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WO2020132752A1 - Installation moderne de production de trioxydes d'antimoine, d'arsénic, ainsi que de plomb métalliques - Google Patents

Installation moderne de production de trioxydes d'antimoine, d'arsénic, ainsi que de plomb métalliques Download PDF

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Publication number
WO2020132752A1
WO2020132752A1 PCT/CL2018/000045 CL2018000045W WO2020132752A1 WO 2020132752 A1 WO2020132752 A1 WO 2020132752A1 CL 2018000045 W CL2018000045 W CL 2018000045W WO 2020132752 A1 WO2020132752 A1 WO 2020132752A1
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Prior art keywords
antimony
lead
arsenic
phase
gases
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Spanish (es)
Inventor
Julio Domingo BUCHI GATICA
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Minera Pargo Minerals SpA Cia
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Minera Pargo Minerals SpA Cia
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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
    • C22B1/00—Preliminary treatment of ores or scrap
    • C22B1/02—Roasting processes
    • C22B1/04—Blast roasting
    • 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
    • C22B13/00—Obtaining lead
    • C22B13/02—Obtaining lead by dry processes
    • 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
    • C22B30/00—Obtaining antimony, arsenic or bismuth
    • C22B30/02—Obtaining antimony
    • 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
    • C22B30/00—Obtaining antimony, arsenic or bismuth
    • C22B30/04—Obtaining arsenic
    • 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
    • C22B5/00—General methods of reducing to metals
    • C22B5/02—Dry methods smelting of sulfides or formation of mattes
    • 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
    • C22B5/00—General methods of reducing to metals
    • C22B5/02—Dry methods smelting of sulfides or formation of mattes
    • C22B5/08—Dry methods smelting of sulfides or formation of mattes by sulfides; Roasting reaction methods
    • 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
    • C22B5/00—General methods of reducing to metals
    • C22B5/02—Dry methods smelting of sulfides or formation of mattes
    • C22B5/16—Dry methods smelting of sulfides or formation of mattes with volatilisation or condensation of the metal being produced

Definitions

  • the present application considers a Plant for the Obtaining of Antimony Trioxide, Arsenic Trioxide and metallic Lead from a mineral, predominant in Antimonite or Stibine (Sb2S3) and of other sulfided minerals of Arsenic (As) and Lead (Pb) contained in the mineral, which chemically contain on average 30% Antimony, 4% Arsenic and 10% Lead.
  • the designed plant has a mineral treatment capacity to produce 300 t / month of Antimony Trioxide (Sb 2 0 3 ), 44 t / month of Arsenic Trioxide (AS2O3) and 89.7 t / month of Lead (Pb) metallic, considering a global metallurgical recovery of 90%, as well as being environmentally sustainable from the gaseous and solid waste generated point of view.
  • Sb 2 0 3 Antimony Trioxide
  • AS2O3 Arsenic Trioxide
  • Pb Lead
  • Antimony Trioxide from metallic sulphide minerals are based on the ease of oxidation between the elements present, arsenic, tin, antimony and lead, which decreases in the following order:
  • Antimony is partially oxidized as long as the concentrate or mineral contains arsenic and tin, and only when these two elements are oxidized, the oxidation of the antimony increases, while the oxidation of lead does not begin until all the antimony is oxidized.
  • Arsenic (As) and Tin (Sn) in the mineral rich in antimonite must be kept in mind before generating the complete oxidation of antimony (Sb).
  • Arsenic (As) its trioxide sublimes at 465 ° C, which facilitates its separation in melting or roasting pyrometallurgical processes. It should be borne in mind in the selection of the process for obtaining antimony trioxide (Sb) that the melting point of antimony (Sb) is 630 ° C and its trioxide
  • the need for air abundance is due to the fact that its oxidizing power decreases when mixed with the gaseous products of oxidation, reducing it by up to 50% of its value.
  • the roasting speed is accelerated, increasing the speed of release of the gaseous products and their replacement by pure air.
  • the speed and also the finish of the roasting are influenced by the size of the raw material.
  • the roasting speed has a maximum point, from the economic point of view, since when exceeding it, the losses of the material in the form of dust that carry the exhaust gases, do not compensate the increase in speed, since the recovery of these powders is expensive.
  • the factors that control roasting are: temperature and time.
  • the heat necessary to carry out the oxidative roasting is produced by the combustion of a fuel, either alone or mixed with the load, or using the heat caused by the exothermic reactions between the mineral and the oxygen in the air.
  • heating is carried out at high temperature with reducing reagents (coke) to originate a molten metal or an alloy or other product, but always in the state molten. (9.2. Pyrometallurgical extraction. Antimony Metallurgy Course, Antonio Ros Moreno, 2009).
  • Antimony trioxide is obtained from the antimonite mineral by roasting it in conventional ovens. Rotary roasting ovens are the most commonly used today. The antimonite beneficiation process mainly depends on the content of antimony and other minerals present.
  • the antimony trioxide is obtained by roasting the antimony sulfide, antimonite (Sb2S3), in conventional roasting ovens. Sulfur roasting is a Gas-Solid reaction process in a (special) furnace in which large amounts of air, sometimes enriched with oxygen, are brought into contact with the sulphide ore concentrates.
  • Antimony sulfide is oxidized to antimony (III) oxide (volatile in roasting) or to antimony (IV) oxide (nonvolatile).
  • Non-volatile antimony (IV) oxide Control of the furnace in the production of non-volatile antimony (IV) oxide is relatively simple, however the oxide does not separate from the residue, to the detriment of the trioxide obtaining efficiency.
  • Roasting has the advantage that S ⁇ 203 volatiles are selectively produced in 98% yield and separated from the gangue, which contains the precious metals in a recoverable form. However, it is difficult to control the oven and temperature.
  • the oxide forms between 290 and 340 ° C in an oxidizing atmosphere, and the reaction rate peaks at 500 ° C, at which antimony (IV) oxide begins to form.
  • the impurities that come to Present in the products are carried away by the gases of sulfur dioxide (SO2) or Antimony Trioxide (Sb 2 03), as the case may be.
  • SO2 sulfur dioxide
  • SB 2 03 Antimony Trioxide
  • antimony (IV) oxide forms:
  • antimony (IV) oxide can react with antimony (III) sulfide and fresh Cervantine, resulting in antimony (III) oxide when the reaction is gestated with low presence of Oxygen (0 2 )
  • the process should be designed so that antimony (III) oxide (Sb 2 0 3 ) is formed quickly and preferably.
  • the temperature must be high enough to guarantee adequate volatilization and the oxygen supply must be kept low to inhibit the formation of antimony (IV) oxide.
  • the temperature is too high, part of the charge melts on other sulphide grains, and prevents optimal oxidation.
  • the oxygen content in the gas phase must be kept low enough to prevent the formation of antimony (IV) oxide.
  • the temperature level is governed by the sulfur content in the mineral.
  • Low grade antimony sulfide minerals (Sb 2 S3) can be roasted between 850 and 1000 ° C.
  • the upper limit is the sulfide melting point (546 ° C); in practice, the temperature should not exceed 400 ° C.
  • the degree of oxidation is controlled by charcoal or coke powder, combined with the charge, admitting only the amount of air necessary to form carbon monoxide and antimony (III) oxide. Carbon monoxide inhibits oxidation to antimony (IV) oxide. Regardless, the formation of antimony (IV) oxide cannot be completely suppressed. In the first condensation, antimony (IV) oxide, lead (II) oxide and smoke powders are obtained. Antimony (III) oxide condenses second, and volatile arsenic (III) oxide last.
  • the oxygen concentration in the furnace is too low, partial oxidation can occur and give a mixture of oxide and molten sulfide at 485 ° C. If the oxygen concentration is too high, it can form arsenates and antimoniates of lead, copper and others. metals that pass into the slag. If the antimony oxide consists of very fine crystals, which adhere firmly to the fingers and do not agglomerate, it is considered to be of good quality. The oxide must be white, a reddish tint indicates the presence of antimony (III) sulfide. The yellowish tone is due to selenium and lead (II) oxides. The arsenic content should be in the order of 0.1%.
  • antimony according to the requirement of fluxes such as hematite, limestone and charcoal, these materials are fed into hoppers with the purpose of mixing in defined proportions. This mixture subsequently feeds a cyclone oven 81 cm in diameter and 130 cm high, where the antimony volatilization process begins with preheated air to obtain an intermediate product called impure antimony trioxide and whose antimony trioxide laws reach content.
  • the powders are recovered in bag filters and electrostatic filters, this material is pelletized with fluxes such as sodium carbonate (Na2CC> 3) and charcoal which is reduced in short drum rotary kilns, to obtain 99 metal antimony. to 99.2%.
  • the metal is refined in stationary type furnaces (reverberatory furnace), until purities of 99.5 or 99.6% are achieved, eliminating mainly arsenic and iron.
  • the oxidation of metallic antimony (regulus) depends on the market for antimony trioxide, which is carried out in an electric furnace to produce trioxide.
  • high purity antimony (Sb 2 C> 3) 99.5% Sb 2 C> 3).
  • This study shows the arrangement of the cyclone kiln and electric kiln of an antimony plant that treat antimony concentrates shown in the process described above, to produce antimony by oxidation / reduction, considering the grade of the mineral shown, 498 kg S0 are produced 2 / t mineral (174 m 3 S0 2 / t mineral).
  • Roasting is a preparatory operation for pyrometallurgical-type minerals. In its oxidizing form, it is used to transform metallic mineral sulphides into oxides and / or sulfates, by reaction with oxygen in the air at temperatures between 500 and 900 ° C, facilitating extraction by both methods.
  • the corresponding chemical-physical system is composed of: metal, sulfur and oxygen (Me-SO), and supports a maximum of five phases in equilibrium. When operating at constant temperature they are reduced to four. Three are combinations of the metal, its sulphide, its oxide and its sulfate, and the fourth is made up of a mixture of gases subjected to an external pressure of 1atm.
  • Roasting consists of changing the chemical composition of a metallic mineral by reaction at high temperature, but without changing its solid state, with the gaseous substances in the furnace's atmosphere.
  • Roasting like calcination, is an operation of a chemical nature but, unlike this, it is not intended to eliminate inert matter but only to transform it, its effects on the metallic concentration of ores are few.
  • Roasting is a preparation applicable to both pyrometallurgical and hydrometallurgical extraction, since its purposes are diverse depending on the nature of the mineral: oxides, sulfides, etc., and the gaseous reagent used: oxygen, carbon oxide, chlorides, being able to distinguish, depending on the latter, in three basic types: oxidizing, reducing, and chlorinating, of which the most characteristic is the first, carried out on sulphides in the presence of air, which corresponds to the strict concept of the term.
  • the oxidizing roasting can be carried out under the modality of death, or complete, and partial, and the latter can be sulfating or non-sulfating. In roasting to death, the sulfide is completely oxidized to facilitate its subsequent reduction by carbon.
  • the sulfur content is decreased to later be able to form a molten phase of sulphides or matte that concentrates the metal; in the sulfant, a part of the sulfur remains as sulfate, to make it soluble in aqueous media.
  • MeS (s) + 3/20 2 (g) MeO (s) + S0 2 (g); DH (T); AG (T)
  • the enthalpy variation of this reaction at temperature T can be made by adding the formation heats in standard conditions of oxide and sulfide, the sensible heat of the system between 298 ° K and T (K), given by its equivalent specific heat: (Cp), according to the equation:
  • roasting is an exothermic operation that requires, for its autogenous development, that the charge reaches the ignition temperature in its reaction zone.
  • the operation proceeds in countercurrent of mineral and gases in such a way that the metallic sulphide: MeS, accompanied by a gangue of other sulphides, generally pyrite and various silicates, gradually heats up as it moves through the reactor from its entrance through the upper part of the rear cylinder head and makes contact with the combustion and roasting gases that in the opposite direction run through the furnace from the front cylinder head to the rear cylinder, in this way the reaction zone until reaching the ignition point is reached at an intermediate point of the reactor , which causes the toasted ore (gangue) to move away from the reaction zone, cooling with the air that enters from the outside, through the discharge opening of this material.
  • T’f outlet of the solids, and Tf, of the gases are different.
  • DH (MeS MeO) AH (MeO + G) (298 Tf) + AHS0 2 (298 T'f) + q
  • the start or priming of the operation requires external input of heat, providing the reactor with the necessary elements for this purpose.
  • the temperatures are regulated so that they do not excessively exceed the ignition temperature or fall below it, graduating the air supply or recycling or extracting sensible heat.
  • the heat balance: q, of the operation varies with the nature of the sulfide, the richness of the ore, and its pyritic content, being able to recover to produce high pressure steam in the reactor itself or outside it.
  • the sulfides with the highest degree of sulfidation such as pyrite: FeS2
  • FeS2 pyrite
  • S sulfur
  • O oxygen
  • the currently most used method is the reduction of the sinter of lead oxide, which in turn is produced by sintering roasting of lead concentrates (galena), mixed with fine recycled sinter and lead sulfate, among others, in sintering.
  • the purpose of this stage is to remove the sulfur from the concentrate as Sulphurous Anhydride (SO2) and to form an appropriate solid mass to load in the reduction furnace.
  • SO2 Sulphurous Anhydride
  • Dwight-Lloyd proceeds at 800-850 ° C and the main reaction is the oxidation of the galena to Lead Oxide (PbO) with generation of Sulphurous anhydride (S0 2 ) according to:
  • the reaction is maintained at 800-850 ° C by diluting the charge with recirculated sinter fines since the melting point of Oxide and Lead (PbO) is 886 ° C and the
  • the sinter contains 40-50% Pb, 1-10% Zn, 1-2% S, 8-10% Si02, 5-8% CaO and 12-15% Fe203. This is crushed and harneanea to have a load of -37 + 1/4 "for the next stage of reduction with coal.
  • a patent published in 1985 describes a method of producing metallic lead, from lead-containing starting materials, by melting the starting materials under oxidation conditions and reducing the resulting oxidized melt, characterized by reducing the melt with agent reducing solid carbonaceous in the melt and ensuring that the carbonate-containing solid material is present in the melt along with the reducing agent.
  • this background describes an optimized process to obtain Lead, by oxidation of the mineral and then reduction with the help of carbonates, which must be added to the molten material.
  • a process for obtaining arsenic trioxide, of more than 98% purity is described.
  • the theoretical basis of this invention is based on the lower constant of the solubility product of antimony trioxide (Sb 2 C> 3 ) with respect to Arsenic trioxide (AS2O3), as well as the adequate adjustment of the solid-liquid ratio and the acidity of the medium; aspects that preferably favor the hydrolysis of the antimony oxychlorinated complexes, which causes their separation from the solution, the arsenic remaining in it.
  • the procedure object of the patent consists of diluting the alkaline solution, which contains arsenic and antimony, with acid with HCI of concentration 4.5 to 5.5 mol / L, until causing the separation of more than 94 % of the latter element, by filtration, this solid constituting an antimony concentrate.
  • the antimony trioxide crystals Sb 2 C> 3 are obtained.
  • FIG. 1 A more detailed description of the industrial plant (Fig. 1) is presented below, which will basically consist of the following two phases of a series of equipment that account for pyrometallurgical processes: First phase: Equipment and processes involved in the volatilization and formation of the Solid Mixture of Products of Interest.
  • This first phase consists of equipment for a controlled oxidizing roasting process, of sulphided minerals at temperatures between 480 and 520 ° C, in rotary kilns inclined longitudinally (between the rear and front cylinder heads of them) and lined internally with refractories , and lifters installed between the rear cylinder head and half its length, which allow the load to be lifted to the highest point of the furnace and so that it spreads in its vertical fall on the gas stream.
  • the supply of the mineral to the furnaces is continuous entering them through the upper part of the rear cylinder head of these, against the current of the combustion gases and the induced air that enter through the front cylinder head of these.
  • the heat required to reach the process operating temperature, between 480 and 520 ° C, in the kiln exhaust gases, is generated with a natural gas burner installed in the center of the front cylinder head of the kiln inserted in the Corresponding combustion chamber, allowing a quantity of heat that makes it possible to generate a temperature greater than 500 ° C at the entrance of the furnace, overheating the outgoing calcined material and ensuring the exit temperature of the furnace with the volatilized products of interest.
  • the mineral material that does not volatilize will remain inside the furnace, which is mainly made up of a mineral gangue and that will be continuously evacuated by the discharge of the furnace located in the lower area of its previous cylinder head, and whose runoff is generated as a result of the vertical inclination that the furnace presents between its rear cylinder head and the previous one.
  • the calcined gangue leaving the furnace is transported to cooling wells, three in total, in which the material is deposited for its subsequent cooling and removal to its final destination, dump or return to the place of origin, the deposit.
  • the three wells will rotate, fulfilling a specific function, either of reception, cooling or removal of the material.
  • the mineral generally has the following generic composition:
  • the received mineral will be treated in three identical lines of operation (Plant), as detailed in the flow diagram that is part of the drawings in Fig. 1.
  • This first phase consists of equipment for a controlled oxidizing roasting process of sulphided minerals at temperatures between 480 and 520 ° C, in rotary kilns (2) inclined longitudinally (between the rear and front cylinder heads of them) and lined internally with refractories, and lifters installed between the rear cylinder head and half its length, which allow the load to be lifted to the highest point of the furnace, so that it spreads in its vertical fall on the gas stream.
  • a sedimentation chamber is a container with an inlet on one side and an outlet located on the opposite side frontally or on top of it, generally of rectangular geometry its central part, where a gas stream is allowed to expand in such a way In this way, the velocity of the gas within it decreases considerably, allowing the action of gravity to settle the particles it carries.
  • the cross section of the equipment is much greater than that of the pipeline that approaches it so that the gas can expand and consequently slow down. Hoppers are used that collect the separated solid in the lower part of the same, from where it is removed by means of a drag chain to be sent to its next destination.
  • the dust collection system is completely well sealed to prevent air from entering through it, which can increase turbulence in the equipment and consequently re-incorporate the removed particles back into the stream.
  • baffle plates that of baffle plates or Howard's model and that of expansion chambers.
  • a sedimentation chamber is a container with an inlet on one side and an outlet located on the opposite side frontally or on top of it, generally of rectangular geometry its central part, where a gas stream is allowed to expand in such a way In this way, the velocity of the gas within it decreases considerably, allowing the action of gravity to settle the particles it carries.
  • the cross section of the equipment is much greater than that of the pipeline that approaches it so that the gas can expand and consequently slow down. Hoppers are used that collect the solid separated at the bottom of it, from where it is removed by means of a drag chain to be sent to its next destination.
  • the operation of the cyclone in this process is applied to those mineral particles that remain in the gas stream (preferably gangue) and that were not recovered in the previous process, with an approximate diameter of less than 20pm.
  • the cyclone is essentially a sedimentation chamber in which gravitational acceleration is replaced by centrifugal acceleration.
  • Cyclones are one of the least expensive means of dust collection, both from an operational and investment point of view. These are basically simple constructions that do not have moving parts, which facilitates maintenance operations; They can be made from a wide range of materials and can be designed for high temperatures (up to 1,000 ° C) and operating pressures. Cyclones are suitable for separating particles with diameters greater than 5 pm; although much smaller particles, in certain cases, can be separated. Cyclones have higher efficiencies than the gravitational sedimentation chamber, and lower efficiencies than pan filters, scrubbers, and electrostatic precipitators.
  • the centrifugal force generated by the gyrations of the gas within the cyclone can be much greater than the gravitational force, since the centrifugal force varies in magnitude depending on the speed of the gas's rotation and the radius of gyration.
  • increasing the speed of entry to the cyclone would imply an increase in the centrifugal force and, therefore, an increase in efficiency; however, very high input speeds generate the resuspension of particulate material from the internal walls of the cyclone, which decreases the efficiency of the cyclone; Additionally, increasing the input speed implies higher energy consumption.
  • the duct that constitutes the radiative cooling system must be dimensioned for high conduction velocity in order to avoid sedimentation of particles inside, which will be generated by solidification of the volatile products upon reaching their dew point due to the fact that their length a decrease in gas temperature of at least 250 ° C will be caused, a range in which the volatile compounds present (AS 2 O 3 , Sb 2 0 3 and PbO) condense.
  • the high speed required and downstream pressure drop in the gas handling system is compensated by the inclusion of a Booster extractor at the inlet of the radiative cooler.
  • the mixture of solid particles of the interesting products Antimony Trioxide (Sb 2 0 3 ), Trapped Arsenic Trioxide (AS 2 O 3 ) and Oxidized Lead (PbO), are removed from the sleeves by an intermittent vibration mechanism, as well as by the emission of pressurized air pulses, which cause them to come off.
  • the obtained product mixture is pneumatically transported to the feeding system of the next phase of the process.
  • the dust present in the gases is separated by passing this gaseous current through filtering tissues, which retain the solid particles present.
  • the operation basically consists of forcing the passage of the gas stream through the filter medium (tissue), whose mission is to retain the dust transported by the gas, accumulating on it and generating a layer that favors the efficiency of the filtration of the smaller particles.
  • the filter medium tissue
  • the pressure drop of the gas through it increases. Therefore, there comes a time when it is necessary to detach the accumulated dust layer to recover the functionality of the equipment, this action being carried out by means of pressurized air pulses in the opposite direction to the passage of gas.
  • Filter surfaces are bag-shaped or sleeves inserted into cells or filter compartments neatly in a number of 10 or more units.
  • the filter is made up of several cells in operation or sealed. It is a device that has high purification yields, even for very fine particles, whose usual yield values are from 99% to 99.9%, for sizes in the sub-micron range up to several hundred microns. Bearing in mind that they cannot operate in humid environments or near the dew point of the gas stream, such as treating adhesive or binder powders, since there is a risk of clogging of the fabric as the wet dust adheres to them after cleaning. Regarding its design, the most important data is the gas flow to be treated, marking the size of the equipment and, consequently, the investment cost.
  • the main design variable of the bag filter is the A / C ratio (actual gas flow and the collection surface) or filtration speed expressed in m / s, and the other important operating parameter is the total pressure drop in the equipment, which determines the energy need to supply gas through the equipment.
  • outgoing gases from the bag filter containing sulfur dioxide (SO2) will enter a packed Gas Cleaning Tower (7) (Gas Washers) where counter current spraying of lime milk 10% dilution on the gas that rises through the packaging material neutralizes S02, generating Plaster (CaS0 3 ) diluted in water, which is removed from the system for final disposal.
  • the clean gas leaving the tower is propelled by the effect of an extractor to the Chimney (8) for gas evacuation from the Plant.
  • Gas scrubbers are gas-liquid contact equipment, in which the liquid acts as a collector of polluting compounds in the gas stream. With the proper design, removal efficiencies of 99% are achieved.
  • the clean gas outgoing from the washing tower consisting mainly of combustion gases and water vapor, is transported and driven by the action of the Extractor that shares and supports the handling of gases from the operational cooling system to their evacuation through the Chimney. .
  • the unique chimney of the plant has the function of evacuating the clean gases from the process and that are emitted at the height that the establish environmental regulations, ensuring the minimum environmental impact on the environment and the surrounding community.
  • This Second Phase of the process is carried out in several teams, starting in a double chamber fixed furnace (reverberation type) with burners (Figs. 2 and 3), one for each chamber inclined towards the floor of the crucibles to avoid dragging of Fine powder (10) that characterizes the mixture of Antimony (Sb), Arsenic (As) and Lead (Pb) oxides, recovered in the Sleeve Filter (5) of the previous stage.
  • the temperature of the process in the oven is between 480 and 520 ° C, in order to generate volatilization of the products of interest, Antimony Trioxide (Sb 2 0 3 ) and Arsenic Trioxide ( AS 2 O 3 ) that are separated according to their different solidification temperatures in equipment other than the Gas Management system, as shown in Fig. 1 below, where Sb 2 C> 3 is recovered in a Radiative Cooling (CER) (12) that operates at the 350 ° C level and the AS 2 O 3 at the end of the system in the Sleeve Filter (FM) (14) at a temperature below 100 ° C.
  • CER Radiative Cooling
  • FM Sleeve Filter
  • this 2nd phase is performed in a dual - chamber furnace (Fig.2 and 3) in two sub-stages, which in Fig 1 are described, and we can detail it as follows:
  • a Radiative Expansion Chamber (12) (Fig. 3 and 4) is used, whose function is to recover the Condensed Antimony Trioxide from the gas flow.
  • the content of the mineral fed to the process has been conditioned to carry out the balance, complying with the following characteristics:
  • TMS dry metric tons
  • the feeder mineral of the process would be composed according to what is shown in Table 1, where the mass of each component is expressed in dry Kg per hour. In this way, taking one hour of production as the basis for calculation, the roaster is fed 1,309.2 kg / h of ore, with 7% humidity. It is considered that 100% of the gangue present in the mineral corresponds to silica (S1O2)
  • Table 1 Composition of the feeder mineral of the process, by elements and mineralogical species.
  • Fig. 1 shows the diagrams of the process and equipment (Plant) for obtaining antimony trioxide, divided into two phases.
  • the first one the volatilization of oxides, cooling and cleaning of oxidation gases are carried out.
  • the second phase divided into two sub-stages per production batch corresponds to the separation of antimony, arsenic and lead oxides, reduction of the latter liquid lead oxide (Pb) and cleaning of reduction gases.
  • the final products of the process are, arsenic trioxide, Pb in ingots and antimony trioxide, as the main product.
  • the chemical reactions of interest that are carried out in the first phase of the process are:
  • the probability of each one occurring is conditioned by various factors, such as: temperature and pressure, among others.
  • the mass balance of the process is carried out in the main equipment, where the aforementioned chemical reactions are carried out and the energy balance is carried out in the same way.
  • Mass balance in the toaster As mentioned above, the feed to the toaster corresponds to 5,219.6 kg / hr of ore that is brought to a temperature between 480 and 520 ° C, by means of a natural gas or diesel oil burner, depending on the facilities of the region where the technology in question is installed. Heat losses in the main equipment are considered close to 10% and the efficiency of the fuel used is assumed to be close to 98%.
  • Table 2 shows the mass of the main roaster output products, considering the three roasting lines as one.
  • the oxidation of the galena (PbS) is carried out by blowing the necessary air downstream of the toaster, to guarantee its oxidation outside this equipment, thus avoiding losses of this oxide in the expansion chamber and in the cyclone.
  • the fuel flow required for roasting is 278.8 l / h and the air required for combustion is 2,755.8 Nm 3 / h.
  • the air for oxidation of the mineral in the roaster is 865.0 Nm 3 / h.
  • Arsenic and Antimony and Galena volatilized are assimilated to Air, in terms of the volume occupied. In this case, the mass to volatilize is 608 kg / h. Volatile flux is calculated under normal conditions.
  • Galena oxidation as specified above, galena oxidation is performed outside the roaster as indicated in Fig. 1 and the chemical reactions associated with such oxidation are numbers (3) and (4), listed previously. The corresponding material balance indicates that the air flow required for this purpose is 123.1 Nm 3 / h.
  • the gases resulting from the first stage of the process, reaction and combustion gases, are directed to a washing tower, in which 10% w / w lime milk is contacted, to generate conditioned gases to comply with the corresponding regulations. and be eliminated into the environment through a fireplace.
  • Table 4 shows the flow of gases sent to the washing tower, generated in the first stage of the process.
  • Abatement of Sulfur Dioxide (SO2) in the washing tower is as follows:
  • Table 4 Flow of inlet gases to the Washing Tower.
  • the second phase of the process is carried out in two cycled sub-phases for each charge introduced into one of the furnace chambers, where it will accumulate, the sufficient amount of PbO that generates the adequate volume of Pb metallic to be continuously molded.
  • the time required in the first sub phase is estimated at two days to start the second sub phase.
  • the first of these which is carried out at a temperature between 480 and 520 ° C, in a fixed reverberatory type furnace with burners in the vault, corresponds to the volatilization of the Arsenic and Antimony trioxides that made up the mixture of oxides together with PbO and recovered in the first stage bag filters.
  • Lead oxide which does not volatilize, remains in the reactor and accumulates to be reduced with coke in the second mineral charge sub-stage.
  • Sb 2 0 3 one of the final products of the process, is captured in a Radiative Cooling Chamber because its condensation occurs between 350 and 400 ° C, and reaches 418.0 kg / hr, which corresponds to a monthly production of 300 tons.
  • Table 5 Exit gases from the first ore-charging sub-phase reactor.
  • the lead oxide retained in the reactor is reduced with Coke Coal, according to the following chemical reactions.
  • the Pb product of said reduction is 115.7 kg / h, so it will be necessary to accumulate the metal inside the oven, to achieve an adequate bleeding height. It is estimated that after 2 days of accumulation, the optimal height of approximately 40.8 cm is generated, considering that the dimensions of each crucible in the furnace is 1.2 m 2 (0.6 x 2.0 m 2 ) of basal area and that the density of Pb is 11, 35 gr / cm 3 .
  • the gases generated in the Lead oxide reduction process are negligible compared to those required to maintain the furnace temperature between 480 and 520 ° C and the Lead oxide that accumulates inside, along with carrying out the volatilization of Antimony and Arsenic trioxides, even more so if the only contribution of gas is due to the formation of carbon dioxide (CO2), at a rate of 6.36 Nm / h during this process, representing 0.2% of the total gas outgoing from the oven.
  • CO2 carbon dioxide
  • the volatile gas mixture generated in the roasting process (in a First Phase of the Obtaining process) undergoes different cooling processes to obtain a solidified mixture of it at the end of the gas handling system (Sb203, AS2O3 and PbO) .
  • the oxidation of Lead Sulfide (PbS) to Lead Oxide (PbO) is induced by injecting air into the gas handling system, through a controlled valve installed at the inlet of one of the components of the cooling system.
  • the condensed mixture at the end of this system is made up of Antimony Trioxides (Sb) and Arsenic (As) and Lead oxide (Pb) and is recovered in a Bag Filter that operates below 100 ° C.
  • the outgoing gases from the bag filter containing sulfur dioxide (SO2) enter a packed gas scrubber where by countercurrent spraying of 10% dilution lime milk onto the Gas that rises through the packaging material neutralizes the sulfur dioxide (SO2) generating Plaster (CaS04) diluted in water, which is removed from the system for final disposal.
  • SO2 sulfur dioxide
  • CaS04 Plaster
  • the non-volatile material of the mineral, the calcined mineral gangue is removed from the furnace, it is transported, together with the powders dragged by the outgoing gases from said equipment and recovered from the gas handling system, to cooling wells, three in total in that the material is deposited for its subsequent cooling and removal to its final destination, dump or return to the place of origin, the deposit.
  • the three wells will rotate, fulfilling a specific function of receiving, cooling or removing the material once it has cooled.
  • the solidified mixture of oxides obtained at the end of the first phase of the process undergoes a second phase with a fixed double chamber oven similar to a reverberation, which inhibit dust entrainment and maintain the oven temperature between 480 and 520 ° C, where by taking advantage of the physical properties inherent in the products to be obtained, they are separated and obtained as commercial products.
  • the process at this stage is subdivided into two production batch operations, as follows:
  • Fig. 1 shows with a block diagram the Plant for obtaining antimony trioxide, arsenic trioxide and metallic lead.
  • Antimonite mineral feeding system which is characterized by being made up of sulfur minerals predominantly Antimony, Arsenic and Lead, whose average contents fluctuate between 20-30% Antimony (Sb), 2-4% Arsenic ( As) and 5-10% of Lead (Pb), which is fed from the storage field to the feed hoppers of the Toasters through a transport circuit consisting of three conveyor belts, to raise the mineral load from the level from the storage field to the horizontal belt feeding mailbox that distributes the mineral to the feeding hoppers to each Toaster, from where it is continuously extracted by means of a channel-type endless screw being transferred to a second screw perpendicular to the previous one, tubular that deposits the load inside the toaster adequately away from its rear end and on the refractory lining and the lifters inside the Toaster.
  • the air to generate the oxidation of Antimony and Arsenic is induced by the draft exerted by an induced draft fan, located upstream in the Gas Management system (between the Bag Filter and the Gas Washing Tower) towards the interior of the toaster, which is why the burner head wall (above) will consist of an adequate number and size of holes, distributed symmetrically in relation to its horizontal axis, each one having a controlled valve for the regulation of the quantity of air to infiltrate in benefit of the adequate oxidation of trioxides in formation.
  • Arsenic and Antimony, and Galena leave the Toaster at a temperature between 480 and 520 ° C, enter an Expansion or Sedimentation Chamber for gases whose function is to reduce the initial velocity of gases (less than 3 m / s) and recovering most of the particles carried by the gas stream, eliminating the largest ones (greater than 20 pm), as well as reducing the temperature of the outgoing gases.
  • Said chamber consists of a lower section of inclined walls that discharge the recovered material to a channel-type endless screw, which collects the gangue dust particles decanted in said chamber and which also collects the gangue particles. separated from the gas flow in the cyclone that precedes it.
  • the Expansion Chamber allows a moderate decrease in the temperature of the gases.
  • the dimensioning of such equipment is closely linked to the knowledge of the nature of the motion of a particle that moves within a fluid, which conforms to the model proposed by Stokes known as Stokes' law.
  • the outgoing gases flow from the Expansion Chamber goes to a second cleaning operation in a Cyclone, equipment that removes the particulate material still present in the gas stream, based on the principle of inertial impaction, as the gaseous flow loaded with particles enters tangentially into the upper cylindrical zone, taking advantage of the increased speed in its circulation and the centrifugal force generated by the rotation of gases and solid particles, the latter, due to their The heavier the weight, they will come out through the Cyclone underflow and the particle-free gases through the overflow. Given the high speed reached by the gases in the process, greater than 20 m / s, the effect of heat losses due to radiation is low, which is why it is estimated that the temperature of the gases when leaving this equipment does not present large variations .
  • the Expansion Chamber and Cyclone assembly generates a temperature decrease of around 150 ° C.
  • the products of interest are Arsenic Trioxide (AS2O3), Antimony Trioxide (Sb2C> 3) already formed and volatilized in roasting and Lead (Pb) in the form of PbS, and that are present in the outgoing gases at 350 ° C of stage 3, said gases will be subjected to a Radiative Cooling process, which is described below.
  • this Galena gases must be oxidized and condensed as lead oxide (PbO), for which the air required for oxidation is induced by the action of the Induced Draft Fan through a controlled opening valve installed at the inlet of this cooling system.
  • PbO lead oxide
  • Said cooling system is made up of parallel coils made up of a series of inverted U's joined together (each one constituting a branch of the system).
  • the gas entering the equipment circulates inside it to cool down from 350 ° to less than 100 ° C, dissipating the latent heat of the gases through the walls of the coils that make up the equipment, releasing this heat through convection phenomena and mainly radiation, into the atmospheric air that surrounds it and circulates around it.
  • the duct that constitutes this cooling system must be dimensioned for a high conduction speed in order to avoid the sedimentation of particles that condense as the temperature decrease advances and the solidification of the volatile products of interest.
  • the heat dissipation capacity according to the pipe size that according to the coil defines the length required for the decrease in the temperature of the gases pursued, which in this case is around 250 ° C.
  • the mixture of solid products consisting of Antimony Trioxides (Sb20 3 ) and Arsenic (AS2O3) powders and Pb oxide (PbO), is removed from the FM by means of a rotary valve, which discharges onto a conveyor chain (harrow) to feeding the material hopper the pneumatic transport system that moves the oxide mixture to the feed hopper 2 to Phase (Separation of Commercial Products).
  • VTI induced draft fan
  • equipment causing the movement of the generated gases in the processes that make up the 1st phase, ie from the Rotary Kiln (Toaster) to the outlet of the baghouse and subsequently boost the outgoing gases from this equipment to a single Gas Cleaning Tower (TL) and cause the evacuation of the pollutant-free gases to the single chimney of the plant.
  • VTI induced draft fan
  • the gases generated by the formation and oxidation of the products of interest contain Sulphurous Anhydride (SO2), which must be neutralized and removed from the gas stream, an operation that is carried out in a Washing Tower, in which apply lime milk as a neutralizer, allowing the transformation of SO2 to Hydrated Gypsum (CaS0 4 * 2H 2 0), a compound that is collected in the liquid retention tank of said Tower.
  • SO2 Sulphurous Anhydride
  • Hydrated Gypsum CaS0 4 * 2H 2 0
  • the 10% dilution lime slurry descends on the gas that rises through the packaging material, thus causing the neutralization of the S0 2 contained in it.
  • These teams are based on the phenomenon of gas absorption in liquid, for which their operation depends on achieving intimate contact between them. To achieve such contact, the gas and / or liquid exposure surfaces must be maximized, which in packed towers occurs by dividing the liquid into an infinity of thin films of the same, low speed, through the type of packaging, in this
  • the clean gas outgoing from the washing tower consisting mainly of combustion gases and water vapor, is driven by the action of a VTI towards its evacuation through the single chimney that will emit the total of clean gases generated by the process, both of its Phase 1 and Phase 2 through at the level that establishes environmental regulations in force, ensuring minimal environmental impact on the environment and the surrounding community.
  • a double reaction chamber fixed oven receives the mixture of solid products from its feed hopper, in which it is carried out at a temperature between 480 and 520 ° C, volatilization of Antimony trioxide (Sb 2 0 3) and arsenic (As 2 0 3) constituting the mixture of oxides generated in the 1 Phase (Sleeve Filter) and retention of the Pb oxide (PbO) that does not volatilize in it, in order to separate the volatilized products according to their different condensation temperatures in different equipment upstream in the Gas Management system of this Phase 2.
  • the mixture of solid products transferred from the 1st to the Phase are fed into the Fixed Furnace (reverberation type) whose crucible has been divided into two equal chambers separated by an interior longitudinal wall, being joined together at the gas phase level, which they take advantage of the heat generated by two burners installed on their rear walls, from each chamber, which with an inclination of 20% and a flame of adequate length, point towards the floor of the corresponding crucible, countercurrent to the flow of gases leaving the furnace, a condition that counteract the possible drag of fine dust that characterizes the fed solids mixture.
  • a vertical deflector plate is installed inside the oven, installed at a suitable distance from the oven's gas evacuation opening.
  • this 2nd phase must be performed in cyclized form dividing operation the oven into two sub-stages, as described below:
  • the powders recovered in this equipment are reincorporated into the furnace through a transport system consisting of a refrigerated conveyor screw, which discharges into a hoist elevator which lifts the recycled load to be deposited in a second conveyor screw, which transfers the material to recycle to the oven feed hopper.
  • the gases containing the Antimony and Arsenic trioxides are sent to the following process.
  • the section 1 to the expansion chamber Radiative (1 of 4) (Fig.3 and 4) is used for recovering these particles, which are incorporated to the recirculation system of powders extracted from the first Cyclone, to be reincorporated into the Kiln.
  • the next three remaining sections of the Radiative Expansion Chamber are used for the recovery of the solidified Antimony Trioxide (Sb 2 0 3 ), which is one of the marketable products of the plant, bearing in mind that the temperature in the gases has already decreased. under the 370 ° C to enter the section 2, temperature from which the antimony trioxide (Sb 2 0 3) and solidify begins to condense into very fine particles (powders).
  • a cyclone is added to the Radiation Expansion Chamber, which allows the recovery of the solids of the product not captured in the Radiation Expansion Chamber.
  • the product recovered by the Radiative Expansion Chamber and the Second Cyclone are discharged onto a refrigerated transport screw, which reduces the temperature of the material to an approximate temperature of 60 ° C, and which in turn discharges the Antimony Trioxide (Sb 2 0 3 ) commercial to the packaging plant of said product.
  • the non-condensed gases in this process are transferred to the following process (Radiative Cooling), to be subsequently recovered.
  • Said cooling system is made up of parallel coils made up of inverted U strings, joined together (each constituting a branch of the system).
  • the gas entering the equipment circulates inside it to cool from 300 ° C to less than 100 ° C, dissipating the latent heat of the gases through the walls of the coils that make up the equipment, releasing this heat through convection phenomena and mainly radiation, into the atmospheric air that surrounds it and circulates around it.
  • the duct that constitutes this cooling system must be dimensioned for a high conduction speed in order to avoid the sedimentation of condensing particles as the temperature decreases and the solidification of Antimony Trioxide (As 2 is generated. 0 3 ).
  • the solid discharge of the Bag Filter, marketable Arsenic Trioxide (As 2 0 3 ) is emptied by a rotary valve on a conveyor screw to discharge the commercial AS2O3 to the packaging plant of said product.
  • Figs. 2 and 3 correspond to an elevation view of the Double Chamber Oven, a cross section and a plan view of the double chamber oven, in section, respectively.
  • each one of the chambers operates consecutively carrying out the following two sub-stages, each sub-stage can be performed simultaneously and out of phase in each chamber: a) Sub-Stage of Volatilization of Trioxides of Sb and As and accumulation of PbO at inside the furnace, with a controlled oxygen-free atmosphere to maintain the chemical characteristics of Sb 2 03 and As 2 0 3 volatilized and to ensure its recovery in terms of quality respectively. Once the optimum volume of PbO that is compatible with the capacity of the furnace is completed, the next sub-stage is developed.
  • the described conceptualization allows conceiving the consecutive realization of the two productive load sub-stages, in a single furnace unit with divided crucible chambers and shared gas chamber, a fact that contributes to reducing the process in question to a line of operation and consequently to reduce fuel consumption and maintenance costs.
  • Suspended vault built in refractory material of straight brick, 12 "x 6" x 3 ", of high Alumina type HA 45 ISO 10081-1.
  • Figs. 4 and 5 correspond to a schematic and cross-sectional view of the Radiative Expansion Chamber (CER), respectively.
  • CER Radiative Expansion Chamber
  • the Cyclone (CL2) has the function of supporting and maximizing the recovery of the commercial product (Sb 2 0 3 ) already solidified in the corresponding sections of the CER (in the range of 370 and 300 ° C).
  • the product recovered in the 3 final sections of the CER and in the CL2 is discharged onto a refrigerated stainless steel conveyor screw that reduces the temperature of the recovered material from around 330 to 60 ° C, which in turn feeds said commercial product. to the corresponding packaging plant. 5.Inlet pipeline for gases from Cyclone 1 to the CER.
  • Deflector plates (Howard Model), which make it difficult for the gas and particles to travel, causing a lower displacement speed and, therefore, a longer residence time for gases and solid particles inside. .

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Abstract

La présente invention concerne une installation moderne qui utilise un procédé pour l'obtention de trioxyde d'antimoine (Sb2O3), de trioxide d'arsénic (As2O3) et de plomb (Pb) métalliques commerciaux à partir d'un minéral, principalement constitué d'antimonite. La première phase débute avec un procédé de grillage oxydant dans des fours rotatifs, à température contrôlée entre 480 et 520°C du minéral soufré, afin de mener à bien l'oxydation en trioxydes de l'antimoine et de l'arsénic et par conséquent leur volatilisation. L'air, lors de cette phase du procédé, est régulé pour assurer l'oxydation appropriée d'antimoine et d'arsénic jusqu'à la formation de leurs trioxydes, en évitant la formation de cervantite (Sb2O4). La seconde phase du procédé dans l'installation est mise en oeuvre dans un four fixe à double chambre, afin de générer la volatilisation des produits d'intérêt, le trioxyde d'antimoine et le trioxyde d'arsénic, qui sont séparés suivant leurs différentes températures de condensation. La température des gaz diminue de 450 à 350°C, séparant le trioxyde d'antimoine en premier, en revanche le trioxyde d'arsénic reste volatil, se solidifiant ultérieurement à la température de gaz de 300° à 90°C. Etant donnée la condition voulant que l'oxyde de plomb ne se volatilise pas à la température de traitement initial, ce composé est maintenu solide à l'intérieur du four, et il est récupéré comme plomb liquide, après réduction au charbon.
PCT/CL2018/000045 2018-12-27 2018-12-27 Installation moderne de production de trioxydes d'antimoine, d'arsénic, ainsi que de plomb métalliques Ceased WO2020132752A1 (fr)

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