the temperature rise rate is greater than the preset temperature rise rate threshold, the pH change rate is greater than the preset pH change rate threshold, or the Baumé parameter enters the range near the target Baumé, reduce the current acceleration rate or suspend the addition of concentrated sulfuric acid; Specifically, the distributed control module determines the acceleration rate correction parameter based on the acidification reaction risk status and the acidification approach status, and uses the acceleration rate correction parameter to adjust the currently executed first acceleration rate, second acceleration rate, or the acceleration rate corrected in the previous sampling period. When the acidification reaction risk is normal and the reactants are far from the target acidification endpoint, the current acceleration rate can be maintained; when the reaction risk gradually increases or the reactants gradually approach the target endpoint, the current acceleration rate can be gradually reduced according to the preset adjustment range. Specifically, when the temperature rise rate is greater than the preset temperature rise rate threshold, it indicates that the heat release per unit time is too fast, and the current acceleration rate needs to be reduced or the addition needs to be paused to wait for the temperature of the reactants to stabilize; when the pH change rate is greater than the preset pH change rate threshold, it indicates that the acidity of the reactants is changing rapidly, and continuing to maintain the current acceleration rate may result in excessively low acidity, so the acid addition needs to be slowed down or paused; when the Baume parameter enters the range near the target Baume, it indicates that the reactants are close to the target concentration, and the current acceleration rate should be reduced and a fine acid replenishment state should be entered. Therefore, the actual addition rate of concentrated sulfuric acid can be adaptively adjusted according to the risk of exothermic changes, the risk of acidity changes, and the degree of proximity to the endpoint, so as to reduce violent exothermic reactions and excessive acid addition while ensuring acidification efficiency.

[0077] S5087: The corrected remaining dosage and the corrected current dosage rate are sent to the concentrated sulfuric acid dosing device, and the concentrated sulfuric acid dosing process is dynamically corrected according to the updated third state parameters in the next sampling cycle until the acidification completion condition is met.

[0078] Specifically, the distributed control module converts the corrected remaining dosage and corrected current dosing rate determined in the current sampling cycle into control commands that the concentrated sulfuric acid dosing device can execute, and sends these control commands to the corresponding metering pump, flow regulating valve, or other concentrated sulfuric acid dosing actuators. The concentrated sulfuric acid dosing device adjusts the concentrated sulfuric acid flow rate per unit time according to the corrected current dosing rate, and limits the total amount of concentrated sulfuric acid allowed to be added subsequently according to the corrected remaining dosage. After entering the next sampling cycle, the distributed control module re-acquires the updated temperature parameters, pH parameters, Baume degree parameters, and cumulative concentrated sulfuric acid dosage, and sequentially updates the temperature rise rate, pH change rate, Baume degree change trend, acidification reaction risk status, and acidification approach status, thereby correcting the remaining dosage and current dosing rate again, forming a cyclic feedback control. When the temperature of the reactants is between 85 and 95°C, the pH value is between 0.5 and 2.0, and the Baume degree parameter reaches 40 ± 3°Bé, the distributed control module shuts down the concentrated sulfuric acid dosing device and determines that the acidification reaction is complete. This allows for a closed-loop acid dosing process based on periodic sampling, state judgment, parameter correction, and command execution, enabling the addition of concentrated sulfuric acid to continuously adapt to the dynamic changes in the state of the reactants.

[0079] Please see Figure 7 In one embodiment, the step of filtering the material after the acidification reaction through a hot filtration pipe to obtain the acidified filtrate includes: S61: A constant temperature control module and a pressure monitoring module are installed in the heat filtration pipeline. The constant temperature control module is used to maintain the material in the pipeline at a preset temperature. The pressure monitoring module is used to detect the pressure parameters inside the pipeline. S62: When the acidified material passes through the hot filtration pipe, the constant temperature control module and the air pressure monitoring module respectively collect the pipe temperature parameters and air pressure parameters of the hot filtration pipe in real time, and input the collected parameters into the distributed control module; S63: The distributed control module determines the pipeline operating status based on the temperature and air pressure parameters. When the pipeline temperature parameter is lower than the preset threshold, it controls the heating device to start for heating compensation. When the air pressure parameter changes abnormally, it controls the alarm device to start.

[0080] Specifically, the acidified material is transported through a hot filtration pipeline to remove solid impurities and obtain acidified filtrate. To ensure the continuity and safety of the filtration process, a constant temperature control module and a pressure monitoring module are installed on the hot filtration pipeline. The constant temperature control module maintains the material within the pipeline within a preset temperature range to prevent material from agglomerating and clogging the pipeline due to temperature drops. The pressure monitoring module monitors changes in the internal pressure of the pipeline in real time, promptly detecting abnormal increases or decreases. During the transport of the acidified material, a transmitter module connected to the hot filtration pipeline collects pipeline temperature and pressure parameters in real time and transmits the collected data to a distributed control module. The distributed control module determines whether the material is in a suitable flow state based on the pipeline temperature parameters. When the detected temperature is below a preset threshold, it automatically activates the heating device for heating compensation to keep the material within the set temperature range. Simultaneously, when abnormal pressure fluctuations are detected, the control module triggers an alarm device, prompting operators to take necessary safety measures or activate a preset emergency procedure to prevent pipeline blockage or system failure. By monitoring both constant temperature and air pressure, and combining the automatic regulation of the distributed control module, the hot filtration pipeline can operate safely and stably, ensuring the continuous output of acidified filtrate. This also effectively reduces material agglomeration, pipeline blockage, and operational risks, thereby improving the automation, controllability, and safety of the entire high-purity copper sulfate production process.

[0081] Please see Figure 8 In one embodiment, the acidified filtrate is conveyed to a crystallization tank, and the cooling rate and crystallization time are controlled by the distributed control module. After crystallization, the product is centrifuged and dried to obtain copper sulfate. S71: The acidified filtrate is transported to a crystallization tank, and the third weight parameter and the fourth state parameter of the acidified filtrate are obtained through the weighing module and the transmitter module of the crystallization tank, respectively, wherein the fourth state parameter includes at least the temperature parameter and the Baumé parameter. S72: Drive the distributed control module to determine the cooling rate and crystallization time according to the third weight parameter and the fourth state parameter, and then control the acidified filtrate to crystallize; S73: After crystallization, the material is automatically fed into a centrifuge to obtain copper sulfate crystals. The copper sulfate crystals are then transported to a drying device by a belt conveyor to dry them and obtain the finished copper sulfate product. S74: The finished copper sulfate product is loaded into a packaging container using an automatic feeding device.

[0082] After the acidification reaction, the material is hot-filtered to obtain acidified filtrate, which is then transported to a crystallization tank for crystal precipitation. During crystallization, the distributed control module determines the cooling rate and crystallization time of the crystallization tank based on the acquired third weight parameter and the fourth state parameter. For example, the distributed control module can establish a crystallization kinetic control model based on the material temperature parameter and Baumé parameter, controlling the cooling curve to gradually decrease from the initial temperature to the target crystallization temperature and maintaining the corresponding crystallization time to promote uniform crystal nucleus generation and stable crystal growth, ensuring that the crystal particle size and morphology meet the expected requirements. After crystallization, the distributed control module automatically controls the discharge device to send the crystal slurry into a centrifuge for centrifugal separation. By adjusting the centrifugal speed and time, the crystals are efficiently separated from the mother liquor to obtain wet crystals with appropriate water content. Subsequently, the centrifuged crystals are transferred to a dryer via a belt conveyor. The distributed control module monitors the drying temperature and time parameters to ensure that the crystals are uniformly heated and thoroughly dried during the drying process, preventing heat damage or agglomeration. After drying, the finished copper sulfate is automatically loaded into ton bags by an automatic feeding device, without manual intervention, realizing fully automated operation from acidified filtrate to final product packaging. This process, through precise control of temperature, flow rate, and time parameters, not only improves the yield and purity of copper sulfate but also ensures batch-to-batch product quality consistency. At the same time, it significantly reduces the risks of manual operation, improves production efficiency and safety, and achieves continuous, stable, and traceable production of high-purity copper sulfate.

[0083] In summary, the production control method for preparing high-purity copper sulfate based on etching waste liquid in this invention deeply integrates the distributed control module with the transmitter modules, weighing modules, and actuators of each process unit, achieving closed-loop data-driven management of the entire process from the transportation of etching waste liquid to the pretreatment tank to the final acquisition of copper sulfate product. In the pretreatment stage, the distributed control module can calculate the target dosage of auxiliary materials (such as phosphoric acid and ammonia) based on the first state parameters of the etching waste liquid (including metal ion concentration, Baumé degree, pH, etc.) collected in real time by the transmitter module of the pretreatment tank, and dynamically adjust the dosage process to ensure accurate addition of auxiliary materials and satisfactory removal of impurities from the waste liquid, thereby improving pretreatment efficiency and the basic quality of the product. Inside the neutralization tank, a transmitter module collects real-time secondary state parameters of the material, such as temperature, pH, and liquid level. A distributed control module, based on this data, controls the feed rate and stirring status of the alkaline etching waste liquid, ensuring the neutralization reaction is completed within a preset temperature (55–75℃) and pH (4.0–6.0) range. The system also automatically controls the alkali copper filter press to obtain an alkali copper filter cake. In the ammonia transfer and pulping stages, the distributed control module calculates the dosage of ammonia and water / copper sulfate mother liquor based on the filter cake weight parameters obtained from the weighing modules of the ammonia transfer and pulping tanks. It also controls the stirring time and speed to ensure complete ammonia transfer and homogenization of the slurry, guaranteeing the stability of subsequent acidification and crystallization reaction conditions. In the acidification stage, the distributed control module controls the segmented addition rate and feed rate of the slurry and acidic material (concentrated sulfuric acid), while simultaneously acquiring real-time tertiary state parameters such as Baume degree, temperature, and pH within the acidification tank. This allows for precise determination of the acidification reaction completion time, preventing the reaction from exothermic and potentially dangerous. In the hot filtration stage, a constant temperature control and air pressure monitoring module is installed. The distributed control module can monitor the pipeline temperature and internal air pressure in real time, realizing automatic heating compensation or alarm control, effectively preventing pipeline blockage and improving filtration continuity and stability. In the crystallization and post-processing stages, the distributed control module controls the cooling rate and crystallization time (6-10 hours). After crystallization, centrifugation, drying, and finished product bagging are automatically performed without manual intervention, ensuring the consistency of high-purity copper sulfate production.

[0084] Through the aforementioned fully automated control and modular parameter standardization management, this invention achieves stable and controllable product quality, with copper sulfate purity consistently above 99.9% (the high-purity copper sulfate mentioned in this embodiment refers to copper sulfate with a purity of 99.9% or higher), impurity content ≤5ppm, and high-purity batches accounting for over 98%. Full-process automation significantly improves production efficiency, shortening the single-batch production cycle to 10-12 hours, approximately 20% shorter than traditional processes, and reducing labor intensity by approximately 60%. Safety and continuity are enhanced; the segmented acidification and dual-monitoring pipeline design prevents reaction runaway and equipment failure, reducing the production failure rate by approximately 80%, and allowing continuous operation for over 72 hours. Real-time data archiving throughout the process supports product quality traceability, meeting the supply chain transparency requirements of the high-end electroplating and electronic materials industries. Simultaneously, precise and automated auxiliary material addition reduces resource waste, achieving energy savings of approximately 15% water and 20% electricity, thereby significantly improving process stability, safety, and economy.

[0085] It should be clarified that the present invention is not limited to the specific configurations and processes described above and shown in the figures. For the sake of brevity, detailed descriptions of known methods are omitted here. In the above embodiments, several specific steps are described and shown as examples. However, the method process of the present invention is not limited to the specific steps described and shown. Those skilled in the art can make various changes, modifications, and additions, or change the order of steps, after understanding the spirit of the present invention.

[0086] It should also be noted that the exemplary embodiments mentioned in this invention describe methods or systems based on a series of steps or apparatus. However, this invention is not limited to the order of the steps described above; that is, the steps can be performed in the order mentioned in the embodiments, or in a different order, or several steps can be performed simultaneously. In the description of this specification, the reference to terms such as "one embodiment / mode," "some embodiments / modes," "example," "specific example," or "some examples," etc., means that a specific feature, structure, material, or characteristic described in connection with that embodiment / mode or example is included in at least one embodiment / mode or example of this application. In this specification, the illustrative expressions of the above terms do not necessarily refer to the same embodiment / mode or example. Moreover, the specific features, structures, materials, or characteristics described can be combined in a suitable manner in any one or more embodiments / modes or examples. Furthermore, without contradiction, those skilled in the art can combine and integrate the different embodiments / modes or examples and the features of different embodiments / modes or examples described in this specification.

[0087] The above description is merely a specific embodiment of the present invention. Those skilled in the art will clearly understand that, for the sake of convenience and brevity, the specific working processes of the systems, modules, and units described above can be referred to the corresponding processes in the foregoing method embodiments, and will not be repeated here. It should be understood that the protection scope of the present invention is not limited thereto. Any person skilled in the art can easily conceive of various equivalent modifications or substitutions within the technical scope disclosed in the present invention, and these modifications or substitutions should all be covered within the protection scope of the present invention.

Claims

1. A production control method for preparing high-purity copper sulfate based on etching waste liquid, characterized in that, The method includes: The etching waste liquid is transported to the pretreatment tank. The transmitter module of the pretreatment tank is controlled to obtain the first state parameter of the etching waste liquid. The distributed control module is driven to calculate and control the amount of auxiliary material added according to the first state parameter of the etching waste liquid until the etching waste liquid reaches the preset treatment state and then the addition of auxiliary material is stopped. The pretreated material is conveyed to the neutralization tank through a conveying device. The transmitter module of the neutralization tank collects the second state parameters of the material in the neutralization tank in real time. The distributed control module is driven to control the feed rate and stirring state of the alkaline etching waste liquid according to the second state parameters. After the reaction system reaches the preset reaction state, the alkaline copper pressure filter is controlled to filter and obtain alkaline copper filter cake. The alkali copper filter cake is transported to the ammonia transfer tank. The weighing module of the ammonia transfer tank is controlled to obtain the first weight parameter of the alkali copper filter cake. The distributed control module is driven to control the amount of ammonia water added and the stirring time according to the first weight parameter. After the ammonia transfer reaction is completed, the copper hydroxide filter press is controlled to perform a second filter press to obtain the copper hydroxide filter cake. The copper hydroxide filter cake is conveyed to a pulping tank. A second weight parameter of the copper hydroxide filter cake is obtained through a weighing module in the pulping tank. The distributed control module is then driven to control the dosage of water or copper sulfate mother liquor and the stirring duration based on this second weight parameter, causing the solid material to form a slurry. This process includes: The copper hydroxide filter cake is conveyed to the pulping tank, and the second weight parameter of the copper hydroxide filter cake is obtained in real time through the weighing module of the pulping tank, and the second weight parameter is input into the distributed control module. The distributed control module is driven to determine the amount of water or copper sulfate mother liquor to be added according to the second weight parameter, and controls the liquid addition device to add water or copper sulfate mother liquor into the pulping tank. The distributed control module is driven to determine the stirring duration based on the second weight parameter; The stirring device of the pulping tank is controlled to operate for the stirring duration; Determine whether the uniformity of the slurry meets the requirements. If it does not meet the requirements, drive the distributed control module to determine the corrected stirring time based on the stirring maintenance time, the second weight parameter, and the amount of water or copper sulfate mother liquor added. The stirring device of the pulping tank is controlled to operate at the corrected stirring time to obtain a slurry with the required uniformity; The slurry is conveyed to the acidification tank. The feeding rate and quantity of the slurry and acidic materials are controlled by the distributed control module. The third state parameter of the reactants is acquired in real time by the transmitter module of the acidification tank. The completion of the acidification reaction is determined based on the third state parameter, including: Obtain the preceding feeding parameters, which include one or more of the following: the amount of auxiliary materials added in the pretreatment stage, the amount of alkaline etching waste liquid fed in the neutralization stage, the amount of ammonia added in the ammonia conversion stage, and the amount of water or copper sulfate mother liquor added in the pulping stage. The distributed control module is driven to determine the initial acidification control parameters based on the preceding feeding parameters. The initial acidification control parameters include the initial target dosage of concentrated sulfuric acid, the initial first acceleration rate, the initial second acceleration rate, and the initial stage switching conditions, wherein the initial first acceleration rate is greater than the initial second acceleration rate. Obtain the actual material parameters of the material to be acidified, including one or more of the following: copper hydroxide filter cake weight parameter, filter cake moisture content, slurry specific gravity parameter, slurry initial pH parameter, slurry initial temperature parameter, and slurry uniformity parameter; The acidification correction parameters are determined based on the actual material parameters, and the initial acidification control parameters are corrected based on the acidification correction parameters to obtain the target acidification control parameters. The target acidification control parameters include the target dosage of concentrated sulfuric acid, the first acceleration rate, the second acceleration rate, and the stage switching conditions. The slurry is transported to an acidification tank, and copper sulfate mother liquor is added by a liquid dosing device to adjust the specific gravity of the slurry to a preset specific gravity range. Concentrated sulfuric acid is added at the first acceleration rate, and when the stage switching condition is met, the acceleration rate of concentrated sulfuric acid is reduced from the first acceleration rate to the second acceleration rate. During the addition of concentrated sulfuric acid, the third state parameters of the reactants in the acidification tank are collected in real time. These third state parameters include temperature, pH and Baume degree. The remaining dosage of concentrated sulfuric acid and the current dosage rate are dynamically corrected based on the third state parameter. When the temperature of the reactants is between 85 and 95°C, the pH value is between 0.5 and 2.0, and the Baume degree parameter reaches 40 ± 3°Bé, the distributed control module is driven to stop the addition of concentrated sulfuric acid and the acidification reaction is determined to be complete. The material after the acidification reaction is completed is filtered through a hot filtration pipeline to obtain the acidified filtrate, which includes: A constant temperature control module and a pressure monitoring module are installed in the heat filtration pipeline. The constant temperature control module is used to maintain the material in the pipeline at a preset temperature. The pressure monitoring module is used to detect the pressure parameters inside the pipeline. When the acidified material passes through the hot filtration pipe, the constant temperature control module and the air pressure monitoring module respectively collect the pipe temperature parameters and air pressure parameters of the hot filtration pipe in real time, and input the collected parameters into the distributed control module. The distributed control module determines the pipeline operating status based on the temperature and air pressure parameters. When the pipeline temperature parameter is lower than the preset threshold, it controls the heating device to start for heating compensation. When the air pressure parameter changes abnormally, it controls the alarm device to start. The acidified filtrate is transported to a crystallization tank, and the cooling rate and crystallization time are controlled by the distributed control module. After crystallization, the product is centrifuged and dried to obtain copper sulfate.

2. The production control method for preparing high-purity copper sulfate based on etching waste liquid according to claim 1, characterized in that, Before the etching waste liquid is transported to the pretreatment tank, the method further includes: registering the source and detecting the components of the etching waste liquid, and inputting the source registration data and component detection data into the distributed control module.

3. The production control method for preparing high-purity copper sulfate based on etching waste liquid according to claim 1, characterized in that, The step of conveying the etching waste liquid to the pretreatment tank, controlling the transmitter module of the pretreatment tank to obtain the first state parameter of the etching waste liquid, driving the distributed control module to calculate and control the amount of auxiliary material added based on the first state parameter of the etching waste liquid, and stopping the addition of auxiliary material after the etching waste liquid reaches the preset treatment state includes: After the etching waste liquid is transported to the pretreatment tank, the first state parameter of the etching waste liquid is collected in real time through the transmitter module of the pretreatment tank. The first state parameter includes at least one or more of the following: metal ion concentration parameter, Baumé parameter and pH parameter. The first state parameter is input into the distributed control module, which then obtains the target dosage of the auxiliary material based on a preset dosage determination rule; wherein the auxiliary material includes phosphoric acid and ammonia. The auxiliary material dosing device is controlled to add phosphoric acid and ammonia water into the pretreatment tank according to the target dosing amount, and the actuator is controlled to adjust the valve opening to achieve dynamic dosing; During the dosing process, the transmitter module continuously collects and updates the first status parameter in real time, and the distributed control module dynamically corrects the target dosing amount based on the real-time collection and update results. When the removal of metal ion impurities meets the standards and the Baume degree of acidic etching waste liquid reaches 30-40°Bé and the pH is 1.0-2.0, and the Baume degree of alkaline etching waste liquid reaches 13-25°Bé and the pH is 8-10, the auxiliary material addition device is controlled to stop adding auxiliary materials.

4. The production control method for preparing high-purity copper sulfate based on etching waste liquid according to claim 3, characterized in that, The pretreated material is conveyed to a neutralization tank via a conveying device. A transmitter module in the neutralization tank collects the second state parameters of the material in the tank in real time. This data drives the distributed control module to control the feed rate and stirring state of the alkaline etching waste liquid based on these second state parameters. After the reaction system reaches a preset reaction state, the alkaline copper pressure filter is controlled to perform pressure filtration to obtain an alkaline copper filter cake. The pretreated materials are fed into the neutralization tank according to a preset ratio; The transmitter module of the neutralization tank collects the second state parameters of the material in the neutralization tank in real time, including temperature, pH and liquid level parameters, and inputs the collection results into the distributed control module. The distributed control module controls the feed rate of alkaline etching waste liquid based on the temperature, pH and liquid level parameters, while adjusting the speed or frequency conversion operation parameters of the stirring device. The reaction system is controlled to react within a pH range of 4.0 to 6.0, a temperature range of 55 to 75°C, and a stirring frequency range of 35 to 40 Hz. When the reaction system reaches the preset reaction state, the distributed control module controls the alkali copper pressure filtration device to start, and the reaction product is pressure filtered to obtain alkali copper filter cake.

5. The production control method for preparing high-purity copper sulfate based on etching waste liquid according to claim 4, characterized in that, The process of conveying the alkali copper filter cake to the ammonia transfer tank, controlling the weighing module of the ammonia transfer tank to obtain the first weight parameter of the alkali copper filter cake, driving the distributed control module to control the ammonia water addition amount and the stirring time according to the first weight parameter, and controlling the copper hydroxide filter press to perform a second filter press after the ammonia transfer reaction is completed to obtain the copper hydroxide filter cake includes: After the alkali copper filter cake is transported to the ammonia transfer tank, the first weight parameter of the alkali copper filter cake is obtained in real time through the weighing module of the ammonia transfer tank, and the first weight parameter is input into the distributed control module. The distributed control module calculates the ammonia dosage based on the first weight parameter and the preset dosage ratio, and controls the ammonia dosing device to add ammonia to the ammonia transfer tank; wherein the preset dosage ratio is: by mass, the ratio of alkali copper filter cake to ammonia is 1:1.2 to 1.

8. Control the stirring device of the ammonia transfer tank to run for 5 to 15 minutes; Once the distributed control module determines that the ammonia conversion reaction is complete, it controls the copper hydroxide filter press to start, and filters the ammonia conversion reaction product to obtain copper hydroxide filter cake.

6. The production control method for preparing high-purity copper sulfate based on etching waste liquid according to claim 5, characterized in that, The acidified filtrate is transported to a crystallization tank, and the cooling rate and crystallization time are controlled by the distributed control module. After crystallization, the product copper sulfate is obtained by centrifugation and drying. The acidified filtrate is transported to a crystallization tank, and the third weight parameter and the fourth state parameter of the acidified filtrate are obtained by the weighing module and the transmitter module of the crystallization tank, respectively, wherein the fourth state parameter includes at least the temperature parameter and the Baumé parameter. The distributed control module determines the cooling rate and crystallization time based on the third weight parameter and the fourth state parameter, and then controls the acidified filtrate to crystallize. After crystallization, the material is automatically fed into a centrifuge to obtain copper sulfate crystals. The copper sulfate crystals are then transported to a drying device by a belt conveyor to dry them and obtain the finished copper sulfate product. The finished copper sulfate product is loaded into a packaging container using an automatic feeding device.

Citation Information

Patent Citations

  • Device and method for preparing copper sulfate from waste etching liquid

    CN117383739B

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    CN121672572A