Graphite tandem reaction device for rare earth ore sulfuric acid slurrying decomposition

Through the design of the graphite series reaction device, the problem of comprehensive utilization of rare earths, fluorine and phosphorus in the wet smelting of rare earth minerals was solved, the efficient decomposition of rare earth minerals and the resource recycling of valuable elements were achieved, and the continuity and controllability of the reaction process were improved.

CN223373183UActive Publication Date: 2025-09-23BAOTOU RESEARCH INSTITUTE OF RARE EARTHS +1
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Patent Information

Application Number
CN202422785927.2
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2024-11-15
Publication Date
2025-09-23
Estimated Expiration
2034-11-15

AI Technical Summary

Technical Problem

In the existing wet smelting technology of rare earth minerals, high-temperature acid and alkaline processes cannot achieve the comprehensive utilization of rare earths, fluorine and phosphorus, and the problems of material heating and continuous input and output have not been effectively solved.

Method used

A graphite series reaction device is used to achieve continuous mixing and heating of rare earth minerals and sulfuric acid solution through a series connection of a reactor, a stirring component and a heating component, thereby avoiding short circuiting and recovering the reaction gas through an exhaust port.

Benefits of technology

It achieves efficient decomposition of rare earth minerals and comprehensive utilization of valuable elements, improves the continuity and controllability of the reaction process, reduces the introduction of impurities, and improves the efficiency of resource recycling.

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Abstract

The utility model discloses a graphite tandem reaction device for rare earth ore sulfuric acid slurrying decomposition, which comprises a reactor, the reactor comprises a plurality of stages of reaction kettles which are sequentially connected in series, two sides of the reaction kettles are respectively provided with an overflow port and a feed port, and the feed port is positioned below the overflow port; the stirring assembly is mounted at the top end of the reaction kettle, and the output end of the stirring assembly extends into the reaction kettle; the heating assembly is mounted on the outer wall of the reaction kettle; wherein the top end of the first-stage reaction kettle is provided with a mineral feeding channel, a feeding hole of the first-stage reaction kettle is fixedly communicated with an acid material supply pipe, and an overflow hole of the last-stage reaction kettle is fixedly connected with a discharging pipe; an exhaust port is formed in the top of the reaction kettle. According to the utility model, the continuous overflow flow of slurry is realized by adopting a mode of connecting the reaction kettles in series, and minerals can enter the bottoms of the reaction kettles to be mixed with a sulfuric acid solution through the mineral feeding channel of the first-stage reaction kettle, so that the minerals are prevented from directly flowing out of the overflow ports of the reaction kettles to cause short circuit.
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Description

Technical Field

[0001] The utility model relates to the technical field of wet smelting of rare earth minerals, in particular to a graphite series reaction device used for sulfuric acid slurry decomposition of rare earth minerals. Background Art

[0002] The Bayan Obo mixed rare earth concentrate is composed of bastnaesite and monazite. Currently, the main industrialized rare earth concentrate decomposition technologies are concentrated sulfuric acid high-temperature roasting decomposition and concentrated alkaline solution atmospheric pressure decomposition. However, neither the high-temperature acid process nor the alkaline process can achieve the comprehensive utilization of the rare earths, fluorine, and phosphorus in the mineral.

[0003] In order to achieve the comprehensive utilization of valuable elements in mixed rare earth minerals, many domestic scientific researchers have developed new processes for rare earth mineral smelting. Patent CN109022838A discloses a method for processing fluorine-containing rare earth mineral particles. The fluorine-containing rare earth mineral particles are mixed with a sulfuric acid solution in a certain proportion, and then heated and insulated to perform a liquid-solid reaction. The tail gas is condensed and absorbed by the tail gas treatment system to obtain a fluorosilicic acid mixed product. The concentration of the sulfuric acid solution is 40-85wt%, and the reaction temperature is 100-180°C. This method can achieve rapid decomposition of fluorine-containing rare earth mineral particles, the reaction is easy to control, and the residual acid resources are recycled at the same time. However, problems such as how to achieve material heating and continuous input and output have not been solved.

[0004] Based on the above technical problems, the present invention provides a graphite series reaction device for sulfuric acid slurry decomposition of rare earth ores. Utility Model Content

[0005] The purpose of the utility model is to provide a graphite series reaction device for sulfuric acid slurry decomposition of rare earth ores, so as to solve the problems existing in the prior art.

[0006] To achieve the above-mentioned purpose, the present invention provides the following solution: The present invention provides a graphite series reaction device for sulfuric acid slurry decomposition of rare earth ores, comprising:

[0007] A reactor comprising several stages of reactors connected in series, with an overflow port and a feed port respectively provided on both sides of the reactor, the feed port being located below the overflow port, and the feed port of the reactor in the next stage being connected to the overflow port of the reactor in the previous stage via a connecting pipe;

[0008] A stirring assembly, the stirring assembly being mounted on the top of the reactor, and an output end of the stirring assembly extending into the reactor;

[0009] A heating component, the heating component being mounted on the outer wall of the reactor;

[0010] Wherein, a mineral feed channel is installed at the top of the first-stage reactor, and the feed port of the first-stage reactor is fixedly connected to the acid feed pipe, and the overflow port of the last-stage reactor is fixedly connected to the discharge pipe;

[0011] An exhaust port is provided on the top of the reactor.

[0012] According to the graphite series reaction device for sulfuric acid slurry decomposition of rare earth ores provided by the utility model, the stirring assembly includes a stirring motor fixedly connected to the top of the reactor, the output shaft of the stirring motor is fixedly connected to a stirring paddle, the stirring paddle extends into the reactor, and the axis of the stirring paddle is collinear with the axis of the reactor.

[0013] According to the graphite series reaction device for sulfuric acid slurry decomposition of rare earth ores provided by the utility model, the heating component includes a jacket fixedly connected to the reactor, a heating chamber is formed between the inner wall of the jacket and the outer wall of the reactor, the heating chamber is filled with a heating medium, a circulation pipe is fixedly connected to the outer wall of the jacket, the circulation pipe is fixedly connected to the heating chamber, and the connecting pipe passes through the jacket and is fixedly connected to the feed port.

[0014] According to the graphite series reaction device for sulfuric acid slurry decomposition of rare earth ores provided by the utility model, a sealing rubber ring is provided between the connecting pipe and the jacket.

[0015] According to the graphite series reaction device for sulfuric acid slurry decomposition of rare earth ores provided by the utility model, a temperature sensor is installed in the reactor.

[0016] According to the graphite series reaction device for sulfuric acid slurry decomposition of rare earth ores provided by the utility model, the exhaust port is fixedly connected to the exhaust gas recovery system through a delivery pipe.

[0017] The utility model discloses the following technical effects:

[0018] When the utility model is used, rare earth minerals are continuously and evenly added from the mineral feed channel of the first-stage reactor; sulfuric acid is configured into a solution of required concentration and continuously added from the feed port of the first-stage reactor at a stable flow rate; a stirring paddle with controllable rotation speed is used to evenly mix the two materials to form a slurry, the slurry flows upward from the bottom of the reactor until it flows out of the overflow port, and then enters the next-stage reactor from the feed port of the next-stage reactor through a connecting pipe, the gas in the reaction process is discharged through the exhaust port, and the reactor is heated by the heating component.

[0019] The utility model realizes the continuous overflow flow of slurry by connecting reactors in series. The mineral feed channel of the first-stage reactor allows the mineral to enter the bottom of the reactor and mix with the sulfuric acid solution, avoiding the mineral flowing out directly from the overflow port of the reactor and causing a short circuit. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the following briefly introduces the drawings required for use in the embodiments. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative work.

[0021] Figure 1 The utility model is a schematic structural diagram of a graphite series reaction device for sulfuric acid slurry decomposition of rare earth ores.

[0022] Among them, 1. Reactor; 2. Agitator; 3. Overflow port; 4. Feed port; 5. Mineral feed channel; 6. Acid feed pipe; 7. Discharge pipe; 8. Exhaust port; 9. Jacket. DETAILED DESCRIPTION

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

[0024] In order to make the above-mentioned objects, features and advantages of the present invention more obvious and easy to understand, the present invention is further described in detail below with reference to the accompanying drawings and specific implementation methods.

[0025] Reference Figure 1 The utility model provides a graphite series reaction device for sulfuric acid slurry decomposition of rare earth ores, comprising:

[0026] The reactor comprises several stages of reactors 1 connected in series, with overflow ports 3 and feed ports 4 respectively provided on both sides of the reactor 1. The feed port 4 is located below the overflow port 3. The feed port 4 of the reactor 1 at the next stage is connected to the overflow port 3 of the reactor 1 at the previous stage through a connecting pipe.

[0027] A stirring assembly is installed at the top of the reactor 1, and the output end of the stirring assembly extends into the reactor 1;

[0028] A heating component is installed on the outer wall of the reactor 1;

[0029] Among them, a mineral feeding channel 5 is installed on the top of the first-stage reactor 1, and the feed port 4 of the first-stage reactor 1 is fixedly connected to the acid feed pipe 6, and the overflow port 3 of the last-stage reactor 1 is fixedly connected to the discharge pipe 7;

[0030] An exhaust port 8 is provided on the top of the reactor 1 .

[0031] When the utility model is used, rare earth minerals are continuously and evenly added from the mineral feed channel 5 of the first-stage reactor 1; sulfuric acid is configured into a solution of required concentration and continuously added from the feed port 4 of the first-stage reactor 1 at a stable flow rate; a stirring paddle 2 with controllable rotation speed is used to mix the two materials evenly to form a slurry, the slurry flows upward from the bottom of the reactor 1 until it flows out of the overflow port 3, and then enters the next-stage reactor 1 from the feed port 4 of the next-stage reactor 1 through a connecting pipe, the gas during the reaction process is discharged through the exhaust port 8, and the reactor 1 is heated by the heating component.

[0032] The utility model realizes the continuous overflow flow of slurry by connecting reactors 1 in series. The mineral feed channel 5 of the first-stage reactor 1 allows the mineral to enter the bottom of the reactor 1 and mix with the sulfuric acid solution, avoiding the mineral from directly flowing out of the overflow port 3 of the reactor 1 and causing a short circuit.

[0033] To further optimize the solution, the stirring assembly includes a stirring motor fixedly connected to the top of the stirring kettle, the output shaft of the stirring motor is fixedly connected to a stirring paddle 2, the stirring paddle 2 extends into the stirring kettle, and the axis of the stirring paddle 2 is collinear with the axis of the reactor 1.

[0034] A further optimized solution is that the heating assembly includes a jacket 9 fixedly connected to the reactor 1, a heating chamber is formed between the inner wall of the jacket 9 and the outer wall of the reactor 1, the heating chamber is filled with a heating medium, a circulation pipe is fixedly connected to the outer wall of the jacket 9, the circulation pipe is fixedly connected to the heating chamber, and the connecting pipe passes through the jacket 9 and is fixedly connected to the feed port 4.

[0035] To further optimize the solution, a sealing rubber ring is provided between the connecting pipe and the jacket 9 .

[0036] To further optimize the solution, a temperature sensor is installed in the reactor 1.

[0037] To further optimize the solution, the exhaust port 8 is fixedly connected to the exhaust gas recovery system through a delivery pipe.

[0038] To further optimize the solution, the number of series stages of reactor 1 is determined according to the processing capacity. The larger the processing capacity, the more series stages there are.

[0039] To further optimize the solution, the reactor 1 is made of isostatically pressed graphite;

[0040] To further optimize the solution, the stirring paddle 2 is made of PFA sprayed steel;

[0041] In this embodiment, rare earth minerals are continuously and evenly added through the mineral feed channel 5 of the first-stage reactor 1; sulfuric acid is prepared into a solution of the desired concentration and continuously added at a steady flow rate through the feed port 4 of the first-stage reactor 1; a stirring paddle 2 with controllable speed is used to evenly mix the two materials to form a slurry, which flows upward from the bottom of the reactor 1 until it flows out of the overflow port 3, and then enters the next-stage reactor 1 through the feed port 4 of the next-stage reactor 1 through a connecting pipe. The device is connected in series, and the mixed slurry will flow out of the overflow port 3 of each stage of the reactor 1. The reaction process produces a mixed gas of hydrogen fluoride, silicon tetrafluoride, water vapor, and sulfuric acid mist, which will enter the tail gas recovery system through the exhaust port 8 of each stage of the reactor 1. After 1-4 hours of reaction in the multi-stage reactor 1, the mixed slurry is finally discharged from the overflow port 3 of the last stage of the reactor 1. Each stage of the reactor 1 is equipped with a jacket 9, which is heated by the jacket 9. Steam or thermal oil is introduced into the jacket 9 as a heating medium, which can heat the material to the required reaction temperature without introducing impurities into the reaction system. The number of series stages of the reactor 1 of this device is determined according to the processing capacity. The larger the processing capacity, the more series stages there are. The reactor 1 is made of isostatic graphite material, which has good thermal conductivity, corrosion resistance and wear resistance; the stirring paddle 2 is made of PFA sprayed steel material, and the connecting pipe is made of steel-lined PTFE material or static graphite material, which can not only make the stirring paddle 2 and the connecting pipe have higher strength, but also solve the corrosion and wear resistance problems of the stirring paddle 2 and the connecting pipe.

[0042] In the description of the present invention, it should be understood that the terms "longitudinal", "transverse", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside", etc., indicating the orientation or position relationship, are based on the orientation or position relationship shown in the accompanying drawings, and are only for the convenience of describing the present invention, and do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation. Therefore, they should not be understood as limitations on the present invention.

[0043] The embodiments described above are merely preferred embodiments of the present invention and are not intended to limit the scope of the present invention. Without departing from the spirit of the present invention, various modifications and improvements to the technical solutions of the present invention made by ordinary technicians in this field should fall within the scope of protection determined by the claims of the present invention.

Claims

1. A graphite series reaction device for sulfuric acid slurry decomposition of rare earth ores, characterized in that: include: A reactor, comprising a plurality of stages of reactors (1) connected in series, an overflow port (3) and a feed port (4) being respectively provided on both sides of the reactor (1), the feed port (4) being located below the overflow port (3), and the feed port (4) of the reactor (1) at the next stage being connected to the overflow port (3) of the reactor (1) at the previous stage via a connecting pipe; A stirring assembly, the stirring assembly being mounted on the top of the reactor (1), and the output end of the stirring assembly extending into the reactor (1); A heating component, the heating component being installed on the outer wall of the reactor (1); The top of the first-stage reactor (1) is provided with a mineral feed channel (5), the feed port (4) of the first-stage reactor (1) is fixedly connected to the acid feed pipe (6), and the overflow port (3) of the last-stage reactor (1) is fixedly connected to a discharge pipe (7); An exhaust port (8) is provided on the top of the reactor (1).

2. The graphite series reaction device for sulfuric acid slurry decomposition of rare earth ores according to claim 1, characterized in that: The stirring assembly comprises a stirring motor fixedly connected to the top of the reactor (1); the output shaft of the stirring motor is fixedly connected to a stirring paddle (2); the stirring paddle (2) extends into the reactor (1); the axis of the stirring paddle (2) is collinear with the axis of the reactor (1).

3. The graphite series reaction device for sulfuric acid slurry decomposition of rare earth ores according to claim 1, characterized in that: The heating assembly comprises a jacket (9) fixedly connected to the reactor (1), a heating chamber is formed between the inner wall of the jacket (9) and the outer wall of the reactor (1), the heating chamber is filled with a heating medium, a circulation pipe is fixedly connected to the outer wall of the jacket (9), the circulation pipe is fixedly connected to the heating chamber, and the connecting pipe passes through the jacket (9) and is fixedly connected to the feed port (4).

4. The graphite series reaction device for sulfuric acid slurry decomposition of rare earth ores according to claim 3, characterized in that: A sealing rubber ring is provided between the connecting pipe and the jacket (9).

5. The graphite series reaction device for sulfuric acid slurry decomposition of rare earth ores according to claim 1, characterized in that: A temperature sensor is installed in the reactor (1).

6. The graphite series reaction device for sulfuric acid slurry decomposition of rare earth ores according to claim 1, characterized in that: The exhaust port (8) is fixedly connected to the exhaust gas recovery system via a delivery pipe.

Citation Information

Patent Citations

  • Treatment method for fluorine-contained rare-earth mineral grains

    CN109022838A