Exchange resin separation device for measuring gallium in rare earth ore

By designing an exchange resin separation device for gallium measurement in rare earth ore, using exchange separation of anionic resin and hydrochloric acid rinsing, the double charge interference problem in gallium measurement and the environmental and health hazards of organic reagents are solved, achieving high efficiency , accurate gallium measurement.

CN222446553UActive Publication Date: 2025-02-11CHINA NUCLEAR EAST CHINA GEOLOGY & MINERAL TECH CO LTD
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Patent Information

Application Number
CN202421233944.9
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2024-06-01
Publication Date
2025-02-11
Estimated Expiration
2034-06-01

AI Technical Summary

Technical Problem

The prior art has double charge interference problems in determining gallium in rare earth ores, and the extraction and separation method of organic reagents is not good for the environment and human health.

Method used

An exchange resin separation device is designed, including a separation support frame, a partition plate, a resin separation device, a separation column, a liquid storage cup, a column, a resin layer, a filter pad and an overflow tube, and is separated by anionic resin and Hydrochloric acid rinse to achieve accurate determination of gallium.

Benefits of technology

This device effectively solves the problem of double charge interference in gallium measurement, improves measurement accuracy and efficiency, reduces manpower and material consumption, and reduces harm to the environment and human health.

✦ Generated by Eureka AI based on patent content.

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Abstract

The utility model discloses an exchange resin separation device for measuring gallium in rare earth ore, which comprises separation support frames, a partition plate A and a partition plate B are mounted between the separation support frames, a resin separation device is connected between the partition plate A and the partition plate B in a penetrating manner, a separation column is mounted at the top of the partition plate A, and a separation column is mounted at the bottom of the separation column. The bottom of the separation column is connected with a liquid storage cup, the bottom of the liquid storage cup is provided with a column body, the column body is internally provided with a resin layer, the bottom of the resin layer is provided with a filter padding, and one side of the column body is connected with an overflow pipe. The exchange resin separation device for measuring the gallium in the rare earth ore comprises a separation column and a separation column bracket, the separation column is composed of a liquid storage cup, a column body, a resin layer, a filter padding and an overflow pipe, and the liquid storage cup is firstly connected with the column body and used for temporarily bearing a solution to be separated.
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Description

Technical Field

[0001] The utility model relates to the field of rare earth resource separation, in particular to an exchange resin separation device used for measuring gallium in rare earth ores. Background Art

[0002] Gallium has an abundance of 1.5×10-3% in the earth's crust. It is a rare dispersed element and can be used as semiconductor materials, fireproof signal materials, and medical equipment materials. Therefore, with the continuous expansion of the use of gallium, how to measure trace amounts of gallium becomes particularly important. The determination of gallium in rare earth ores by inductively coupled plasma-mass spectrometry is interfered by the double charge of rare earth elements, such as 69Ga is interfered by 138Ce2+, and 71Ga is interfered by 142Ce2+ and 142Nd2+. A certain matrix separation is required for accurate determination.

[0003] Currently, the main method for enriching gallium and separating it from coexisting elements is extraction and separation through organic reagents. The separation efficiency is relatively high, but the use of organic reagents can have adverse effects on the environment and human health.

[0004] In view of this, research and improvement are carried out on the existing problems, and an exchange resin separation device for measuring gallium in rare earth ores is provided. This equipment mainly changes the previous defects of scattered placement and the inability of test operators to effectively control it. It can effectively save manpower and material resources, improve test accuracy, and greatly improve test efficiency. The purpose is to solve problems and improve practical value through this technology. Utility Model Content

[0005] The utility model aims to solve the shortcomings in the prior art and proposes an exchange resin separation device for measuring gallium in rare earth ores.

[0006] In order to achieve the above-mentioned purpose, the utility model adopts the following technical scheme: an exchange resin separation device for measuring gallium in rare earth ores, comprising a separation support frame, between which a partition plate A and a partition plate B are installed, a resin separation device is connected through the partition plate A and the partition plate B, a separation column is installed on the top of the partition plate A, a liquid storage cup is connected to the bottom of the separation column, a column is installed at the bottom of the liquid storage cup, a resin layer is arranged inside the column, a filter pad is installed at the bottom of the resin layer, and an overflow pipe is connected to one side of the column.

[0007] As a further description of the above technical solution:

[0008] The height of the separation support frame is 200 mm, and the partition plate A and the partition plate B are fixedly installed between the separation support frames. The sizes of the partition plate A and the partition plate B are the same, and the distance between the partition plate A and the partition plate B is 80 mm.

[0009] As a further description of the above technical solution:

[0010] The distance between the partition plate A and the top of the separation support frame is 70 mm, and the distance between the partition plate B and the bottom of the separation support frame is 50 mm.

[0011] As a further description of the above technical solution:

[0012] The column is detachably installed between the partition plate A and the partition plate B. There are several columns, and the resin layer is fixedly installed on the inner wall of the column.

[0013] As a further description of the above technical solution:

[0014] The liquid storage cup is integrally connected to the top of the column, the separation column is integrally connected to the top of the liquid storage cup, the separation column has a diameter of 20 mm, and the diameter of the cross section at the connection between the column and the liquid storage cup is 8 mm.

[0015] As a further description of the above technical solution:

[0016] The filter pad is fixedly installed at the bottom of the column, the overflow pipe is fixedly connected to the column through the filter pad, and the overflow pipe is communicated with the column.

[0017] The utility model has the following beneficial effects:

[0018] In the utility model, the exchange resin separation device for measuring gallium in rare earth ores includes a separation column and a separation column bracket. The separation column is composed of a liquid storage cup, a column, a resin layer, a filter pad and an overflow pipe, wherein the liquid storage cup is first connected to the column, and the liquid storage cup is used to temporarily receive the solution to be separated; the column and the resin layer are used to exchange and adsorb the solution to be separated, the filter pad is used to fix the resin layer, and the overflow pipe is used for the outflow of the solution. After the pre-treatment of the ore dissolution is completed, the rare earth ore is transferred to the liquid storage cup, and the column equipped with an anion resin is exchanged and separated. After the liquid surface of the solution is flush with the resin layer, it is eluted with hydrochloric acid, and the elution liquid is discarded (the rare earth element is washed away). At this time, the gallium element is adsorbed in the separation column, and then the gallium is eluted with deionized water. The eluent flowing out of the overflow pipe is received by a 25mL volumetric flask, and the volume is constant. Finally, the eluent is measured by an inductively coupled plasma mass spectrometer to achieve accurate determination of gallium in the rare earth ore. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] Figure 1 This is a schematic diagram of the overall structure of an exchange resin separation device for measuring gallium in rare earth ores proposed by the utility model;

[0020] Figure 2The utility model discloses a schematic structural diagram of a column of an exchange resin separation device for measuring gallium in rare earth ores.

[0021] Legend:

[0022] 1. Separation support frame; 2. Partition plate A; 3. Partition plate B; 4. Separation column; 5. Liquid storage cup; 6. Resin layer; 7. Column; 8. Filter pad; 9. Overflow pipe. DETAILED DESCRIPTION

[0023] The following will be combined with the drawings in the embodiments of the utility model to clearly and completely describe the technical solutions in the embodiments of the utility model. Obviously, the described embodiments are only part of the embodiments of the utility model, not all of the embodiments. Based on the embodiments in the utility model, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the utility model.

[0024] In the description of the present utility model, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inside", "outside" and the like indicate positions or positional relationships based on the positions or positional relationships shown in the drawings, which are only for the convenience of describing the present utility model and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific position, be constructed and operated in a specific position, and therefore cannot be understood as a limitation on the present utility model; the terms "first", "second" and "third" are only used for descriptive purposes, and cannot be understood as indicating or implying relative importance. In addition, unless otherwise clearly specified and limited, the terms "installed", "connected" and "connected" should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection, or it can be an indirect connection through an intermediate medium, or it can be a communication between the two elements. For ordinary technicians in this field, the specific meanings of the above terms in the present utility model can be understood according to specific circumstances.

[0025] Reference Figure 1-2 The utility model provides an embodiment: an exchange resin separation device for measuring gallium in rare earth ores, comprising a separation support frame 1, a partition plate A2 and a partition plate B3 are installed between the separation support frame 1, a resin separation device is connected through the partition plate A2 and the partition plate B3, a separation column 4 is installed on the top of the partition plate A2, a liquid storage cup 5 is connected to the bottom of the separation column 4, a column 7 is installed at the bottom of the liquid storage cup 5, a resin layer 6 is arranged inside the column 7, a filter pad 8 is installed at the bottom of the resin layer 6, and an overflow pipe 9 is connected to one side of the column 7.

[0026] In the utility model, the height of the separation support frame 1 is 200 mm, the partition plate A2 and the partition plate B3 are fixedly installed between the separation support frame 1, the sizes of the partition plate A2 and the partition plate B3 are the same, the distance between the partition plate A2 and the partition plate B3 is 80 mm, and the partition plate A2 and the partition plate B3 are made of wear-resistant and corrosion-resistant materials to ensure their stability and durability during use.

[0027] Furthermore, the distance between the partition plate A2 and the top of the separation support frame 1 is 70 mm, and the distance between the partition plate B3 and the bottom of the separation support frame 1 is 50 mm.

[0028] Furthermore, the column 7 is detachably installed between the partition plate A2 and the partition plate B3 , the number of the column 7 is several, and the resin layer 6 is fixedly installed on the inner wall of the column 7 .

[0029] Furthermore, the liquid storage cup 5 is integrally connected to the top of the column 7, the separation column 4 is integrally connected to the top of the liquid storage cup 5, the separation column 4 has a diameter of 20 mm, and the diameter of the cross section at the connection between the column 7 and the liquid storage cup 5 is 8 mm.

[0030] Furthermore, the filter pad 8 is fixedly installed at the bottom of the column 7 , and the overflow pipe 9 is fixedly connected to the column 7 through the filter pad 8 , and the overflow pipe 9 is communicated with the column 7 .

[0031] Specifically, in order to improve the use effect and stability of the resin layer 6, the material of the resin layer 6 is selected from high-performance ion exchange resin, which has excellent adsorption and separation properties and can effectively remove impurities and harmful substances in the liquid. At the same time, the thickness and distribution of the resin layer 6 are carefully designed to ensure that it can fully play its role during use and maintain long-term stability.

[0032] Working principle and usage process:

[0033] After the rare earth ore sample is pre-treated by dissolution, 10 mL of the solution is taken and passed through an anion exchange resin separation device to separate the rare earth matrix and the gallium element. The separated solution is measured by an inductively coupled plasma mass spectrometer to achieve accurate determination of gallium in the rare earth ore.

[0034] Experimental steps: Accurately weigh 0.1g (accurate to 0.01mg) of sample into the inner tank of the closed sample dissolver, add 2mL of hydrofluoric acid and 1mL of concentrated nitric acid, seal, put the sample dissolver into the oven, bake at 180℃ for 24h, take out the inner tank and cool it to room temperature, add 0.5mL of sulfuric acid, place it on the hot plate and heat it until the sulfuric acid smoke is gone, add 5mL of 4mol / L hydrochloric acid, heat and extract, cool it, and make up the volume with 4mol / L hydrochloric acid. Accurately take 10mL of digestion solution into the exchange column storage cup, wait for the liquid level to drop to the same level as the resin layer, wash it with 20mL of 4mol / L hydrochloric acid for 5 times, wash the rare earth, and then elute gallium with 16mL of deionized water, use a 25mL volumetric flask to receive the eluent, add water to the scale line, and wait for measurement. At the same time, prepare a blank solution in parallel with the above steps.

[0035] The device can process 6 (or more) rare earth ore samples at a time, and the life of the column anion resin elution test under this size is more than 30 times. It is more suitable for the separation-ICP-MS determination test of gallium in large quantities of rare earth ore samples.

[0036] Finally, it should be noted that the above is only a preferred embodiment of the present invention and is not intended to limit the present invention. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art can still modify the technical solutions described in the aforementioned embodiments or make equivalent substitutions for some of the technical features therein. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. An exchange resin separation device for measuring gallium in rare earth ores, comprising a separation support frame (1), characterized in that: A partition plate A (2) and a partition plate B (3) are installed between the separation support frame (1); a resin separation device is connected through the partition plate A (2) and the partition plate B (3); a separation column (4) is installed on the top of the partition plate A (2); a liquid storage cup (5) is connected to the bottom of the separation column (4); a column (7) is installed on the bottom of the liquid storage cup (5); a resin layer (6) is arranged inside the column (7); a filter pad (8) is installed at the bottom of the resin layer (6); and an overflow pipe (9) is connected to one side of the column (7).

2. The exchange resin separation device for measuring gallium in rare earth ores according to claim 1, characterized in that: The height of the separation support frame (1) is 200 mm, and the partition plate A (2) and the partition plate B (3) are fixedly installed between the separation support frame (1). The sizes of the partition plate A (2) and the partition plate B (3) are the same, and the distance between the partition plate A (2) and the partition plate B (3) is 80 mm.

3. The exchange resin separation device for measuring gallium in rare earth ores according to claim 1, characterized in that: The distance between the partition plate A (2) and the top of the separation support frame (1) is 70 mm, and the distance between the partition plate B (3) and the bottom of the separation support frame (1) is 50 mm.

4. The exchange resin separation device for measuring gallium in rare earth ores according to claim 1, characterized in that: The column (7) is detachably mounted between the partition plate A (2) and the partition plate B (3), the number of the column (7) is several, and the resin layer (6) is fixedly mounted on the inner wall of the column (7).

5. The exchange resin separation device for measuring gallium in rare earth ores according to claim 1, characterized in that: The liquid storage cup (5) is integrally connected to the top of the column (7), and the separation column (4) is integrally connected to the top of the liquid storage cup (5). The diameter of the separation column (4) is 20 mm, and the diameter of the cross section at the connection between the column (7) and the liquid storage cup (5) is 8 mm.

6. The exchange resin separation device for measuring gallium in rare earth ores according to claim 1, characterized in that: The filter pad (8) is fixedly mounted at the bottom of the column (7), the overflow pipe (9) is fixedly connected to the column (7) via the filter pad (8), and the overflow pipe (9) is communicated with the column (7).