Electrochemical test device and method for in-situ leaching of leaching mining minerals

Abstract

The invention discloses an electrochemical test device and method for in-situ leaching of leaching mining minerals, and the device comprises a liquid inlet system which comprises a liquid reservoir, a liquid inlet pipe and a peristaltic pump, one end of the liquid inlet pipe is connected with the liquid reservoir, the other end of the liquid inlet pipe is connected with a reaction system, and the peristaltic pump is installed on the liquid inlet pipe; the reaction system comprises an ore leaching column, a fixing plate and a supporting frame, the fixing plate is arranged above the ore leaching column, the ore leaching column and the fixing plate are fixed through the supporting frame, an ore sample to be detected is arranged in the ore leaching column, and a liquid inlet pipe penetrates through the fixing plate and then is located in the center above the ore sample to be detected; the liquid collecting system comprises a funnel, filter paper and a liquid collector, the funnel is fixed below the ore leaching column through a supporting frame, the filter paper is placed above the funnel, and the liquid collector is placed below the funnel; the electrochemical testing system comprises a working electrode, a counter electrode and a reference electrode, one end of each electrode penetrates through the fixing plate and is connected to the interior of the to-be-tested ore sample, and the other end of each electrode is connected with the electrochemical workstation through a wire. According to the invention, in-situ, lossless and dynamic testing can be carried out.

Description

Technical Field

[0001] The present invention relates to an electrochemical test device and method for in-situ leaching of minerals in leaching mining, belonging to the field of electrochemical test equipment for mineral leaching. Background Technique

[0002] Leaching mining is a mining method that, based on physical and chemical principles and chemical processes, uses certain chemical solvents and microorganisms to selectively dissolve, leach, and recover useful components in deposits, ores, or waste rocks. It plays an important role in improving the comprehensive utilization rate of resources and mainly includes in-situ leaching method, heap leaching method, and in-situ fragmentation leaching method. Among them, the in-situ leaching method reduces the links of mining, transporting, and processing minerals and is directly carried out on the mine body, effectively reducing production costs. It is outstanding in dealing with small and medium-sized deposits with low grades and complex and difficult-to-treat ores, including copper ores, rare earth ores, uranium ores, etc. During the in-situ leaching process, since the leaching solution will chemically react with the minerals themselves, directly affecting the leaching rate and leaching efficiency of target elements, and the chemical reaction is accompanied by ion migration and electrical phenomena, it has electrochemical characteristics. Conducting electrochemical tests on the leaching process through an electrochemical test device is of great significance for studying the chemical reaction mechanism and electrochemical reaction mechanism of the mineral leaching process, and is also of great significance for realizing the dynamic monitoring of the leaching process and further achieving precise control.

[0003] Currently, the widely used electrochemical test device is mainly an electrolytic cell, and some studies also use self-made devices. The electrolytic cell is mostly used for the monitoring of the coexistence body of electrode materials and solutions, with a wide application range and relatively mature technology. However, the bottom of this device is in a closed state, only the top is open, and it cannot meet the requirements of the continuous flow dynamic process monitoring required by the in-situ leaching process. The self-made devices in other studies are also mostly designed according to their respective working conditions and are not suitable for the electrochemical tests of in-situ leaching of minerals in leaching mining. Summary of the Invention

[0004] Aiming at the problems existing in the above-mentioned prior art, the present invention provides an electrochemical test device and method for in-situ leaching of minerals in leaching mining, which can meet the electrochemical test requirements of mineral leaching in leaching mining.

[0005] In order to achieve the above purpose, an electrochemical test device for in-situ leaching of minerals in leaching mining adopted by the present invention includes:

[0006] A liquid inlet system, including a liquid storage device, a liquid inlet pipe, and a peristaltic pump. One end of the liquid inlet pipe is connected to the liquid storage device, the other end is connected to the reaction system, and the peristaltic pump is installed on the liquid inlet pipe;

[0007] The reaction system comprises a leaching column, a fixed plate and a support frame, wherein the fixed plate is placed above the leaching column, the leaching column and the fixed plate are fixed by the support frame, a sample to be tested is placed in the leaching column, and the liquid inlet pipe passes through the fixed plate and is located at the center above the sample to be tested;

[0008] The liquid collecting system comprises a funnel, filter paper and a liquid collector, wherein the funnel is fixed below the leaching column through a support frame, the filter paper is placed above the funnel, and the liquid collector is placed below the funnel;

[0009] The electrochemical test system includes a working electrode, a counter electrode and a reference electrode. One end of each electrode passes through a fixing plate and is connected to the inside of the mineral sample to be tested, and the other end is connected to the electrochemical workstation through a wire.

[0010] As an improvement, the fixed plate is provided with a liquid inlet pipe fixing groove and three regularly arranged electrode fixing grooves, the liquid inlet pipe fixing groove is located at the center of the three electrode fixing grooves, the liquid inlet pipe is installed in the liquid inlet pipe fixing groove, and the working electrode, counter electrode and reference electrode are respectively installed in the electrode fixing grooves.

[0011] As an improvement, the liquid inlet tube, the working electrode, the counter electrode and the reference electrode are respectively fixed on the fixed plate by limiters.

[0012] As an improvement, the electrochemical workstation is connected to a computer and a host computer.

[0013] As an improvement, the bottom of the leaching column is a pinhole liquid outlet plate.

[0014] As an improvement, the diameter of the funnel is larger than the diameter of the pinhole liquid outlet plate.

[0015] As an improvement, the electrochemical workstation is equipped with an electrode main wire, the other end of which is provided with a working electrode wire, a counter electrode wire and a reference electrode wire, each with an alligator clip, and the working electrode, counter electrode and reference electrode are connected to the working electrode wire, the counter electrode wire and the reference electrode wire, respectively.

[0016] As an improvement, filter paper is placed on the surface of the mineral sample to be tested.

[0017] In a second aspect of the present invention, there is also provided an electrochemical test method for in-situ leaching of solution-mined minerals, using the electrochemical test device for in-situ leaching of solution-mined minerals, comprising the following steps:

[0018] S1. Install a peristaltic pump on a liquid inlet pipe, one end of which is connected to a liquid reservoir, the liquid reservoir is filled with leaching liquid, the leaching liquid is fully mixed with the ore sample to be tested, and then the ore sample to be tested is placed in a leaching column;

[0019] S2. Place a filter paper above the ore sample to be tested. Pass the liquid inlet tube through the fixing plate and position it above the filter paper. Additionally, pass the pre-prepared working electrode, counter electrode, and reference electrode through the fixing plate and the filter paper above the ore sample to be tested and bury them into the ore sample to be tested. Fix the liquid inlet tube and the three electrodes respectively with limiters, control the depth of each electrode buried in the ore sample to be tested to be the same, and fix the fixing plate.

[0020] S3. Connect the working electrode wire, counter electrode wire, and reference electrode wire with crocodile clips to the working electrode, counter electrode, and reference electrode respectively.

[0021] S4. Place the funnel and the liquid receiver below the leaching column, and also place a filter paper in the funnel.

[0022] S5. Turn on the power supply of the electrochemical workstation and the test software to conduct the test. Before starting the peristaltic pump, the static electrochemical impedance spectrum of the ore sample to be tested can be measured. After starting the peristaltic pump, the dynamic electrochemical impedance spectrum of the entire leaching process can be measured. The obtained data is plotted using Origin software.

[0023] Compared with the prior art, the present invention has the following beneficial effects:

[0024] (1) It can effectively control the reaction conditions and improve the leaching efficiency. The liquid inlet system of the present invention is an independent system, which can effectively control the reaction conditions, including the inlet liquid concentration, type, temperature, and inlet liquid speed. By controlling different reaction conditions, it can be adjusted at any time during the test, and tests under different reaction conditions can also be carried out, which can meet the different scenario requirements of the test. Through continuous monitoring, the flow situation of the leaching solution in the ore layer can be understood in real time, so as to adjust the mining parameters in a timely manner, ensure that the leaching solution can contact the ore evenly and effectively, improve the leaching efficiency, and the monitoring data can be used to optimize the injection volume and injection speed of the leaching solution to further improve the leaching efficiency.

[0025] (2) It can achieve non-destructive, in-situ, and dynamic online monitoring under continuous flow conditions and reduce production costs. The reaction system of the present invention is a connected "upper-in and lower-out" system, which provides convenient conditions for continuous testing. During the test, the minerals react with the leaching solution. Through the electrochemical workstation and the three-electrode system, real-time testing can be carried out, and the flow of the leaching solution is synchronized with the electrochemical testing, realizing dynamic monitoring of the reaction process of the leaching process, which is crucial for studying the reaction mechanism of the entire leaching process. Through mechanism research and optimization of mining parameters, the consumption of raw materials and energy can be reduced, thereby reducing production costs.

[0026] (3) The height of the electrode is adjustable, enabling three-dimensional testing, which provides guidance for process scale-up production. In the electrochemical test device of the present invention, the fixed plate and the limiter adopted can be used to control the embedding depth of the electrode in the ore sample, which is beneficial for conducting tests even when the amount of ore sample used is small. At the same time, by adjusting the height of the electrode, the requirements for testing different depths of the same ore sample can be met, realizing "three-dimensional" testing, and also providing important guidance for subsequent process scale-up production and application. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] To more clearly illustrate the technical solutions in the embodiments of the present application or the prior art, the following will briefly introduce the drawings required for use in the description of the embodiments or the prior art. Obviously, the drawings in the following description are only some embodiments of the present application. For those skilled in the art, without creative efforts, other drawings can be obtained based on these drawings.

[0028] Figure 1 is a schematic structural diagram of the electrochemical test device of the present invention;

[0029] Figure 2 is a schematic partial structural diagram of the reaction system of the present invention;

[0030] Figure 3 is an electrochemical impedance spectrogram (partial time period) of the leaching process of ionic rare earth ore in Example 2;

[0031] In the figure: 1. Liquid storage device, 2. Liquid inlet pipe, 3. Peristaltic pump; 4. Leaching column, 5. Fixed plate, 6. Support frame, 7. Working electrode fixing groove, 8. Counter electrode fixing groove, 9. Reference electrode fixing groove, 10. Liquid inlet pipe fixing groove, 11. Working electrode limiter, 12. Counter electrode limiter, 13. Reference electrode limiter, 14. Liquid inlet pipe limiter, 15. Pinhole liquid outlet plate; 16. Funnel, 17. Filter paper, 18. Liquid collector; 19. Working electrode, 20. Counter electrode, 21. Reference electrode, 22. Electrochemical workstation, 23. Computer, 24. Host, 25. Total electrode wire, 26. Working electrode wire, 27. Counter electrode wire, 28. Reference electrode wire. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0032] To make the objectives, technical solutions, and advantages of the present invention clearer, the following will provide a detailed description of the technical solutions of the present application through the drawings and specific embodiments. It should be understood that the specific features in the embodiments of the present application and the embodiments are detailed descriptions of the technical solutions of the present application, rather than limitations on the technical solutions of the present application. Without conflict, the technical features in the embodiments of the present application and the embodiments can be combined with each other.

[0033] Example 1

[0034] As shown in Figure 1 、 Figure 2 Figure(s) [to be filled], an electrochemical test device for in-situ leaching of minerals by solution mining includes a liquid inlet system, a reaction system, a liquid collection system, and an electrochemical test system;

[0035] The liquid inlet system includes a liquid storage tank 1, a liquid inlet pipe 2, and a peristaltic pump 3. One end of the liquid inlet pipe 2 extends into the liquid storage tank 1, and the other end is connected to the reaction system. The peristaltic pump 3 is installed on the liquid inlet pipe 2 to drive the liquid into the reaction system and control the flow rate and direction of the liquid. The independent liquid inlet system of the present invention provides convenience for controlling reaction conditions. It can test the electrochemical parameters of the ore sample leaching process under different working conditions by independently changing the concentration, temperature, and type of the leaching solution, and can also realize tests at different speeds by controlling the flow rate with the peristaltic pump, providing convenience for tests under different reaction conditions. The independent liquid inlet system can be adjusted and optimized according to different needs, thus providing higher flexibility;

[0036] The reaction system includes a leaching column 4, a fixing plate 5, and a support frame 6. The fixing plate 5 is placed above the leaching column 4, and the leaching column 4 and the fixing plate 5 are fixed by the support frame 6. The leaching column 4 contains the ore sample to be tested, and the liquid inlet pipe 2 passes through the fixing plate 5 and is located at the center above the ore sample to be tested. This reaction system is a connected "upper inlet and lower outlet" system, ensuring the continuity of the leaching process, enabling the leaching solution to pass through the ore sample to be tested in a continuous flow manner. The entire leaching process realizes leaching by pumping the leaching solution, with liquid inlet at the upper end and liquid outlet at the lower end, providing favorable conditions for in-situ, non-destructive, and on-line monitoring of the leaching process;

[0037] The liquid collection system includes a funnel 16, a filter paper 17, and a liquid collector 18. The funnel 16 is fixed below the leaching column 4 by the support frame 6. The filter paper 17 is placed above the funnel 16, and the liquid collector 18 is placed below the funnel 16;

[0038] The electrochemical test system includes a working electrode 19, a counter electrode 20, and a reference electrode 21. One end of each electrode passes through the fixing plate 5 and is connected to the inside of the ore sample to be tested, and the other end is connected to an electrochemical workstation 22 through a wire.

[0039] As an improved embodiment, as shown in Figure 2As shown in the figure, a liquid inlet pipe fixing groove 10 and three regularly arranged electrode fixing grooves are formed on the fixing plate 5. The liquid inlet pipe fixing groove 10 is located at the center of the three electrode fixing grooves. The liquid inlet pipe 2 is installed in the liquid inlet pipe fixing groove 10, and the working electrode 19, counter electrode 20, and reference electrode 21 are respectively installed in the electrode fixing grooves. The aperture of the electrode fixing groove is determined according to the electrode size, and the aperture of the liquid inlet pipe fixing groove is determined according to the diameter of the liquid inlet pipe. The fixing plate 5 of the present invention integrates a liquid inlet pipe fixing groove and three electrode fixing grooves, forming a "center - triangle" symmetric layout, which can ensure that the incoming liquid evenly diffuses from the center to the electrode area, facilitating the realization of consistent reaction interface conditions. The triangular arrangement of the electrodes ensures the symmetric layout of the electrodes, ensuring the consistent relative position of the electrodes in each test, effectively reducing human error, eliminating the influence of uneven distance, reducing electric field distortion, improving the uniformity of potential distribution, and avoiding the reaction rate difference caused by uneven current distribution. The aperture can be independently determined according to actual needs, improving the versatility of the device.

[0040] As an improved embodiment, as Figure 1 shown, the liquid inlet pipe 2 uses a liquid inlet pipe limiter 14, the working electrode 19 uses a working electrode limiter 11, the counter electrode 20 uses a counter electrode limiter 12, and the reference electrode 21 uses a reference electrode limiter 13, which are respectively fixed on the fixing plate 5, and the electrodes are buried inside the ore sample. The burial depth of the electrodes is controlled by the electrode limiters. By setting limiters at the upper ends of the electrodes, the burial depth of the electrodes in the ore sample can be effectively adjusted to achieve tests at different positions of the ore sample. At the same time, when the mass of the ore sample is small, the test under the condition of less ore sample can also be achieved by adjusting the burial depth, and the test conditions are more flexible. The limiter can be a circular rubber product, which is relatively simple to install and use and is convenient to operate.

[0041] As an improved embodiment, as Figure 1 shown, the electrochemical workstation 22 is connected to the computer 23 and the host 24, and the information of the electrochemical workstation 22 is processed and analyzed through the computer 23 and the host 24.

[0042] As an improved embodiment, as Figure 2 shown, the bottom of the ore leaching column 4 is a pinhole liquid outlet plate 15, and the liquid leached from the ore sample enters the liquid collection system through the pinhole liquid outlet plate 15. Further, the diameter of the funnel 16 is larger than the diameter of the pinhole liquid outlet plate 15, and a filter paper 17 is placed in the funnel 16 for filtering the leaching solution.

[0043] As an improved embodiment, as Figure 1As shown, the electrochemical workstation 22 is equipped with a main electrode wire 25. At the other end of the main electrode wire 25, there are a working electrode wire 26, a counter electrode wire 27, and a reference electrode wire 28, each with an alligator clip. The working electrode 19, the counter electrode 20, and the reference electrode 21 are respectively connected to the working electrode wire 26, the counter electrode wire 27, and the reference electrode wire 28.

[0044] This test device can perform in-situ, non-destructive, and dynamic tests, and can truly reflect the dynamic reaction conditions of all stages of the in-situ leaching process, realizing the monitoring of electrochemical parameters during the entire ore leaching process.

[0045] Example 2

[0046] Use this electrochemical test device to carry out an exploration test on the evolution law of electrochemical impedance spectroscopy during the in-situ leaching process of ionic rare earth ore, including the following steps:

[0047] S1. Install the peristaltic pump 3 on the inlet pipe 2. One end of the inlet pipe 2 is connected to the reservoir 1, and the reservoir 1 contains the ore leaching solution. Use ammonium sulfate solution as the ore leaching solution. Weigh a certain amount of pretreated ionic rare earth ore samples, fully mix the ore leaching solution with the rare earth ore samples, and then place the rare earth ore samples into the leaching column 4 with a diameter of Φ59mm×90mm.

[0048] S2. The aperture of the inlet pipe fixing groove 10 is 6mm and it is located at the center of the fixing plate 5. The aperture of the electrode fixing groove is 6mm, and the number is 3 (evenly arranged in an equilateral triangle outside the inlet pipe fixing groove 10, and the center distance between the centers of each electrode fixing groove is 2cm). Place a filter paper above the rare earth ore samples, pass the inlet pipe 2 through the fixing plate 5 and place it above the filter paper, filter the ore leaching solution of the inlet pipe 2 through this filter paper, and respectively pass the pre-prepared working electrode 19, counter electrode 20, and reference electrode 21 through the fixing plate 5 and the filter paper above the ore sample to be measured and bury them into the rare earth ore samples. Fix the inlet pipe 2 and the three electrodes with limiters respectively. The buried depths of the three electrodes should be the same to ensure that the test ends of the three electrodes correspond to each other, and fix the fixing plate 5.

[0049] S3. Connect the working electrode wire 26, the counter electrode wire 27, and the reference electrode wire 28, each with an alligator clip, to the working electrode 19, the counter electrode 20, and the reference electrode 21 respectively.

[0050] S4. Place the funnel 16 and the liquid collector 18 under the leaching column 4, and also place a filter paper 17 in the funnel.

[0051] S5. Turn on the power supply of the electrochemical workstation and the test software to conduct the test. The static electrochemical impedance spectrum of ionic rare earth ores can be tested before starting the peristaltic pump, and the dynamic electrochemical impedance spectrum of the whole process of ore leaching can be tested after starting the peristaltic pump. The obtained data is plotted using Origin software. See Figure 3 .

[0052] The above are only the preferred embodiments of the present invention, and do not impose any form of limitation on the present invention. Although the present invention has been disclosed above with the preferred embodiments, it is not intended to limit the present invention. Any person skilled in the art of this patent, without departing from the scope of the technical solution of the present invention, may make some modifications or equivalent changes using the technical content prompted above as equivalent embodiments. However, as long as it does not depart from the content of the technical solution of the present invention, any simple modification, equivalent change and modification made to the above embodiments according to the technical essence of the present invention still fall within the scope of the present invention.

Claims

1. An electrochemical test device for in-situ leaching of solution-mined minerals, characterized in that: include: A liquid inlet system, comprising a liquid reservoir (1), a liquid inlet pipe (2) and a peristaltic pump (3), wherein one end of the liquid inlet pipe (2) is connected to the liquid reservoir (1), and the other end is connected to the reaction system, and the peristaltic pump (3) is installed on the liquid inlet pipe (2); The reaction system comprises a leaching column (4), a fixing plate (5) and a support frame (6), wherein the fixing plate (5) is placed above the leaching column (4), the leaching column (4) and the fixing plate (5) are fixed by the support frame (6), a mineral sample to be tested is placed in the leaching column (4), and the liquid inlet pipe (2) passes through the fixing plate (5) and is located at the center above the mineral sample to be tested; A liquid collecting system comprises a funnel (16), a filter paper (17) and a liquid collector (18), wherein the funnel (16) is fixed below the leaching column (4) via a support frame (6), the filter paper (17) is placed above the funnel (16), and the liquid collector (18) is placed below the funnel (16); The electrochemical testing system comprises a working electrode (19), a counter electrode (20) and a reference electrode (21), one end of each electrode respectively passes through a fixing plate (5) and is connected to the inside of a mineral sample to be tested, and the other end is connected to an electrochemical workstation (22) via a wire.

2. The electrochemical test device for in-situ leaching of solution-mined minerals according to claim 1, characterized in that: The fixing plate (5) is provided with a liquid inlet pipe fixing groove (10) and three regularly arranged electrode fixing grooves, the liquid inlet pipe fixing groove (10) is located at the center of the three electrode fixing grooves, the liquid inlet pipe (2) is installed in the liquid inlet pipe fixing groove (10), and the working electrode (19), the counter electrode (20) and the reference electrode (21) are respectively installed in the electrode fixing grooves.

3. The electrochemical test device for in-situ leaching of solution-mined minerals according to claim 2, characterized in that: The liquid inlet tube (2), the working electrode (19), the counter electrode (20) and the reference electrode (21) are respectively fixed on the fixed plate (5) via limiters.

4. The electrochemical test device for in-situ leaching of solution-mined minerals according to claim 1, characterized in that: The electrochemical workstation (22) is connected to a computer (23) and a host computer (24).

5. The electrochemical test device for in-situ leaching of solution-mined minerals according to claim 1, characterized in that: The bottom of the leaching column (4) is a pinhole liquid outlet plate (15).

6. The electrochemical test device for in-situ leaching of solution-mined minerals according to claim 5, characterized in that: The diameter of the funnel (16) is greater than the diameter of the pinhole liquid outlet plate (15).

7. The electrochemical test device for in-situ leaching of solution-mined minerals according to claim 1, characterized in that: The electrochemical workstation (22) is equipped with an electrode main wire (25), and the other end of the electrode main wire (25) is provided with a working electrode wire (26), a counter electrode wire (27) and a reference electrode wire (28) each with an alligator clip, and the working electrode (19), the counter electrode (20) and the reference electrode (21) are connected to the working electrode wire (26), the counter electrode wire (27) and the reference electrode wire (28) respectively.

8. The electrochemical test device for in-situ leaching of solution-mined minerals according to claim 1, characterized in that: Filter paper is placed on the surface of the ore sample to be tested.

9. An electrochemical test method for in-situ leaching of solution-mined minerals, characterized in that: The electrochemical test device for in-situ leaching of solution-mined minerals according to any one of claims 1 to 8 comprises the following steps: S1, installing a peristaltic pump (3) on a liquid inlet pipe (2), one end of the liquid inlet pipe (2) is connected to a liquid reservoir (1), the liquid reservoir (1) is filled with leaching liquid, the leaching liquid and the ore sample to be tested are fully mixed, and then the ore sample to be tested is placed in a leaching column (4); S2. Place filter paper above the mineral sample to be tested, pass the liquid inlet pipe (2) through the fixed plate (5) and place it above the filter paper, and pass the pre-prepared working electrode (19), counter electrode (20) and reference electrode (21) through the fixed plate (5) and the filter paper above the mineral sample to be tested and bury them in the mineral sample to be tested, fix the liquid inlet pipe (2) and the three electrodes with stoppers, control the depth of each electrode buried in the mineral sample to be tested to be consistent, and fix the fixed plate (5); S3, connecting the working electrode wire (26), the counter electrode wire (27) and the reference electrode wire (28) with the crocodile clip to the working electrode (19), the counter electrode (20) and the reference electrode (21), respectively; S4, placing a funnel (16) and a liquid collector (18) below the leaching column (4), and the funnel is also equipped with filter paper (17); S5. Turn on the power supply of the electrochemical workstation and the test software to start the test. Before the peristaltic pump (3) is turned on, the static electrochemical impedance spectrum of the ore sample to be tested can be tested. After the peristaltic pump (3) is turned on, the dynamic electrochemical impedance spectrum of the whole leaching process can be tested. The obtained data is plotted using Origin software.

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