CN113249576B - Waste cathode carbon block, fluoride and metal sodium recovery processing equipment and use method - Google Patents
Waste cathode carbon block, fluoride and metal sodium recovery processing equipment and use method Download PDFInfo
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- CN113249576B CN113249576B CN202110422354.5A CN202110422354A CN113249576B CN 113249576 B CN113249576 B CN 113249576B CN 202110422354 A CN202110422354 A CN 202110422354A CN 113249576 B CN113249576 B CN 113249576B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B9/00—General methods of preparing halides
- C01B9/08—Fluorides
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/10—Obtaining alkali metals
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/02—Refining by liquating, filtering, centrifuging, distilling, or supersonic wave action including acoustic waves
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C3/00—Electrolytic production, recovery or refining of metals by electrolysis of melts
- C25C3/06—Electrolytic production, recovery or refining of metals by electrolysis of melts of aluminium
- C25C3/08—Cell construction, e.g. bottoms, walls, cathodes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention relates to a recovery treatment device and a process for waste cathode carbon blocks, fluorides and sodium metal in aluminum electrolysis, which comprises an evaporator, wherein an outlet of the evaporator is connected with an alkali metal recovery treatment system through a first pipeline, an outlet connected with the alkali metal recovery treatment system is connected with a liquid sodium metal collecting system through a second pipeline, a crystallizer is arranged at the outlet of the evaporator, an air cooling system is sleeved on the crystallizer, a first inert gas inlet and a first inert gas outlet are arranged on the alkali metal recovery treatment system, and a second inert gas inlet and a second inert gas outlet are arranged on the liquid sodium metal collecting system. The invention has the advantages and effects that: the method can separate each component in the waste cathode carbon block and effectively recover the components, particularly can recover the metallic sodium with high quality, ensures the safety of treating the waste cathode carbon block, and simultaneously obtains the high-purity metallic sodium and fluoride salt with higher added value.
Description
Technical Field
The invention relates to a recovery treatment device and a process, in particular to a recovery treatment device and a process for aluminum electrolysis waste cathode carbon blocks, fluoride and metal sodium, belonging to the field of comprehensive utilization of hazardous solid waste resources.
Background
In the industrial aluminum electrolysis production, aluminum liquid is deposited on the surface of a cathode, and sodium ions in electrolyte continuously permeate to a cathode carbon block, a fire-resistant layer and a heat-insulating layer of a cathode lining in the form of NaF or metal Na steam, so that the lining of an electrolytic cell is damaged, and the service life of the aluminum electrolytic cell is shortened. Statistically, about 25 + -15 kg of waste tank liner is generated per 1 ton of raw aluminum, which contains carbonaceous materials, fluoride salt, cyanide, and a small amount of aluminum carbide, aluminum nitride, etc., wherein fluoride and cyanide are toxic substances. Carbon and fluoride in the waste cathode are valuable substances, and are worth recycling so as to facilitate resource regeneration, and the method conforms to the policies of clean production and circular economy.
Along with the rapid development of the aluminum electrolysis industry in China, the pollution problem of the waste tank lining is more and more prominent, and the problem becomes a bottleneck problem which restricts the aluminum electrolysis enterprises to save resources, reduce pollution and reduce emission, and is mainly shown in the following steps: soluble fluoride and cyanide in the waste tank lining can pollute surface water and underground water, have great harm to the growth of animals and plants, blacken and necrose animal bones/plant tissues and influence the agricultural ecological balance. The open stockpiled waste liners are a potential source of concentrated hazards and can create hazards from rain or moisture absorption in the air. When the waste tank lining is drenched with rain, the contained soluble fluoride and cyanide can be mixed into rivers along with the rain water and permeate into underground polluted soil and water, and can also generate chemical reaction with the water. The reaction of the waste tank lining and water is violent, and the waste tank lining and water easily generate and emit a large amount of gas at normal temperature and normal pressure, and the strong ammonia smell is often smelled. HCN gas generated by the reaction is extremely toxic, and can cause poisoning and death in a few seconds when being used in a small amount.
The cost of the waste tank lining for the standardized disposal is 3000 to 5000 yuan/ton, and the economic burden of an enterprise is further increased. Resource regeneration and cyclic economy development are urgent. At present, the technology for treating the waste slot lining at home and abroad is generally divided into two types: one is that the harmful waste is preferentially disposed and stabilized, and the waste is treated in landfills after being innoxious; one is the bias towards utilizing waste to produce usable products. Both wet and fire processes are known as the two types of processes.
1) The foreign waste slot lining processing technology has early development and relatively high technical maturity. The technologies that are important and representative are SPLIT technology of aluminum Pechiney, rotary kiln technology of Reynolds, COMTOR technology of Comalco, LCL & L technology of Rio Tinto Alcan, and Ausmelt furnace technology of Alcoa/Ausmelt.
2) The domestic waste slot lining treatment technology is developed late, and the technical maturity is relatively low. A flotation method, an alumina clinker sintering process, a rotary kiln sintering process, a flotation acid leaching process and a wet harmless treatment process appear in sequence. The scale of the waste tank liner treatment in China is small and the proportion is low. Whether the method is pyrogenic landfill, pyrogenic recovery or wet recovery, the related technology has certain gap with the advanced level of the world.
The research and practical experience of foreign countries for many years proves that HF and HCN are separated out during the wet treatment process of the waste tank lining, so that the equipment is seriously corroded, the operation environment is polluted, and the human health is harmed. In addition, the wet treatment process of the waste tank lining has long flow, complex process and large investment. The pyrometallurgical treatment technology of different technical lines can well realize the harmless utilization of the waste tank liners, and has the characteristics of simple process, low investment and thorough harmful substance treatment, so the pyrometallurgical treatment technology is the leading direction of the harmless treatment and comprehensive utilization of the waste tank liners at home and abroad.
Disclosure of Invention
The invention provides a waste cathode carbon block, fluoride and metallic sodium recovery treatment equipment and a use method thereof, aiming at treating the waste cathode carbon block for aluminum electrolysis and by-products of fluoride and metallic sodium with low energy consumption and low cost so as to realize the harmlessness, reduction and recycling of the treatment of the waste cathode carbon block.
The waste cathode carbon block, the fluoride and the sodium metal recovery treatment equipment comprise an evaporator, wherein an outlet of the evaporator is connected with an alkali metal recovery treatment system through a first pipeline, an outlet connected with the alkali metal recovery treatment system is connected with a liquid sodium metal collection system through a second pipeline, a crystallizer is arranged at the outlet of the evaporator, an air cooling system is sleeved on the crystallizer, a first inert gas inlet and a first inert gas outlet are arranged on the alkali metal recovery treatment system, and a second inert gas inlet and a second inert gas outlet are arranged on the liquid sodium metal collection system.
The evaporator is internally provided with a material container, and the air cooling system is provided with an air inlet and an air outlet.
The alkali metal recovery processing system comprises a liquid sodium circulation pipeline, wherein an inert gas pipeline is sleeved on the liquid sodium circulation pipeline, and a first heating device is sleeved on the inert gas pipeline.
The gas inlet end of the inert gas pipeline is connected with the first inert gas inlet, and the gas outlet end of the inert gas pipeline is connected with the first inert gas outlet.
The liquid sodium circulation pipeline is a porous liquid sodium circulation pipeline.
The liquid metal sodium collecting system comprises a tank body, a second heating device is sleeved outside the tank body, a tank cover is arranged at the top of the tank body, a second pipeline penetrates through the tank cover to be inserted into the tank body, a second inert gas inlet and a second inert gas outlet are inserted into the tank body from the tank cover, and a third pipeline is inserted into the tank body from the tank cover.
The third pipeline is provided with a pressure gauge, and the outlet of the third pipeline is connected with a vacuum port.
The using method of the waste cathode carbon block and the fluoride and metal sodium recovery processing equipment comprises the steps of crushing the waste cathode carbon block to a certain granularity, then loading the waste cathode carbon block into an evaporator, starting to vacuumize through a vacuum port, after air is pumped out, stopping vacuumization, introducing inert gas into an alkali metal recovery processing system and a liquid metal sodium collection system, starting to vacuumize again, extracting the inert gas in the alkali metal recovery processing system and the liquid metal sodium collection system, after the vacuum degree is balanced, heating the evaporator to 400 ℃, starting a first heating device and a second heating device, controlling the temperature to be 100-150 ℃, keeping the temperature at 900-1200 ℃ after the preset temperature of the evaporator is reached, keeping the temperature at 1h-5h at constant temperature, cooling the evaporator to 500 ℃ through an air cooling system, stopping the vacuumization operation, simultaneously introducing the inert gas into the alkali metal recovery processing system and the liquid metal sodium collection system, closing a valve between the evaporator and the alkali metal recovery processing system, closing the air cooling system, separating the evaporator and the alkali metal recovery processing system, and taking out the waste cathode carbon block and the fluoride on a crystallizer after the evaporator; in a constant temperature state, sodium vapor enters the porous liquid sodium circulation pipeline from the evaporator, and gaseous sodium is converted into liquid sodium; and the liquid sodium enters a liquid sodium metal collecting system through a second pipeline to complete the recovery of the sodium metal.
And when the temperature is constant, the temperature of the liquid metal sodium collecting system is controlled to be 100-150 ℃, after the evaporator is cooled to 500 ℃ for 30min, the inert gas is stopped from being introduced into the alkali metal recovery processing system, and the alkali metal recovery processing system and the liquid metal sodium collecting system are separated.
The vacuum degree is from 3Pa to 50Pa when the vacuum degree is balanced; the evaporator is made of rigid material resistant to fluoride corrosion, the container is made of carbonaceous material or ceramic material, and fluoride salt distilled out is crystallized at a crystallization position; the temperature gradient on the crystallizer is controlled by an air cooling system, so that the crystallized product is crystallized at different positions.
The invention has the advantages and effects that: the invention can carry out efficient harmless, reduction and resource treatment on the waste cathode lining, and the whole equipment has the characteristics of convenient operation, simple process flow, low recovery cost, great social value and the like. Most importantly, the components in the waste cathode carbon block can be separated and effectively recovered, particularly, the high-quality metal sodium can be recovered, the safety of treating the waste cathode carbon block is ensured, and meanwhile, the high-purity metal sodium and fluoride salt with higher added values are obtained.
Drawings
Fig. 1 is a schematic structural view of the present invention.
Fig. 2 is a sectional view at the mold of fig. 1.
FIG. 3 is a cross-sectional view of an alkali metal recovery processing system.
In the figure: 1. an evaporator; 2. an alkali metal recovery processing system; 3. a liquid sodium collection system; 4. an air cooling system; 5. a crystallizer; 6. a first heating device; 7. an inert gas conduit; 8. a first inert gas inlet; 9. a first inert gas outlet; 10. a pressure gauge; 11. a second inert gas inlet; 12. a second inert gas outlet; 13. a second heating device; 14. a liquid sodium circulation pipeline; 15. a vacuum port; 16. a first pipe; 17. a second pipe; 18. a third pipeline; 19. a wind inlet; 20. an air outlet; 21. a tank body; 22. a can lid; 23. a container.
Drawings
The invention will be further explained with reference to the drawings.
Example 1
As shown in the figure, the recovery processing device for waste cathode carbon block, fluoride and sodium metal comprises an evaporator 1, wherein an outlet of the evaporator 1 is connected with an alkali metal recovery processing system 2 through a first pipeline 16, an outlet connected with the alkali metal recovery processing system 2 is connected with a liquid sodium metal collecting system 3 through a second pipeline 17, a crystallizer 5 is arranged at the outlet of the evaporator 1, an air cooling system 6 is sleeved on the crystallizer 5, a first inert gas inlet 8 and a first inert gas outlet 9 are arranged on the alkali metal recovery processing system 2, and a second inert gas inlet 11 and a second inert gas outlet 12 are arranged on the liquid sodium metal collecting system 3.
The evaporator 1 is internally provided with a container 23, and the air cooling system 4 is provided with an air inlet 19 and an air outlet 20.
The alkali metal recovery processing system 2 is a three-layer cylinder structure and comprises a liquid sodium circulation pipeline 14, an inert gas pipeline 7 is sleeved on the liquid sodium circulation pipeline 14, and a first heating device 6 is sleeved on the inert gas pipeline 7. In order to protect the liquid sodium metal from contacting with air, the inert gas is rapidly cooled and converted into liquid sodium in the liquid sodium circulation pipeline 14, the liquid sodium circulation pipeline 14 is a cylindrical porous device, the alkali metal liquid can flow conveniently, and the liquid sodium flows into the liquid sodium metal collection system 3 through the discharge hole.
The gas inlet end of the inert gas pipeline 7 is connected with a first inert gas inlet 8, and the gas outlet end of the inert gas pipeline 7 is connected with a first inert gas outlet 9.
The liquid sodium circulation pipeline 14 is a porous liquid sodium circulation pipeline.
The liquid sodium metal collecting system 3 comprises a tank body 21, a second heating device 13 is sleeved outside the tank body 21, a tank cover 22 is arranged at the top of the tank body 21, a second pipeline 17 is inserted into the tank body 21 through the tank cover 22, a second inert gas inlet 11 and a second inert gas outlet 12 are inserted into the tank body 21 from the tank cover 22, and a third pipeline 18 is inserted into the tank body 21 from the tank cover 22.
The third pipeline 18 is provided with a pressure gauge 10, and the outlet of the third pipeline 18 is connected with a vacuum port 15. The liquid sodium metal collection system 3 allows the sodium metal to be converted between a liquid state and a solid state.
The using method of the waste cathode carbon block and the recovery processing equipment of fluoride and metal sodium comprises the steps of crushing the waste cathode carbon block to a certain particle size, then loading the waste cathode carbon block into an evaporator 1, starting to vacuumize through a vacuum port 15, after air is pumped out, stopping vacuumization, introducing inert gas into an alkali metal recovery processing system 2 and a liquid metal sodium collecting system 3, starting vacuumization again, extracting inert gas in the alkali metal recovery processing system 2 and the liquid metal sodium collecting system 3, after the vacuum degree is balanced, heating the evaporator 1 to 400 ℃, starting a first heating device 6 and a second heating device 13, controlling the temperature to be 120 ℃, after the preset temperature of the evaporator 1 is 1100 ℃, keeping the temperature at constant temperature for 3 hours, closing the heating system, after the evaporator 1 is cooled to 500 ℃ through an air cooling system 4, stopping vacuumization, simultaneously introducing inert gas into the alkali metal recovery processing system 2 and the liquid metal sodium collecting system 3, closing a valve between the evaporator 1 and the alkali metal recovery processing system 2, separating the evaporator 1 from the air cooling system 4 from the evaporator 1, and the alkali metal sodium metal recovery processing system 2, and taking the fluoride from the aluminum electrolysis cathode carbon block 1 to form an electrolytic solution with higher added value than that can be used in an aluminum electrolysis bath and an electrolysis bath after the waste carbon block 5 is recovered; at a constant temperature, sodium vapor enters the porous liquid sodium circulation pipeline from the evaporator 1, and gaseous sodium is converted into liquid sodium; the liquid sodium enters the liquid sodium metal collecting system 3 through the second pipeline 17, and the recovery of the sodium metal is completed.
And in the constant temperature state, the temperature of the liquid metal sodium collecting system 3 is controlled to be 120 ℃, after the evaporator 1 is cooled to 500 ℃ for 30min, the inert gas is stopped to be introduced into the alkali metal recovery processing system 2, and the alkali metal recovery processing system 2 and the liquid metal sodium collecting system 3 are separated.
The vacuum degree is 25Pa when balanced; the evaporator 1 is made of rigid material resistant to fluoride corrosion, the container 23 is made of carbon material or ceramic material, and the distilled fluoride salt is crystallized at the crystallization position; the temperature gradient on the crystallizer 5 is controlled by the air cooling system 4, so that the crystallized product is crystallized at different positions.
Example 2
In example 1, the temperature of the first heating device 6 and the second heating device 13 was controlled to 150 ℃, the preset temperature of the evaporator 1 was 900 ℃, the constant temperature was maintained for 5 hours, and the vacuum degree was 50Pa at equilibrium. Otherwise, the same procedure as in example 1 was repeated.
Example 3
The temperature of the first heating device 6 and the second heating device 13 in the embodiment 1 is controlled at 130 ℃, the preset temperature of the evaporator 1 is 1200 ℃, the constant temperature is kept for 1h, and the vacuum degree is 3Pa when being balanced. Otherwise, the same procedure as in example 1 was repeated.
Example 4
In example 1, the temperature of the first heating device 6 and the second heating device 13 was controlled to 100 ℃, the preset temperature of the evaporator 1 was 1000 ℃, the constant temperature was 4 h, and the vacuum was 10Pa when the vacuum was balanced. Otherwise, the same procedure as in example 1 was repeated.
The above description is only a preferred embodiment of the present invention and should not be taken as limiting the scope of the invention, which is intended to cover any modifications, equivalents, improvements, etc. within the spirit and scope of the present invention.
Claims (8)
1. The recovery processing equipment for the waste cathode carbon block, the fluoride and the sodium metal is characterized by comprising an evaporator, wherein an outlet of the evaporator is connected with an alkali metal recovery processing system through a first pipeline, an outlet connected with the alkali metal recovery processing system is connected with a liquid sodium metal collecting system through a second pipeline, a crystallizer is arranged at the outlet of the evaporator, an air cooling system is sleeved on the crystallizer, a first inert gas inlet and a first inert gas outlet are arranged on the alkali metal recovery processing system, and a second inert gas inlet and a second inert gas outlet are arranged on the liquid sodium metal collecting system; the alkali metal recovery treatment system comprises a liquid sodium circulation pipeline, wherein an inert gas pipeline is sleeved on the liquid sodium circulation pipeline, and a first heating device is sleeved on the inert gas pipeline; the liquid sodium circulation pipeline is a porous liquid sodium circulation pipeline.
2. The apparatus as claimed in claim 1, wherein the evaporator is provided with a container, and the air cooling system is provided with an air inlet and an air outlet.
3. The apparatus as claimed in claim 1, wherein the inlet end of the inert gas pipe is connected to the first inert gas inlet, and the outlet end of the inert gas pipe is connected to the first inert gas outlet.
4. The spent cathode blocks and fluoride and sodium metal recovery processing equipment as claimed in claim 1, wherein the liquid sodium metal collection system comprises a tank body, a second heating device is sleeved outside the tank body, a tank cover is arranged at the top of the tank body, a second pipeline is inserted into the tank body through the tank cover, a second inert gas inlet and a second inert gas outlet are inserted into the tank body from the tank cover, and a third pipeline is inserted into the tank body from the tank cover.
5. The apparatus as claimed in claim 4, wherein the third pipeline is provided with a pressure gauge, and the outlet of the third pipeline is connected with a vacuum port.
6. The method for using the waste cathode carbon block and the equipment for recycling and treating fluoride and metallic sodium as claimed in claim 1, wherein the waste cathode carbon block is crushed to a certain particle size, then is loaded into the evaporator, vacuum pumping is started through a vacuum port, after air is pumped out, vacuum pumping operation is stopped, inert gas is introduced into the alkali metal recycling and treating system and the liquid metallic sodium collecting system, vacuum pumping is started again, inert gas in the alkali metal recycling and treating system and the liquid metallic sodium collecting system is pumped out, after the vacuum degree is balanced, the evaporator is heated to 400 ℃, the first heating device and the second heating device are started, the temperature is controlled to be 100-150 ℃, after the preset temperature of the evaporator is 900-1200 ℃, the constant temperature is kept for 1h-5h, after the evaporator is cooled to 500 ℃ through the air cooling system, the vacuum pumping operation is stopped, simultaneously, the inert gas is introduced into the alkali metal recycling and treating system and the liquid metallic sodium collecting system, the valve between the evaporator and the alkali metal recycling and treating system is closed, the air cooling system, the evaporator and the fluoride recovering and the waste cathode carbon block are taken out from the evaporator and the crystallizer; in a constant temperature state, sodium vapor enters the porous liquid sodium circulation pipeline from the evaporator, and gaseous sodium is converted into liquid sodium; and the liquid sodium enters a liquid sodium metal collecting system through a second pipeline to complete the recovery of the sodium metal.
7. The use method of the waste cathode carbon block and the equipment for recovery and treatment of fluoride and metallic sodium as claimed in claim 6, characterized in that in the constant temperature state, the temperature of the liquid metallic sodium collection system is controlled at 100-150 ℃, after the evaporator is cooled to 500 ℃ for 30min, the introduction of inert gas into the alkali metal recovery treatment system is stopped, and the alkali metal recovery treatment system and the liquid metallic sodium collection system are separated.
8. The use method of the waste cathode carbon block and the equipment for recovering and treating fluoride and metallic sodium as claimed in claim 6, characterized in that the vacuum degree is from 3Pa to 50Pa when the vacuum degree is balanced; the evaporator is made of fluoride corrosion resistant rigid material, the container is made of carbon material or ceramic material, and the distilled fluoride salt is crystallized at the crystallization position; the temperature gradient on the crystallizer is controlled by an air cooling system, so that the crystallized product is crystallized at different positions.
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| CN202110422354.5A CN113249576B (en) | 2021-04-20 | 2021-04-20 | Waste cathode carbon block, fluoride and metal sodium recovery processing equipment and use method |
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| CN111363922A (en) * | 2020-02-28 | 2020-07-03 | 内蒙古工业大学 | Vacuum distillation device and process for continuously recovering metal sodium and calcium from sodium slag |
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2021
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| CN103667708A (en) * | 2013-12-06 | 2014-03-26 | 内蒙古兰太实业股份有限公司 | Process and device for recovering solid sodium metal waste residues |
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