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WO2023246367A1 - Procédé et appareil de production en continu par électrolyse d'un sel fondu à base d'un minerai contenant du sulfure d'antimoine - Google Patents

Procédé et appareil de production en continu par électrolyse d'un sel fondu à base d'un minerai contenant du sulfure d'antimoine Download PDF

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Publication number
WO2023246367A1
WO2023246367A1 PCT/CN2023/093924 CN2023093924W WO2023246367A1 WO 2023246367 A1 WO2023246367 A1 WO 2023246367A1 CN 2023093924 W CN2023093924 W CN 2023093924W WO 2023246367 A1 WO2023246367 A1 WO 2023246367A1
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Prior art keywords
antimony
electrolysis
furnace
molten salt
electrolytic
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English (en)
Chinese (zh)
Inventor
杨建广
朱强
丁瑞泽
唐朝波
南天翔
曾伟志
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Central South University
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Central South University
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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
    • C25C3/34—Electrolytic production, recovery or refining of metals by electrolysis of melts of metals not provided for in groups C25C3/02 - C25C3/32
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00—Electrolytic production of inorganic compounds or non-metals
    • C25B1/01—Products
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B15/00—Operating or servicing cells
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
    • C25C7/00—Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells
    • C25C7/06—Operating or servicing
    • 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

Definitions

  • the invention relates to a method and device for the continuous electrolysis production of molten salt containing antimony sulfide ore, and belongs to the technical field of non-ferrous metal metallurgy.
  • Antimony is a rare strategic metal widely used in flame retardant, alloys, ceramics, pigments, semiconductors and chemical industries.
  • the raw material for antimony smelting in China is mainly antimony ore (Sb 2 S 3 ).
  • antimony smelting enterprises mainly use the "blast furnace volatilization-reverberatory furnace reduction smelting" process to produce metallic antimony. That is, after the antimony is granulated, it is added to the blast furnace together with coke and flux for volatilization and smelting, so that the antimony enters the high-temperature flue gas and is recovered in the form of crude antimony oxide after condensation and dust collection.
  • the low-concentration SO 2 generated during the smelting process is desulfurized and discharged null.
  • Blast furnace volatilization smelting has the advantages of strong raw material adaptability, large processing capacity, high metal recovery rate, easy mechanical operation, and low labor intensity. Since the successful research of the Yuan Tin Mine Bureau, it has developed rapidly in our country and has now become a major Antimony smelting method. However, the special operating conditions of "low material column, thin material layer, high coke rate, and high temperature furnace top" determine that this process has the disadvantages of high coke rate, high energy consumption, short furnace life, and complicated flue gas cooling and dust collection systems.
  • the purpose of the present invention is to provide a method for the continuous electrolysis production of molten salts containing antimony sulfide ores, using two electrolytic furnaces to smelt antimony in sections, so as to solve the problem of the current single electrolytic furnace, namely patents 201710775124.0 and 202010114724.4.
  • the above-mentioned antimony sulfide-containing ore molten salt electrolysis antimony refining method cannot achieve continuous production in the true sense.
  • the current efficiency is low, the electrolysis energy consumption is high, the electrolysis process parameters are difficult to control in real time, and the antimony content in the residue is high.
  • a method for continuous electrolysis production of antimony sulfide ore molten salt including the following steps:
  • step (2) Enter the electrolyzed melt obtained in step (1) through the chute into the depletion electrolytic furnace for constant voltage depletion electrolysis. Before electrolysis, replenish molten salt, metallic antimony liquid and elemental sulfur to discharge antimony from the depletion electrolytic furnace respectively.
  • the flue gas port of the depleted electrolytic furnace is discharged, and the depleted slag is released from the slag discharge port.
  • the mass percentage of antimony sulfide ore and eutectic molten salt is 10:1 to 5:4, preferably 6:1 to 5:2.
  • the eutectic molten salt is a mixture of sodium chloride and potassium chloride, and the mass percentage of sodium chloride and potassium chloride is 7:3-2:7, preferably 4:5-2:5.
  • step (1) the temperature in the high antimony electrolysis furnace is 700-950°C, and the heating rate is 8-15°C/min, preferably 850-900°C.
  • the anode current density during electrolytic smelting is 1000-5000 A ⁇ m -2 , preferably 2000-3000 A ⁇ m -2 ; the cell voltage is controlled below 4 V, preferably 3.8 V or less; the distance between anode and cathode is 1 to 8cm, preferably 2 to 4cm.
  • the inert gas is preferably nitrogen or argon, the pressure of the inert gas blown is 0.12-0.35MPa, and the inert gas flow rate is 40-1100 L/(min ⁇ m 3 ).
  • the inert gas needs to be preheated before blowing in.
  • the preferred temperature of the preheated gas is 700 to 950°C.
  • Preheating the inert gas can prevent the local temperature in the high antimony electrolysis furnace from being too cold, resulting in insufficient melt temperature and affecting the electrolysis efficiency.
  • the electrolytic smelting reaction time is 2 to 20 hours, preferably 8 to 15 hours.
  • the high antimony electrolysis furnace adopts the electrolysis method of constant current limiting voltage and inert gas blowing to stir the molten salt, and replenishing materials according to the theoretical consumption, including electrolysis consumption and volatilization loss.
  • the replenishing materials are antimony sulfide ore, chlorine A mixture of sodium chloride and potassium chloride.
  • the material concentration in the electrolysis furnace can be maintained sufficient, uniform and stable.
  • step (2) the molten salt supplemented before the depletion electrolysis is eutectic molten salt, and the molten salt supplementary amount is 5 to 40% (5 to 40% based on the melt coming out of the high antimony electrolysis furnace). %).
  • Supplementing molten salt before electrolysis can reduce the viscosity value of the melt coming out of the high antimony electrolysis furnace, reduce the energy consumption loss in the electrolysis process and facilitate the subsequent discharge of depleted slag.
  • Results of current efficiency and energy consumption based on experiments with different amounts of molten salt supplementation. Determine the amount of molten salt to replenish.
  • step (2) the temperature in the depletion electrolysis furnace is 700-1050°C, and the heating rate is 8-15°C/min, preferably 850-950°C.
  • the temperature in the depleted electrolytic furnace is higher than the temperature in the high antimony electrolytic furnace. Since the higher the temperature, the smaller the viscosity of the melt. Increasing the temperature and supplementing molten salt are both to reduce the viscosity of the melt in the depleted electrolytic bath, so as to improve The current efficiency of the electrolysis process and the reduction of electrolysis energy consumption.
  • step (2) the cell voltage during depletion electrolysis is 1.5-4.5 V, preferably 2.5-3.5 V; the distance between cathodes and anodes is 1-8 cm, preferably 2-4 cm.
  • the depletion electrolysis reaction time is 2 to 6 hours, preferably 3 to 4 hours; the antimony in the slag discharged from the slag outlet after the depletion electrolysis is ⁇ 1wt.%.
  • the depleted electrolytic furnace uses constant voltage electrolysis to deplete the post-electrolysis melt of the electrolytic high antimony electrolysis furnace, so that the antimony in the final residue reaches a lower level (the antimony in the slag released from the slag outlet after depletion electrolysis ⁇ 1wt.%), and separate the molten salt from the gangue and other components in the mineral to achieve the opening of impurities.
  • two consecutive furnaces are combined into the process of antimony refining by molten salt electrolysis of antimony sulfide ores.
  • the antimony liquid is discharged from the antimony discharge port.
  • the remaining impurities including gangue and unelectrolyzed The antimony sulfide melt enters the depletion electrolytic furnace through the chute.
  • constant voltage depletion electrolysis is performed, so that the antimony in the final discharged residue is at a lower level.
  • the invention creatively performs constant current and voltage limiting electrolysis in the high antimony electrolytic furnace, and performs constant voltage depletion electrolysis in the depleted electrolytic furnace.
  • the antimony content in the residue can be effectively reduced and energy consumption can be saved.
  • the reasons are as follows: Due to the high concentration of antimony in the high-antimony electrolysis furnace, the process of constant current and voltage-limited electrolysis of antimony has high current efficiency and low electrolysis energy consumption. However, if constant current and voltage-limited electrolysis is maintained, the accumulation of impurities will lead to changes in the physical properties of the melt. , the current efficiency decreases and energy consumption increases, so it needs to be transferred to a depleted electrolysis furnace.
  • the molten salt supplement, cell voltage, electrode spacing and electrolysis temperature are controlled within the above ranges respectively.
  • the electrolysis efficiency is the highest and the energy consumption is the lowest. This is due to the molten salt supplement,
  • the increase in temperature can effectively improve the viscosity, conductivity and other physical properties of the molten salt, which is more conducive to the progress of molten salt electrolysis.
  • the constant voltage process can effectively ensure that the current density is controlled according to the concentration of antimony sulfide in the melt during the electrolysis process to avoid excessive waste of electrical energy.
  • Another object of the present invention is to provide a combined molten salt electrolysis furnace device matched with the above-mentioned method for continuous electrolysis production of molten salt containing antimony sulfide ores.
  • the electrolytic furnace includes a hollow furnace body and an electrolysis unit arranged in the furnace body; the furnace body is provided with a feed inlet and a flue gas port respectively in the upper part, and is respectively provided in the lower part.
  • the slag discharge port of the high antimony electrolytic furnace is connected through a chute.
  • the high antimony electrolytic furnace is equipped with a gas lance that extends into the furnace body and blows inert gas.
  • a thermal resistor is provided on the outer wall of the electrolysis furnace, and the thermal resistor is covered with an insulation layer; the chute is equipped with a discharge valve and a sampling observation port, and the flow rate of the melt in the chute is 0.1 to 0.8 m ⁇ s. -1 ;
  • the electrolysis unit includes a cathode arranged at the bottom of the furnace body and an anode arranged at the upper part of the furnace body.
  • the anode is connected to an anode guide rod extending out of the furnace body to connect the positive electrode of the power supply through a wire; the cathode is connected through a wire Connect the negative terminal of the power supply.
  • the gas spray gun and anode guide rod are made of aluminum oxide.
  • the feeder continuously feeds the material and the gas spray gun stirs the melt.
  • the antimony liquid obtained by electrolysis is discharged from the antimony discharge port.
  • the sulfur-containing flue gas is collected from the flue gas port, and the slag is discharged from the slag discharge port.
  • Sampling and analysis are carried out from the sampling observation port of the chute to achieve optimal control of the electrolysis process parameters of the depletion electrolysis furnace.
  • the amount of electrolytic materials obtained from the depleted electrolysis furnace can be controlled and the physical properties of the components can be observed.
  • the melt flow in the chute can be controlled within the above preferred range, which can effectively avoid the loss of melt heat. loss or blockage of the chute.
  • the method and device for the continuous electrolysis production of antimony sulfide ore molten salt of the present invention have the following advantages:
  • the design of the two-furnace molten salt electrolysis antimony smelting of high antimony electrolytic furnace and depleted electrolytic furnace enables the entire electrolysis process to be carried out simultaneously under two different process parameters according to needs, meeting the needs of the molten salt electrolysis process of antimony sulfide materials.
  • the inert gas blows and stirs the constant current electrolysis to achieve high current efficiency, and the static depletion constant voltage electrolysis process realizes the purpose of low antimony content in the molten salt electrolytic slag and the stratification and separation of the molten salt and slag components; fully satisfying the industrial needs Technologically and economically viable requirements for the production process.
  • the present invention realizes the circulation and reuse of inert molten salt through the depletion electrolysis of the melt after electrolysis in the high antimony electrolysis furnace and the separation and purification of components such as gangue, which greatly reduces the cost of antimony sulfide ores.
  • Raw material costs for molten salt electrolysis.
  • the present invention can achieve complete continuous production of one-step antimony smelting, and significantly reduce the pyrometallurgical smelting temperature of antimony concentrate, directly producing It produces metallic antimony and elemental sulfur without SO2 emissions. It has the advantages of low energy consumption and high direct recovery rate of antimony and sulfur. It is of great significance to promote the progress of China's antimony metallurgical technology and energy conservation and emission reduction.
  • Figure 1 is a schematic diagram of the continuous electrolysis production device of molten salt containing antimony sulfide ore according to the present invention (1-feeder, 2-thermal resistor, 3-antimony discharge port, 4-gas spray gun, 5-anode guide rod, 6-height Antimony electrolytic furnace, 7-flue gas port, 8-graphite anode, 9-chute, 10-graphite cathode, 11-sampling observation port, 12-coarse antimony tank, 13-depletion electrolytic furnace, 14-insulation layer, 15- Slag discharge port, 16-DC power supply, 17-slag, 18-antimony sulfide, 19-molten salt, 20-antimony liquid).
  • the two-furnace molten salt electrolysis device in this embodiment uses two electrolytic furnaces with the same structure, in which each electrolytic furnace includes a hollow furnace body and an electrolysis unit arranged in the furnace body.
  • the furnace body is equipped with a feeding port and a flue gas port on the upper part, and an antimony discharging port and a slag discharging port on the lower part.
  • a thermal resistor is provided on the outer wall of the furnace body, and the thermal resistor is covered with an insulation layer. The melt is heated by the thermal resistor.
  • the electrolytic furnaces are used as a high antimony electrolytic furnace, and the slag discharge port of this high antimony electrolytic furnace is positioned higher than the feed port of the other as a depleted electrolytic furnace.
  • the slag discharge port of the high antimony electrolytic furnace is then moved through the chute.
  • the chute Connected to the feed inlet of the depletion electrolysis furnace, the chute is equipped with a discharge valve to start or stop the discharge. It is also equipped with a sampling observation port to facilitate sampling from the chute.
  • the flow rate of the melt in the chute is 0.1 ⁇ 0.8 m ⁇ s -1 .
  • the high antimony electrolysis furnace is also equipped with a gas lance that extends into the furnace body and blows inert gas to stir the molten salt.
  • the antimony liquid obtained by electrolysis is discharged from the antimony discharge port, and the sulfur-containing flue gas is collected from the flue gas port.
  • the slag of the depleted electrolytic furnace is discharged from the slag
  • the electrolysis unit in the furnace body includes a cathode located at the bottom of the furnace body and an anode located at the upper part of the furnace body.
  • the anode is connected to an anode guide rod extending out of the furnace body to connect the positive electrode of the power supply through a wire, and the cathode is directly connected to the power supply through a wire. negative electrode.
  • the chemical composition of antimony sulfide concentrate A is (wt. %): Sb 52.91, S 23.12, Si 7.15, Fe 1.61, As 0.53, Al 1.08, Pb 0.29, Ca 0.33, Mg 0.14.
  • the chemical composition of antimony sulfide concentrate B is (wt. %): Sb 32.56, S 28.12, Si 2.51, Fe 5.61, As 2.53, Al 1.12, Pb 0.45, Ca 0.31, Mg 0.28.
  • Example 2 The same raw materials as in Example 1 above. Weigh the mixture of antimony sulfide and molten salt with a ratio of 6:1, place it in a high antimony electrolytic furnace, turn on the thermal resistor to increase the temperature to 850°C, adjust the electrode spacing to 5cm, and turn on the gas spray gun to control the gas pressure to 0.15MPa , the flow rate is 185 L/(min ⁇ m 3 ). Start the power supply and set the current density to 1800 A ⁇ m -2 and the cell voltage to 4.0V. Continue to add materials according to the theoretical consumption. After 15 hours of electrolysis, the crude antimony is released and the sulfur-containing smoke is collected.
  • the remaining high antimony electrolytic furnace melt passes through The chute enters the depleted electrolytic furnace, and 10% of the molten salt is added (calculated based on the melt coming out of the high antimony electrolytic furnace).
  • the temperature in the electrolytic furnace is controlled at 900°C, and the voltage of the tank is controlled at 2 V when the power is turned on.
  • the current efficiency of the entire electrolysis furnace process is 85.8%, the electrolysis energy consumption is 2.83kWh ⁇ kg -1 , and the electrolysis residue contains 0.95% antimony.
  • This comparative example is a single electrolytic furnace gas agitation constant voltage molten salt electrolysis scheme: the same raw materials as the above-mentioned Example 1, according to the patent "A method and device for molten salt electrolysis of antimony sulfide-containing materials (Chinese Patent 202010114724.4)"
  • the plan is to carry out a molten salt electrolysis test. The difference is that the electrolysis cycle is extended to 12 hours, and the amount of feed during the electrolysis process is the same as in Example 1.
  • the current efficiency was 72.85%
  • the electrolysis energy consumption was 3.65kWh ⁇ kg -1
  • the stratification effect of the slag and molten salt was poor
  • the antimony content in the slag was 2.56%.
  • This comparative example is a single electrolytic furnace non-gas agitation constant voltage molten salt electrolysis scheme: the same raw materials as the above-mentioned Example 1, according to the patent "A low-temperature molten salt electrolysis clean metallurgical method and device (Chinese Patent 201710775124.0)"
  • the plan is to carry out a molten salt electrolysis test.
  • the difference is that the electrolysis cycle is extended to 12 hours, and the amount of feed during the electrolysis process is the same as in Example 1.
  • the current efficiency was 65.23%
  • the electrolysis energy consumption was 3.86kWh ⁇ kg -1
  • the antimony content in the slag was 1.58%.
  • This comparative example is the same electrolysis temperature solution for the high antimony electrolytic furnace and the depleted electrolytic furnace: the same raw materials as in the above example 1, weigh a mixture of antimony sulfide and molten salt with a mass percentage of 5:1, and place it in the high antimony electrolytic furnace in sequence. , turn on the thermal resistor to increase the temperature to 900°C, adjust the electrode spacing to 4cm, turn on the gas spray gun to control the gas pressure to 0.15Mpa, and the flow rate to 185 L/(min ⁇ m 3 ). Start the power supply and set the current density to 2100 A ⁇ m -2 and the cell voltage limit to 3.8V. Continue to replenish materials according to the theoretical consumption.
  • This comparative example uses a constant current scheme for both the high antimony electrolytic furnace and the depleted electrolytic furnace: the same raw materials as in Example 1 above, weigh a mixture of antimony sulfide and molten salt with a mass percentage of 5:1, and place them in the high antimony electrolysis furnace in sequence.
  • the furnace turn on the thermal resistor to increase the temperature to 900°C, adjust the electrode spacing to 4cm, turn on the gas spray gun to control the gas pressure to 0.15Mpa, and the flow rate to 185 L/(min ⁇ m 3 ).

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Electrolytic Production Of Metals (AREA)

Abstract

Procédé et appareil de production en continu par électrolyse d'un sel fondu à base d'un minerai contenant du sulfure d'antimoine. Le procédé consiste à : (1) placer un minerai de sulfure d'antimoine et un sel eutectique fondu dans un four électrolytique à forte production d'antimoine en vue d'une fusion électrolytique par chauffage à limitation de tension et à courant constant, lors du processus de fusion, souffler un gaz inerte pour agiter la masse fondue, et évacuer respectivement de l'antimoine métallique fondu et du soufre élémentaire hors d'un orifice d'évacuation d'antimoine du four électrolytique à forte teneur en antimoine et d'un orifice de gaz de combustion du four électrolytique à forte production d'antimoine ; et (2) introduire la masse fondue obtenue après électrolyse à l'étape (1) dans un four électrolytique d'appauvrissement à travers une goulotte en vue d'une électrolyse à dilution à tension constante, compléter avec du sel fondu avant l'électrolyse, évacuer respectivement l'antimoine métallique liquide et le soufre élémentaire hors d'un orifice d'évacuation d'antimoine du four électrolytique d'appauvrissement et d'un orifice de gaz de combustion du four électrolytique d'appauvrissement, et évacuer le laitier après appauvrissement hors d'un orifice d'évacuation de laitier. Selon la conception de la fusion de l'antimoine par électrolyse d'un sel fondu dans deux fours connectés, l'intégralité du processus d'électrolyse peut être réalisé simultanément en vertu de deux paramètres de traitement différents selon les exigences, de telle sorte que l'objectif consistant à obtenir une faible teneur en antimoine dans le laitier d'électrolyse d'un sel fondu, et à séparer le sel fondu du composant de laitier est atteint, et les exigences économiques et de faisabilité de la technologie de production industrielle sont satisfaites.
PCT/CN2023/093924 2022-06-20 2023-05-12 Procédé et appareil de production en continu par électrolyse d'un sel fondu à base d'un minerai contenant du sulfure d'antimoine Ceased WO2023246367A1 (fr)

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CN202210694653.9A CN115012003B (zh) 2022-06-20 2022-06-20 一种硫化锑矿熔盐电解连续化生产的方法及装置
CN202210694653.9 2022-06-20

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CN115012003B (zh) * 2022-06-20 2024-02-06 中南大学 一种硫化锑矿熔盐电解连续化生产的方法及装置
CN115762834B (zh) * 2022-12-01 2024-05-31 中国原子能科学研究院 熔盐净化装置和熔盐净化方法

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CN104313643A (zh) * 2014-07-31 2015-01-28 贵州重力科技环保有限公司 一种两段熔盐电解法生产高纯锑的方法
CN107326400A (zh) * 2017-08-31 2017-11-07 中南大学 一种锑的低温熔盐电解清洁冶金方法及装置
CN111172563A (zh) * 2020-02-25 2020-05-19 中南大学 一种含硫化锑物料熔盐电解的方法及装置
CN115012003A (zh) * 2022-06-20 2022-09-06 中南大学 一种硫化锑矿熔盐电解连续化生产的方法及装置

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