On-line sampling and detecting device for extraction and separation of rare earth

Abstract

The utility model discloses an on-line sampling and detecting device for extraction and separation of rare earth. The on-line sampling and detecting device comprises a sampling container, a sampling pump, a filter, a sample diluting component, a remote transmission component and an on-line analyzer, the sampling container is connected with a feed liquid inlet of the sampling pump through a sampling pipeline, a feed liquid outlet of the sampling pump is connected with a feed liquid inlet of the filter through a sampling pipeline, a feed liquid outlet of the filter is connected with a feed liquid inlet of the sample dilution component through a sampling pipeline, and a sample outlet of the sample dilution component is connected with the remote transmission component. And the remote transmission component is connected with the on-line analyzer through a sample transmission pipeline. The device disclosed by the utility model can realize real-time, continuous and full-flow detection of the REO and impurity contents in the key control points of the tank body of the extraction tank.

Description

TECHNICAL FIELD

[0001] The utility model belongs to the field of rare earth hydrometallurgy, and particularly relates to a rare earth extraction separation online sampling and detecting device. BACKGROUND

[0002] Rare earth elements are difficult to separate due to their extremely similar chemical properties, and the separation cost is high. At present, China separates single rare earth by using the method of rare earth cascade extraction, and the separation process is complex, and a large number of process control parameters are required, and hundreds of extraction tanks are needed, and a large amount of organic phase, lye and acid and other raw and auxiliary materials are consumed in the process.

[0003] Publication No. CN113495058A discloses a rare earth extraction online analysis system and an analysis method thereof, which comprises an analysis system, a communication device and a main control system, and the analysis system is connected with the main control system through the communication device; the analysis system comprises a spectral measurement device, a cleaning device and a to-be-measured liquid preparation device; the to-be-measured liquid preparation device comprises a preparation dish, and the preparation dish is connected with a to-be-measured liquid suction pipe, an enrichment device and a dilution device respectively; a spectral measurement probe of the spectral measurement device and the cleaning device are arranged in the preparation dish and adjacent to each other. The analysis method is composed of a spectral analysis method and a color analysis method, and in the case that the absorbance of the to-be-measured liquid is not in the set range, a measurement liquid needs to be prepared, thereby causing a long detection period and being unable to timely guide production.

[0004] The document "Research on Online Detection System for Rare Earth Extraction Process" is composed of two parts "Research on Rare Earth Online Monitoring System by Spectrophotometry" and "Research on Solution Acidity Online Monitoring System", and the document discloses a flow injection-spectrophotometry rare earth online monitoring device, and the system repeatability (RSD) is less than 2%, which is relatively low.

[0005] The document "Simultaneous Online Determination of Total Rare Earth Content and Component Rare Earth Content in Light Rare Earth Extraction Separation" studies the online simultaneous determination of total rare earth content and component rare earth content in light rare earth extraction separation by using a multi-channel energy spectrometer, and the relative standard deviation of the total rare earth content analysis method adopted in the document is 4.2%, which is relatively high.

[0006] At present, most rare earth enterprises still rely on laboratory offline analysis to determine the distribution content and impurity content of rare earth to guide the process, and the sampling and analysis period is long, thereby causing problems such as low production efficiency, large resource consumption, unstable tank operation and product quality and the like of the enterprise. Therefore, an online sampling and analysis system with high efficiency and stability, automatic, real-time and continuous monitoring is urgently needed. UTILITY MODEL CONTENT

[0007] The utility model aims at providing a rare earth extraction separation online sampling and detecting device, which can realize real-time, continuous and full-process detection of REO and impurity content in the key control points of the tank body of the extraction tank.

[0008] To achieve the above object, the technical solution used by the utility model is:

[0009] The rare earth extraction separation on-line sampling detection device comprises a sampling container, a sampling pump, a filter, a sample dilution component, a remote transmission component and an on-line analyzer.

[0010] Further, the sampling container is arranged outside the extraction tank and is communicated with the extraction tank.

[0011] Further, the upper part of the sampling container is open, and the lower part is connected with the liquid inlet of the sampling pump through the sampling pipeline.

[0012] Further, the filter is of a closed structure and is internally filled with filter fibers.

[0013] Further, the sample dilution component comprises a water storage tank, a mixing tank, a liquid taking pump, a mixing pump and a liquid control valve.

[0014] Further, the remote transmission component is located at the liquid outlet position of the mixing tank, and the outlet of the remote transmission component is connected with the sample transmission pipeline.

[0015] Further, the remote transmission component is located at the liquid outlet position of the mixing tank, and the remote transmission component comprises a sampling bottle, a collection bottle, a sampling pipeline, a high-pressure gas cylinder, a gas pipeline and a six-way valve.

[0016] Further, the six-way valve is internally provided with a quantitative ring, and the quantitative ring is located at the liquid inlet.

[0017] Further, the on-line analyzer is located at the end of the sample transmission pipeline, and the on-line analyzer adopts an inductively coupled plasma atomic emission spectrometer (ICP-OES).

[0018] Further, the signal output end of the online analyzer is connected to the signal input end of the single-chip microcomputer through a signal line, and the single-chip microcomputer is connected to a computer at a remote end.

[0019] The technical effects of the utility model include:

[0020] The introduction of the new equipment and the selection of the process control points can realize real-time, continuous and full-process detection of REO (rare earth oxide) and impurity content in the key control points of the tank body of the extraction tank, thereby realizing production guidance, stabilizing the operation of the extraction tank body, ensuring product quality and solving the problems of low data real-time performance, poor sample expression, poor data effectiveness and large artificial workload caused by the traditional offline monitoring method.

[0021] Through the application of the online analysis system, the artificial input in the production process is greatly reduced, the automation, intelligence and informatization level of the production process management are improved, the product quality is stabilized, and the economic benefit is increased. The utility model can be popularized and applied in rare earth wet smelting enterprises and other chemical industries. After the implementation of the online sampling analysis system, the following effects are brought about:

[0022] 1. The real-time performance of the detection data is improved.

[0023] The rare earth content and impurity content detection data acquisition time of the tank monitoring point is reduced from 2h-4h to 15min-30min.

[0024] The application adopts the online analyzer (inductively coupled plasma atomic emission spectrometry, ICP-OES) with high precision, good repeatability and small relative deviation, which contains online sampling, filtering, dilution and analysis functions, can realize multi-point, real-time continuous online detection, and avoids the technical defects of long detection period and inability to timely guide production.

[0025] 2. The artificial sampling frequency is reduced.

[0026] From 12-24 times / day to 2-3 times / day.

[0027] 3. Through the timely feedback and guidance of online data, the adjustment of control parameters due to manual operation experience is avoided, the optimal feed amount and reaction conditions are ensured, and the stable operation of production and the quality of products are ensured.

[0028] 4. The repeatability precision of the detection and the relative standard deviation of the total rare earth content are effectively improved.

[0029] The application adopts completely different detection methods, and the system repeatability precision (RSD) can reach ≤0.5%, and the system repeatability precision is effectively improved.

[0030] The application can realize automatic sampling, on-line analysis and detection by using on-line diluent, and the relative standard deviation of total rare earth content is less than or equal to 2%.

[0031] 5. The application can realize the automation and intelligent process control of extraction.

[0032] The application can realize the automation, intelligent and informatization of production process management, meet the demand of intelligent sensing in the construction process of intelligent smelting plant, promote the transformation and upgrading, high-quality development of enterprises, and improve the comprehensive competitiveness and sustainable development ability of enterprises. BRIEF DESCRIPTION OF DRAWINGS

[0033] Figure 1 is the structural principle diagram of the rare earth extraction separation on-line sampling detection device in the utility model;

[0034] Figure 2 is the structural principle diagram of the sample dilution component in the utility model;

[0035] Figure 3 is the structural principle diagram of the remote transmission component in the utility model. DETAILED DESCRIPTION

[0036] The following description fully illustrates the specific implementation of the utility model, so that those skilled in the art can practice and reproduce.

[0037] As Figure 1 shown, it is the structural principle diagram of the rare earth extraction separation on-line sampling detection device in the utility model.

[0038] The rare earth extraction separation on-line sampling detection device comprises a sampling container 1, a sampling pump 2, a filter 4, a sample dilution component 6, a remote transmission component 7, an on-line analyzer 9, a single-chip microcomputer 10 and a computer 11.

[0039] The upper part of the sampling container 1 is open, the lower part is connected with the liquid inlet of the sampling pump 2 through the sampling pipeline 3, the liquid outlet of the sampling pump 2 is connected with the liquid inlet of the filter 4 through the sampling pipeline 3, the liquid outlet of the filter 4 is connected with the liquid inlet of the sample dilution component 6 through the sampling pipeline 3, the sample outlet of the sample dilution component 6 is located at the side of the remote transmission component 7 (or the sample outlet is close to the remote transmission component 7), the remote transmission component 7 is connected with the on-line analyzer 9 through the sample transmission pipeline 8, the signal input end of the single-chip microcomputer 10 is connected with the on-line analyzer 9 through a signal line, and the single-chip microcomputer 5 is connected with the remote computer 11.

[0040] The sampling container 1 is arranged outside the extraction tank and communicates with the extraction tank, and the feed liquid in the extraction tank enters the sampling container 1 to be collected as a sample solution.

[0041] The sampling pump 2 is powered by an external power supply and is used for conveying the sample solution collected by the sampling container 1 into the filter 4, and the sampling pump 2 returns the excessive sample solution to the sampling container 1 through the reflux pipeline 5.

[0042] The filter 4 is arranged on the sampling pipeline 3 and is used for online filtering of the sample solution, and the filter 4 is a closed structure and is internally filled with filter fibers.

[0043] As shown in Figure 2 Fig. 3 is a structural principle view of the sample dilution component 6 in the utility model.

[0044] The sample dilution component 6 is connected to the sampling pipeline 3 and is used for online dilution of the sample solution to achieve 10-100 times dilution.

[0045] The sample dilution component 6 comprises a water storage tank 61, a mixing tank 62, a liquid taking pump 63, a mixing pump 64 and a feed liquid control valve 65, the mixing pump 64 is connected between the water outlet of the water storage tank 61 and the water inlet of the mixing tank 62 through a dilution pipeline, the feed liquid inlet of the mixing tank 62 is connected to the sampling pipeline 3 through a dilution pipeline, the liquid taking pump 63 is arranged at the feed liquid inlet of the mixing tank 62, and the feed liquid outlet of the mixing tank 62 is provided with the feed liquid control valve 65.

[0046] The water storage tank 61 stores pure water used for diluting the sample solution, the liquid taking pump 63 takes the sample solution from the sampling pipeline 3 and sends it into the mixing tank 62, the mixing pump 64 sends the pure water into the mixing tank 62 and mixes the sample solution, the detection personnel opens the feed liquid control valve 65, takes the diluted sample solution from the mixing tank 62, puts it into a sampling bottle 71, and puts the sampling bottle into the remote transmission component 7.

[0047] As shown in Figure 3 Fig. 4 is a structural principle view of the remote transmission component 7 in the utility model.

[0048] The remote transmission component 7 is located at the liquid outlet position of the mixing tank 62, and the remote transmission component 7 comprises a sampling bottle 71, a collection bottle 72, a sampling pipeline 73, a high-pressure gas cylinder 74, a gas pipeline 75, a six-way valve 76 and a three-way valve 77; the sampling bottle 71 is connected with the liquid inlet of the six-way valve 76 through the sampling pipeline 73, and the sampling pipeline 73 on one side of the sampling bottle 71 is provided with a sampling needle 78; the collection bottle 72 is connected with the liquid outlet of the six-way valve 76 through the sampling pipeline 73; the high-pressure gas cylinder 74 is connected with the three-way valve 77 through the gas pipeline 75; the outlet of the three-way valve 77 is connected with the carrier gas inlet of the six-way valve 76; and the carrier gas outlet of the six-way valve 76 is connected with the sample transmission pipeline 8.

[0049] The high-pressure gas cylinder 74 is used for storing high-pressure inert gas. The three-way valve 77 is an electromagnetic valve, which is used for controlling the opening and closing of the gas pipeline 75. The six-way valve 76 is a six-way valve sampler, and the working principle is as follows: when being located at the sampling (Load) position, the sample solution is injected into the quantitative ring in the six-way valve 76 through the sampling needle 78 from the sampling hole at the liquid inlet of the six-way valve 76; after the quantitative ring is filled, the excess sample is discharged from the liquid outlet of the six-way valve 76; when being located at the injecting (Inject) position, the flow channel between the carrier gas inlet and the carrier gas outlet of the six-way valve 76 is connected, the inert gas conveying mobile phase flushes the quantitative ring, and the sample solution is pushed into the sample transmission pipeline 8 to reach the liquid phase analysis column of the online analyzer 9 for analysis.

[0050] The online analyzer 9 is located at the end of the sample transmission pipeline 8, and an ICP-OES analyzer is adopted; the operator takes down the sampling bottle, detects the REO (rare earth oxide) and impurity content in the sample solution through the ICP-OES analyzer, and forms detection data.

[0051] The signal input end of the single-chip microcomputer 10 is connected with the signal output end of the ICP-OES analyzer through a signal line; the signal output end is connected with the remote computer 11 through a signal line (of course, the signal output end can also be transmitted to the computer 11 located in the central control room at the remote end in the form of a network); the single-chip microcomputer 5 is used for receiving and storing the detection data of the sampling containers 1 at different positions, and sending the detection data to the computer 11 at the remote end through a signal line.

[0052] The computer 11 realizes online analysis of the sample by calling the detection data of different sampling containers 1.

[0053] The terms used in the utility model are illustrative and non-restrictive terms. Since the utility model can be embodied in various forms without departing from the spirit or essence of the technical scheme, it should be understood that the above examples are not limited to any of the above details, but should be widely interpreted within the spirit and scope defined by the appended claims, and therefore all changes and modifications falling within the scope of the claims or their equivalents should be covered by the appended claims.

Claims

1. A device for on-line sampling and detecting in rare earth extraction separation, characterized in that, The application relates to a sampling device for on-line analysis of liquid samples, which comprises a sampling container, a sampling pump, a filter, a sample dilution component, a remote transmission component and an on-line analyzer; the sampling container is connected to the liquid inlet of the sampling pump through a sampling pipeline, the liquid outlet of the sampling pump is connected to the liquid inlet of the filter through a sampling pipeline, the liquid outlet of the filter is connected to the liquid inlet of the sample dilution component through a sampling pipeline, the sample outlet of the sample dilution component is located on the side of the remote transmission component, and the remote transmission component is connected to the on-line analyzer through a sample transmission pipeline. The sampling container is arranged outside the extraction tank and is connected to the extraction tank.

2. The on-line sampling and detecting device for rare earth extraction separation according to claim 1, characterized in that, The upper part of the sampling container is open, and the lower part is connected to the liquid inlet of the sampling pump through a sampling pipeline; the liquid outlet of the sampling pump is connected to the upper part of the sampling container through a reflux pipeline.

3. The on-line sampling and detecting device for rare earth extraction separation according to claim 1, characterized in that, The filter is a closed structure and is filled with filter fibers inside.

4. The on-line sampling and detecting device for rare earth extraction separation according to claim 1, characterized in that, The sample dilution component comprises a water storage tank, a mixing tank, a liquid taking pump, a mixing pump and a liquid control valve; the mixing pump is connected between the water outlet of the water storage tank and the water inlet of the mixing tank through a dilution pipeline; the liquid inlet of the mixing tank is connected to the sampling pipeline through a dilution pipeline; the liquid taking pump is arranged at the liquid inlet of the mixing tank; and the liquid outlet of the mixing tank is provided with the liquid control valve.

5. The on-line sampling and detecting device for rare earth extraction separation according to claim 1, characterized in that, The remote transmission component is located at the liquid outlet position of the mixing tank, and the outlet of the remote transmission component is connected to the sample transmission pipeline.

6. The on-line sampling and detecting device for rare earth extraction separation according to claim 5, characterized in that, The remote transmission component is located at the liquid outlet position of the mixing tank and comprises a sampling bottle, a collection bottle, a sampling pipeline, a high-pressure gas bottle, a gas pipeline and a six-way valve and a three-way valve; the sampling bottle is connected to the liquid inlet of the six-way valve through the sampling pipeline; the sampling pipeline on one side of the sampling bottle is provided with a sample injection needle; the collection bottle is connected to the liquid outlet of the six-way valve through the sampling pipeline; the high-pressure gas bottle is connected to the inlet of the three-way valve through the gas pipeline; the outlet of the three-way valve is connected to the carrier gas inlet of the six-way valve; and the carrier gas outlet of the six-way valve is connected to the sample transmission pipeline.

7. The on-line sampling and detecting device for rare earth extraction separation according to claim 5, characterized in that, The six-way valve is internally provided with a quantitative ring, and the quantitative ring is located at the liquid inlet.

8. The on-line sampling and detecting device for rare earth extraction separation according to claim 7, characterized in that, The on-line analyzer is located at the end of the sample transmission pipeline, and the on-line analyzer adopts an inductively coupled plasma atomic emission spectrometer (ICP-OES) analyzer.

9. The on-line sampling and detecting device for rare earth extraction separation according to claim 1, characterized in that, The signal output end of the on-line analyzer is connected to the signal input end of a single-chip microcomputer through a signal line, and the single-chip microcomputer is connected to a computer at a remote end.

10. The on-line sampling and detecting device for rare earth extraction separation according to claim 9, characterized in that, ​

Images