A device and process for closed-circuit extraction of beryllium from siliceous minerals
Through the device for siliceous mineral closed-circuit extraction of beryllium, microwave drying, Raymond milling, plasma gasification and carbon thermal reduction, the problems of many processes, low recovery rates and environmental pollution in the existing processes are solved, and high efficiency is achieved. Environmentally friendly beryllium extraction and recycling, suitable for high-demand fields such as the nuclear industry.
Patent Information
- Application Number
- CN202011042286.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2020-09-28
- Publication Date
- 2025-01-10
- Estimated Expiration
- 2040-09-28
AI Technical Summary
In the existing industrial production methods, the extraction process of beryllium is long, the process is many, the equipment is complex, the beryllium oxide recovery rate is low, the product quality is unstable, the waste water volume is large, the waste residue is large, and the environmental pollution is serious, making it difficult to meet the high requirements of the nuclear industry and other industries. .
Devices that use siliceous mineral closed circuit extraction beryllium, including microwave dryers, Raymond mills, aggregates, dust collectors, frefluxate mixers, plasma gasification and melting furnaces, crushers, circulating leaching tanks and microwave carbon heat The reduction furnace achieves efficient extraction and recovery of beryllium through steps such as freflux mixing, plasma gasification and smelting, precipitation purification, cyclic leaching and carbon thermal reduction.
It improves the recovery rate of beryllium, saves energy and is environmentally friendly, and has achieved zero emissions of gas, liquid and solids. It has stable product quality and wide adaptability, reducing environmental pollution.
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Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of metallurgy, and in particular relates to a device for extracting beryllium from siliceous minerals in a closed circuit and an extraction method thereof. Background Art
[0002] Beryllium is a light rare metal with special properties. Some of its properties, especially nuclear properties and physical properties, cannot be replaced by any other metal material. Beryllium has a high melting point of about 1284°C, which is nearly 1 times higher than aluminum and magnesium. Beryllium has a high specific strength, which exceeds that of titanium alloys and aluminum alloys, and is 4 times greater than steel, and it maintains its strength at high temperatures. Beryllium also has a high specific elastic modulus (i.e. elastic modulus / density), which is 6 times that of stainless steel. Beryllium has a small atomic weight, a small neutron capture cross section, and a particularly high scattering cross section. Therefore, beryllium is very suitable as one of the special engineering materials required by the nuclear industry.
[0003] In the emerging fields, the nuclear technology field firstly applied metal beryllium as a structural material. Metal beryllium is widely used as a neutron moderator and reflector in nuclear reactors, especially in test reactors and nuclear weapons. It may also be used as a beryllium target for generating microparticles in nuclear medical devices, a coating material for plasma fusion and confinement rings in thermonuclear fusion devices, etc. It is used as a structural material for a variety of space vehicles, including base frames, beams, fixed trusses, front frames, rotating and derotation platforms used in satellites and spacecrafts, base frames for solar panels for satellites, etc. Beryllium plates have also been used to make satellite skins, missile transfer shells, honeycomb panels, instrument mounting panels, and major components such as wing boxes and tail rudders of aircraft structures. The application of beryllium in space structures reduces the weight of components by 20-50%, thereby saving a lot of investment in launch and use, and the processing and performance of beryllium components have not had major problems in these application tests. Mainly because beryllium has excellent specific stiffness, good dimensional stability and thermal expansion compatibility, many missiles, aircraft, submarines, space shuttles and even long-distance civil aircraft use inertial navigation systems equipped with beryllium precision instrument components, which greatly improves navigation accuracy. Beryllium has become the basic structural material for manufacturing gyroscopes, accelerometers, gimbals and platforms. Other precision instrument components made of beryllium include substrate trackers, inertial wheels, reaction wheels, housings of proportional calculators, housings of space cameras, rotating mirrors of high-speed cameras, swinging scanning mirrors for satellites, and applications in large-diameter cylindrical high-grazing telescopes and small-diameter X-ray microscopes, lightweight laser optical systems, such as laser communications, high-speed fax systems, etc. The fields that use beryllium's excellent thermal properties include aircraft brake discs, rocket engine propulsion chambers, etc., which use beryllium as a heat-absorbing material in the spacecraft nose cone, radiator, black box, etc., which also have load functions in the thermal system. Beryllium has become an indispensable and important industrial material in national economic construction.
[0004] The conventional industrial production methods are: (i) one acid and one base method, that is, sulfuric acid is first used to make beryllium into an ionic state and enter the solution, and then alkali is used to precipitate the ionic beryllium in the solution in the form of hydroxide. (ii) one acid and two base method, first use sodium carbonate and minerals to melt into beryllium glass, leaching with sulfuric acid, precipitating with ammonia water, dissolving with sodium hydroxide, hydrolyzing to obtain beryllium hydroxide, and calcining to obtain beryllium oxide. This process has a long process flow, many steps, complex equipment, corresponding large unnamed losses, low beryllium oxide recovery rate, unstable product quality, large amount of wastewater, large amount of waste residue, narrow adaptability, and great environmental pollution. Summary of the invention
[0005] The first object of the present invention is to provide a device for closed-circuit extraction of beryllium from siliceous minerals.
[0006] The second object of the present invention is to provide a process for extracting beryllium using a closed-loop device for extracting beryllium from siliceous minerals.
[0007] The first object of the present invention is achieved in this way, comprising a microwave dryer I, a Raymond mill I, a collector and a dust collector I, wherein the Raymond mill I and the collector are sequentially arranged downstream of the microwave dryer I, the dust outlet of the collector is connected to the dust collector I, the material outlet is connected to the ferrofluoride mixer I, the material outlet of the ferrofluoride mixer I is connected to the plasma gasification melting furnace, the material outlet of the plasma gasification melting furnace is connected to the crusher II, the crusher II is sequentially connected to the Raymond mill II, the storage tank, the dust collector IV, the gas-liquid mixer II, the circulating leaching tank, the belt vacuum filter I, the sedimentation tank and the belt vacuum filter II, the sediment outlet of the belt vacuum filter II is connected to the drying tower II, the drying tower II is connected to the carbon material mixer, and the carbon material mixer is connected to the microwave carbon thermal reduction furnace.
[0008] The second object of the present invention is achieved by comprising the steps of:
[0009] Step 1: After the siliceous minerals are crushed by crusher I, they are sent to microwave dryer I for drying. The dried materials are sent to the conveyor and then to the feeder for quantitative feeding into Raymond mill I for crushing and collected by the collector. The dust generated by Raymond mill I and the collector is recovered by dust collector I and discharged into clean air. The materials in the collector and the dust collected by dust collector I are sent to ferrofluoride mixer I together, and the materials and drugs are mixed at a ratio of 5:4.5;
[0010] Step 2: After being mixed in the ferrofluoride mixer I, it is sent to a plasma gasification melting furnace for smelting into beryllium glass. The smoke from the plasma gasification melting furnace is separated by a dust collector II. The smoke is sent to a gas-liquid mixer I for mixing, and then precipitated and purified with sodium hydroxide or sodium carbonate in an air purifier I to meet environmental standards for discharge. The precipitate from the air purifier I is sent to a drying tower I for drying and collected by a dust collector III. The exhaust gas is sent to a gas-liquid mixer I for mixing and then sent to an air purifier I for purification. The fine dust collected by the dust collectors II and III is sent back to the ferrofluoride mixer I for mixing and reuse.
[0011] Step 3: After the beryllium glass melted in the plasma gasification melting furnace is cooled, it is sent to the crusher II for crushing, and then sent to the unloading machine for even distribution and sent to the Raymond mill II for grinding to 0.050 mm and sent to the storage tank. The dust is collected by the dust collector IV, and the waste gas is sent to the air-liquid mixer II for mixing and then sent to the air purifier II for purification with sodium hydroxide or sodium carbonate. The waste gas meets the environmental protection standard for discharge, and the sediment, the material in the storage tank and the dust in the dust collector IV are sent to the circulating leaching tank together with the material in the storage tank and the dust in the dust collector IV to leach the beryllium with pure water at room temperature;
[0012] Step 4: After checking the leachate in the circulating leaching tank and confirming that beryllium has been completely leached, open the valve of the circulating leaching tank and send it to the belt vacuum filter I for filtration. The liquid is sent to the beryllium hydroxide constant temperature precipitation tank and stirred with a circulating pump. The pH value is adjusted to 10.5-11 with sodium hydroxide. The stirring is stopped and the liquid temperature is controlled to degrees Celsius. The temperature is kept for 10-30 minutes until the precipitation is complete. The reaction materials are sent to the belt vacuum filter II for filtration. The liquid is sent to the ferrofluoride synthesizer II for reuse. The precipitation The product is sent to the drying tower II for dehydration and drying. After drying, it is collected by the dust collector V and sent to the carbon material mixer to mix beryllium hydroxide with electrode-grade high-purity graphite in a ratio of 1:0.5~1. After mixing, it is sent to the microwave carbon thermal reduction furnace for reduction to metal beryllium product, which is collected by the metal beryllium product recovery device. The electrode-grade high-purity graphite is recycled. The smoke from the microwave carbon thermal reduction furnace is sent to the gas-liquid mixer III together with the water vapor from the drying tower II. Calcium oxide is used to absorb carbon dioxide in the air purifier III to become calcium carbonate by-product.
[0013] Beneficial effects of the present invention: beryllium salts and oxides have certain toxicity and cannot leak during the production process. The process of the present invention has high recovery rate, drug recycling, energy saving, safety, environmental protection, and zero gas, liquid, and solid emissions. BRIEF DESCRIPTION OF THE DRAWINGS
[0014] Figure 1 It is a schematic diagram of the overall structure of the present invention;
[0015] In the figure: 1-crusher I, 2-microwave dryer I, 3-microwave power supply, 4-controller, 5-microwave generator, 6-conveyor, 7-feeder I, 8-Raymond mill I, 9-collector, 10-dust collector I, 11-ferrofluoride mixer I, 12-plasma gasification melting furnace, 13-dust collector II, 14-gas-liquid mixer I, 15-air purifier I, 16-drying tower I, 17-dust collector III, 18-crusher II, 19-feeder II, 20-Raymond mill II, 21-storage tank, 22-dust collector IV, 23-gas-liquid Mixer II, 24-air purifier II, 25-circulating leaching tank, 26-belt vacuum filter I, 27-sedimentation tank, 28-belt vacuum filter II, 29-drying tower II, 30-dust collector V, 31-carbon material mixer, 32-microwave carbon thermal reduction furnace, 33-metal beryllium product recovery device, 34-gas-liquid mixer III, 35-air purifier III, 36-ultrasonic cleaning machine, 37-silicon dioxide recovery device, 38-ferrofluoride synthesizer II, 39-belt vacuum filter III, 40-drying tower III, 41-dust collector VI. DETAILED DESCRIPTION
[0016] The present invention is further described below in conjunction with the accompanying drawings, but the present invention is not limited in any way. Any changes or improvements made based on the teachings of the present invention belong to the protection scope of the present invention.
[0017] like Figure 1 As shown, a closed-loop device for extracting beryllium from siliceous minerals comprises a microwave dryer Ⅰ2, a Raymond mill Ⅰ8, a collector 9 and a dust collector Ⅰ10. Raymond mill Ⅰ8 and collector 9 are sequentially arranged downstream of the microwave dryer Ⅰ2. The dust outlet of the collector 9 is connected to the dust collector Ⅰ10, and the material outlet is connected to the ferrofluoride mixer Ⅰ11. The material outlet of the ferrofluoride mixer Ⅰ11 is connected to the plasma gasification melting furnace 12. The material outlet of the plasma gasification melting furnace 12 is connected to the crusher Ⅱ18. The crusher Ⅱ18 is sequentially connected to the Raymond mill Ⅱ20, the storage tank 21, the dust collector Ⅳ22, the gas-liquid mixer Ⅱ23, the circulating leaching tank 25, the belt vacuum filter Ⅰ26, the sedimentation tank 27 and the belt vacuum filter Ⅱ28. The sediment outlet of the belt vacuum filter Ⅱ28 is connected to the drying tower Ⅱ29, the drying tower Ⅱ29 is connected to the carbon material mixer 31, and the carbon material mixer 31 is connected to the microwave carbon thermal reduction furnace 32.
[0018] The smoke outlet of the plasma gasification melting furnace 12 is connected to the dust collector II13, the smoke outlet of the dust collector II13 is connected to the gas-liquid mixer I14, the gas-liquid mixer I14 is connected to the air purifier I15, the sediment outlet of the air purifier I15 is connected to the drying tower I16, the drying tower I16 is connected to the dust collector III17, and the exhaust gas outlet of the dust collector III17 is connected to the gas-liquid mixer I14.
[0019] The fine dust outlets of the dust collectors III 17 and II 13 are connected to the ferrofluorite mixer I 11 .
[0020] The liquid outlet of the belt vacuum filter II 28 is connected to the ferrofluoride synthesizer II 38, the ferrofluoride synthesizer II 38 is sequentially connected to the belt vacuum filter III 39, the drying tower III 40 and the dust collector VI 41, and the dust outlet of the dust collector VI 41 is connected to the material inlet of the ferrofluoride synthesizer II 38 and / or the material inlet of the ferrofluoride mixer I 11.
[0021] The drying tower II 29 is connected to the dust collector V 30 , the dust collector V 30 is connected to the carbon material mixer 31 , the water vapor outlet of the drying tower II 29 is connected to the gas-liquid mixer III 34 , and the gas-liquid mixer III 34 is connected to the air purifier III 35 .
[0022] The solid outlet of the belt vacuum filter I 26 is connected to an ultrasonic cleaning machine 36 .
[0023] A loop structure is formed between the gas-liquid mixer II 23 and the air purifier II 24 via a circulation pump.
[0024] The top of the circulating leaching tank 25 is a material inlet, and the bottom is a material outlet. A loop structure is formed between the inlet and the outlet through a circulating pump. A valve is set on the material channel between the circulating leaching tank 25 and the belt vacuum filter I26.
[0025] A loop structure is formed between the gas-liquid mixer III 34 and the air purifier III 35 via a circulation pump.
[0026] The dust outlet of the dust collector Ⅰ10 is connected to the ferrofluorite mixer Ⅰ11.
[0027] The material inlet of the microwave dryer Ⅰ2 is connected to the crusher Ⅰ1.
[0028] The material outlet of the microwave dryer Ⅰ2 is sequentially connected to a conveyor 6 and a feeder 7, and the feeder 7 is connected to a Raymond mill 8.
[0029] A process for extracting beryllium using a closed-circuit device for extracting beryllium from siliceous minerals comprises the following steps:
[0030] Step 1: After the siliceous mineral is crushed by the crusher Ⅰ1, it is sent to the microwave dryer Ⅰ2 for drying. The dried material is sent to the conveyor 6 and sent to the feeder 7 for quantitative feeding into the Raymond mill Ⅰ8 for crushing and collected by the collector 9. The dust generated by the Raymond mill Ⅰ8 and the collector 9 is recovered by the dust collector Ⅰ10 and discharged into clean air. The material in the collector 9 and the dust collected by the dust collector Ⅰ10 are sent to the ferrofluoride mixer Ⅰ11 together, and the material and the drug are mixed at a ratio of 5:4.5;
[0031] Step 2: After being mixed in the ferrofluoride mixer Ⅰ11, it is sent to the plasma gasification melting furnace 12 for smelting into beryllium glass. The smoke from the plasma gasification melting furnace 12 is separated by the dust collector Ⅱ13. The smoke is sent to the gas-liquid mixer Ⅰ14 for mixing, and then precipitated and purified with sodium hydroxide or sodium carbonate in the air purifier Ⅰ15 to meet the environmental protection standard for discharge. The precipitate from the air purifier Ⅰ15 is sent to the drying tower Ⅰ16 for drying and collected by the dust collector Ⅲ17. The exhaust gas is sent to the gas-liquid mixer Ⅰ14 for mixing and then sent to the air purifier Ⅰ15 for purification. The fine dust collected by the dust collectors Ⅱ13 and Ⅲ17 is returned to the ferrofluoride mixer Ⅰ11 for mixing and reuse.
[0032] Step 3: The beryllium glass melted by the plasma gasification melting furnace 12 is cooled and sent to the crusher II 18 for crushing, and then sent to the unloader 19 for balanced delivery to the Raymond mill II 20 for grinding to 0.050 mm and sent to the storage tank 21. The fine dust is collected by the dust collector IV 22, and the waste gas is sent to the air-liquid mixer II 23 for mixing and then sent to the air purifier II 24 for purification with sodium hydroxide or sodium carbonate. The waste gas meets the environmental protection standard for discharge, and the precipitate, the material in the storage tank 21 and the fine dust in the dust collector IV 22 are sent to the circulating leaching tank 25 together with the material in the storage tank 21 and the fine dust in the dust collector IV 22 to leach the beryllium with pure water at room temperature;
[0033] Step 4: After checking the leachate in the circulating leaching tank 25 and confirming that beryllium has been completely leached, the valve of the circulating leaching tank 25 is opened and sent to the belt vacuum filter I 26 for filtration. The liquid is sent to the beryllium hydroxide constant temperature precipitation tank 27, stirred with a circulating pump, and the pH value is adjusted to 10.5-11 with sodium hydroxide. The stirring is stopped, and the liquid temperature is controlled to 80-100 degrees Celsius. The temperature is kept for 10-30 minutes until the precipitation is complete. The reaction material is sent to the belt vacuum filter II 28 for filtration, and the liquid is sent to the ferrofluoride synthesizer II 38 for reuse. The precipitation The product is sent to the drying tower II 29 for dehydration and drying. After drying, it is collected by the dust collector V 30 and sent to the carbon material mixer 31 for mixing beryllium hydroxide with electrode-grade high-purity graphite in a ratio of 1:0.5~1. After mixing, it is sent to the microwave carbon thermal reduction furnace 32 for reduction into metallic beryllium product, which is collected by the metallic beryllium product recovery device 33. The electrode-grade high-purity graphite is recycled. The smoke from the microwave carbon thermal reduction furnace 32 is sent to the gas-liquid mixer III 34 together with the water vapor from the drying tower II 29, and is absorbed by calcium oxide in the air purifier III 35 to become a calcium carbonate by-product.
[0034] The solid filtered out by the belt vacuum filter I26 in step 4 is cleaned by an ultrasonic cleaner 36, and the solid silicon dioxide is collected by a silicon dioxide recovery device 37. The liquid is sent to a ferrofluoride synthesizer II38, sodium fluoride is added to form a saturated solution, and then a ferric chloride solution is added dropwise to complete precipitation. The solution is filtered by a belt vacuum filter III39, and the liquid is recycled. The precipitate is sent to a drying tower III40 for drying, and the dried product is collected by a dust collector VI41 and returned to the ferrofluoride mixer I11 for re-dosing. The dust in the dust collector VI41 is returned to the ferrofluoride synthesizer II38 for recycling.
[0035] In the present invention:
[0036] 1. Preparation of Sodium Ferrofluoride
[0037] Drop the concentrated FeCl3 solution into the saturated NaF solution, filter and wash to obtain white Na3FeF6;
[0038] 6NaF+ FeCl3 ⇄ Na3FeF6+3NaCl
[0039] 2. Preparation of Beryllium Glass
[0040] The 0.074mm ore sample is fully mixed with Na3FeF6 in proportion, sent to a plasma furnace for melting into beryllium glass, cooled and ground to 0.074mm for later use;
[0041] 3Beo+ 2 Na3FeF6 ⇄ 3Na2BeF6+Fe2o3
[0042] 3. Leaching
[0043] Beryllium glass fine powder and deionized water are stirred at a solid-liquid ratio of 1:5 and leached at room temperature for 30-60 minutes. Sampling is performed midway to detect complete leaching as the end point.
[0044] 4. Precipitation of Beryllium Hydroxide
[0045] After leaching, the filtrate is vacuum filtered, heated and boiled to remove iron, vacuum filtered, and the clean liquid is adjusted to pH 10.5-11 with sodium hydroxide, heated to 90 degrees Celsius in a water bath to precipitate beryllium hydroxide, which is vacuum filtered, washed, and dried to obtain beryllium hydroxide, which is then sent to a microwave carbon hot furnace to be reduced to metallic beryllium.
[0046] 5. Filtrate recovery and recycling
[0047] The filtrate is adjusted to slightly acidic with NaF, and concentrated Fe2(SO4)3 or FeCl3 solution is dropped into the filtrate to obtain Na3FeF6.
[0048] Example 1
[0049] Since the minerals are mined and piled in the open air, there is a certain amount of surface water. After being crushed by crusher Ⅰ1, they are sent to microwave dryer Ⅰ2 for drying. The microwave power supply 3 of microwave dryer Ⅰ2 adjusts the appropriate power to microwave generator 5 through controller 4. Microwave generator 5 provides microwave energy to microwave dryer Ⅰ2 for material drying. The dried materials are sent to conveyor 6 and then to feeder 7 for quantitative feeding into Raymond mill Ⅰ8 for crushing to 0.074mm and collected by aggregate 9. The dust generated by Raymond mill Ⅰ8 and aggregate 9 is recovered by dust collector Ⅰ10 and discharged into clean air. The materials in aggregate 9 and the dust collected by dust collector Ⅰ10 are sent to ferrofluoride mixer Ⅰ11 together, and the materials are mixed with the drug at a ratio of 5:4.5.
[0050] After being mixed in the ferrofluorite mixer Ⅰ11, it is sent to the plasma gasification melting furnace 12 for smelting into beryllium glass. The smoke from the plasma gasification melting furnace 12 is separated by the dust collector Ⅱ13, and the smoke is sent to the gas-liquid mixer Ⅰ14 for mixing. It is then precipitated and purified with sodium hydroxide or sodium carbonate in the air purifier Ⅰ15 to meet the environmental emission standards. The precipitate from the air purifier Ⅰ15 is sent to the drying tower Ⅰ16 for drying and collected by the dust collector Ⅲ17. The exhaust gas is sent to the gas-liquid mixer Ⅰ14 for mixing and then sent to the air purifier Ⅰ15 for purification. The fine dust collected by the dust collectors Ⅱ13 and Ⅲ17 is returned to the ferrofluorite mixer Ⅰ11 for mixing and reuse.
[0051] The beryllium glass melted out of the plasma gasification melting furnace 12 is cooled and sent to the crusher II 18 for crushing, and then sent to the unloader 19 for even distribution and sent to the Raymond mill II 20 for grinding to 0.050 mm and sent to the storage tank 21. The fine dust is collected by the dust collector IV 22, and the waste gas is sent to the air-liquid mixer II 23 for mixing and then sent to the air purifier II 24 for purification with sodium hydroxide or sodium carbonate. The waste gas meets the environmental protection standard for discharge, and the precipitate is sent to the circulating leaching tank 25 together with the material in the storage tank 21 and the fine dust in the dust collector IV 22 to leach the beryllium with pure water at room temperature.
[0052] After the beryllium has been completely leached out by testing the leaching liquid in the circulating leaching tank 25, the valve of the circulating leaching tank 25 is opened and sent to the belt vacuum filter I 26 for filtration. The liquid is sent to the beryllium hydroxide constant temperature precipitation tank 27, stirred by a circulating pump, and the pH value is adjusted to 10.5-11 with sodium hydroxide. The stirring is stopped, and the liquid temperature is controlled to 80-100 degrees Celsius. The temperature is kept for 10-30 minutes until the precipitation is complete. The reaction materials are sent to the belt vacuum filter II 28 for filtration, and the liquid is sent to the ferrofluoride synthesizer II 38 for reuse. The precipitate is sent to The product is sent to drying tower II 29 for dehydration and drying. After drying, it is collected by dust collector V 30 and sent to carbon material mixer 31 for mixing beryllium hydroxide with electrode-grade high-purity graphite in a ratio of 1:0.5~1. After mixing, it is sent to microwave carbon thermal reduction furnace 32 for reduction into metallic beryllium product, which is collected by metallic beryllium product recovery device 33. The electrode-grade high-purity graphite is recycled. The smoke from microwave carbon thermal reduction furnace 32 is sent to gas-liquid mixer III 34 together with water vapor from drying tower II 29. Carbon dioxide is absorbed by calcium oxide in air purifier III 35 to become calcium carbonate by-product.
[0053] Since the silicon content of siliceous minerals is between 90-95%, the solids filtered out by the belt vacuum filter I26 are cleaned by an ultrasonic cleaning machine 36. The solids are almost all silicon dioxide, which are collected by a silicon dioxide recovery device 37 and can be used as a raw material for making precipitated white carbon black. The liquid is sent to a ferrofluoride synthesizer II38, sodium fluoride is added to form a saturated solution, and then a ferric chloride solution is added dropwise to complete precipitation. The liquid is filtered by a belt vacuum filter III39, and the liquid is recycled. The precipitate is sent to a drying tower III40 for drying. The dried material is collected by a dust collector VI41 and returned to the ferrofluoride mixer I11 for re-dosing. The dust from the dust collector VI41 is returned to the ferrofluoride synthesizer II38 for recycling.
Claims
1. A closed-circuit device for extracting beryllium from siliceous minerals, comprising a microwave dryer I (2), a Raymond mill I (8), a material collector (9) and a dust collector I (10), characterized in that A Raymond mill I (8) and a collector (9) are sequentially arranged downstream of the microwave dryer I (2); the dust outlet of the collector (9) is connected to the dust collector I (10); the material outlet is connected to the ferrofluoride mixer I (11); the material outlet of the ferrofluoride mixer I (11) is connected to the plasma gasification melting furnace (12); the material outlet of the plasma gasification melting furnace (12) is connected to the crusher II (18); the crusher II (18) is sequentially connected to the Raymond mill II (20), the storage tank (21), the dust collector IV (22), the gas-liquid mixer II (23), the circulating leaching tank (25), the belt vacuum filter I (26), the sedimentation tank (27) and the belt vacuum filter II (28); the sediment outlet of the belt vacuum filter II (28) is connected to the drying tower II (29); the drying tower II (29) is connected to the carbon material mixer (31); the carbon material mixer (31) is connected to the microwave carbon thermal reduction furnace (32); The liquid outlet of the belt vacuum filter II (28) is connected to the ferrofluoride synthesizer II (38), the ferrofluoride synthesizer II (38) is sequentially connected to the belt vacuum filter III (39), the drying tower III (40) and the dust collector VI (41), and the dust outlet of the dust collector VI (41) is connected to the material inlet of the ferrofluoride synthesizer II (38) and / or the material inlet of the ferrofluoride mixer I (11); The water vapor outlet of the drying tower II (29) is connected to the gas-liquid mixer III (34), and the gas-liquid mixer III (34) is connected to the air purifier III (35); The solid outlet of the belt vacuum filter I (26) is connected to an ultrasonic cleaning machine (36); A loop structure is formed between the gas-liquid mixer II (23) and the air purifier II (24) via a circulation pump; The top of the circulating leaching tank (25) is a material inlet, and the bottom is a material outlet. A loop structure is formed between the inlet and the outlet through a circulating pump. A valve is provided on the material channel between the circulating leaching tank (25) and the belt vacuum filter I (26).
2. The device for closed-circuit extraction of beryllium from siliceous minerals according to claim 1, characterized in that The smoke outlet of the plasma gasification melting furnace (12) is connected to the dust collector II (13), the smoke outlet of the dust collector II (13) is connected to the gas-liquid mixer I (14), the gas-liquid mixer I (14) is connected to the air purifier I (15), the sediment outlet of the air purifier I (15) is connected to the drying tower I (16), the drying tower I (16) is connected to the dust collector III (17), and the exhaust gas outlet of the dust collector III (17) is connected to the gas-liquid mixer I (14).
3. The device for closed-circuit extraction of beryllium from siliceous minerals according to claim 2, characterized in that The dust outlets of the dust collector III (17) and the dust collector II (13) are connected to the ferrofluorite mixer I (11).
4. A process for extracting beryllium using the device described in any one of claims 1 to 3, characterized in that The steps include: Step 1: After the siliceous mineral is crushed by a crusher I (1), it is sent to a microwave dryer I (2) for drying. The dried material is sent to a conveyor (6) and then to a feeder (7) for quantitative feeding into a Raymond mill I (8) for crushing. The material is collected by a collector (9). The dust generated by the Raymond mill I (8) and the collector (9) is recovered by a dust collector I (10) and discharged to clean air. The material in the collector (9) and the dust collected by the dust collector I (10) are sent to a ferrofluoride mixer I (11) together, and the material and drug ratio is 5:4.5 for mixing. Step 2: After being mixed in the ferrofluoride mixer I (11), the mixture is sent to the plasma gasification melting furnace (12) for smelting into beryllium glass. The smoke from the plasma gasification melting furnace (12) is separated by the dust collector II (13). The smoke is sent to the gas-liquid mixer I (14) for mixing and then precipitated and purified with sodium hydroxide or sodium carbonate in the air purifier I (15) to meet the environmental emission standards. The precipitate from the air purifier I (15) is sent to the drying tower I (16) for drying and collected by the dust collector III (17). The waste gas is sent to the gas-liquid mixer I (14) for mixing and then sent to the air purifier I (15) for purification. The fine dust collected by the dust collectors II (13) and III (17) is sent back to the ferrofluoride mixer I (11) for mixing and reuse. Step 3: The beryllium glass melted by the plasma gasification melting furnace (12) is cooled and sent to the crusher II (18) for crushing, and then sent to the unloader (19) for even distribution and sent to the Raymond mill II (20) for grinding to 0.050 mm and sent to the storage tank (21, the dust is collected by the dust collector IV (22), the exhaust gas is sent to the air-liquid mixer II (23) for mixing and then sent to the air purifier II (24) for purification with sodium hydroxide or sodium carbonate, and the exhaust gas meets the environmental protection standard. The precipitate, the material in the storage tank (21) and the dust in the dust collector IV (22) are sent to the circulation leaching tank (25) together with the material in the storage tank (21) and the dust in the dust collector IV (22) to leach the beryllium with pure water at room temperature; Step 4: After checking the leaching liquid in the circulating leaching tank (25) and confirming that the beryllium has been completely leached, the valve of the circulating leaching tank (25) is opened and the leaching liquid is sent to the belt vacuum filter I (26) for filtration. The liquid is sent to the beryllium hydroxide constant temperature precipitation tank (27), stirred by a circulating pump, and the pH value is adjusted to 10.5-11 with sodium hydroxide. Stirring is stopped and the liquid temperature is controlled to 80 ~ 100 degrees Celsius, keep warm for 10-30 minutes until precipitation is complete, the reaction material is sent to a belt vacuum filter II (28) for filtration, the liquid is sent to a ferrofluoride synthesizer II (38) for reuse, the precipitate is sent to a drying tower II (29) for dehydration and drying, after drying, it is collected by a dust collector V (30) and sent to a carbon material mixer (31) for mixing beryllium hydroxide with electrode-grade high-purity graphite in a ratio of 1:0.5-1, and after mixing, it is sent to a microwave carbon thermal reduction furnace (32) for reduction to a metal beryllium product, which is collected by a metal beryllium product recovery device (33), and the electrode-grade high-purity graphite is recycled, and the smoke from the microwave carbon thermal reduction furnace (32) and the water vapor from the drying tower II (29) are sent to a gas-liquid mixer III (34) together, and carbon dioxide is absorbed by calcium oxide in an air purifier III (35) to become a calcium carbonate byproduct.
5. The process according to claim 4, characterized in that The solid filtered out by the belt vacuum filter I (26) in step 4 is cleaned by an ultrasonic cleaning machine (36), and the solid silicon dioxide is collected by a silicon dioxide recovery device (37). The liquid is sent to the ferrofluoride synthesizer II (38), sodium fluoride is added to form a saturated solution, and then a ferric chloride solution is added dropwise to complete precipitation. The liquid is filtered by a belt vacuum filter III (39), and the liquid is recycled. The precipitate is sent to a drying tower III (40) for drying. The dried product is collected by a dust collector VI (41) and returned to the ferrofluoride mixer I (11) for re-dosing. The dust in the dust collector VI (41) is returned to the ferrofluoride synthesizer II (38) for recycling.
Citation Information
Patent Citations
A leach device for producing berillia
CN207243489U
Device for extracting beryllium from siliceous mineral in closed circuit
CN212388086U