CN103492592A - Refining of platinum group metals concentrates - Google Patents

Refining of platinum group metals concentrates Download PDF

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Publication number
CN103492592A
CN103492592A CN201280007776.5A CN201280007776A CN103492592A CN 103492592 A CN103492592 A CN 103492592A CN 201280007776 A CN201280007776 A CN 201280007776A CN 103492592 A CN103492592 A CN 103492592A
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roasting
slag
alloy
melting
temperature
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格特·阿德里安·伯泽伊登霍特
雅各布斯·约翰内斯·埃克斯廷
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Western Platinum Ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • 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
    • C22B11/00—Obtaining noble metals
    • C22B11/02—Obtaining noble metals 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
    • C22B1/00—Preliminary treatment of ores or scrap
    • C22B1/02—Roasting 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
    • C22B11/00—Obtaining noble metals
    • C22B11/02—Obtaining noble metals by dry processes
    • C22B11/021—Recovery of noble metals from waste materials
    • 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

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Abstract

This invention relates to a process in which a Platinum Group Metal (PGM)-rich residue from a BMR (Base Metals Refinery) process is subjected to a high temperature roast to remove contaminants, typically volatile elements (for example Se, Te, As, S, Bi, Os) and obtain a roast product. The roast product is smelted with a flux to form a slag phase and an alloy phase, and to vaporize sulphates and heavy metals like Pb, Te, and remove stable oxide compounds such as Si02 and oxides of Fe, Ni, Co, Cu, Cr, Te, Bi to the slag phase. The alloy and the slag phase are separated, and the alloy phase is then melted and atomized with a gas or liquid atomization process to form fine alloy particles that can be dissolved in water and treated in a hydrometallurgical PMR (Precious Metals Refinery) process.

Description

The refining of platinum metals concentrate
Technical field
The present invention relates to the production of platinum metals (PGM) (it comprises Pt, Pd, Rh, Ru, Ir) and gold (Au), it generally is comprised of flotation step, most of described PGM and and during sulfide mineral all concentrates in slip during this step.Flotation has selectivity and typical case very much > 80% the PGM rate of recovery can adopt 1.8%～4% quality to take out (being reported as the charging quality % of washed ore) numeral and realize.Unfortunately, some elements often with sulfide or PGM mineralogy (as the element of As, Se, Te, Bi, Cd, Hg, Pb) thus combine and some of these elements are also taken out of and become the refining furnace feed material along with flotation concentrate.
Background technology
In the typical melting step that PGM produces, at first concentrate melts in AC or DC stove, thereby wherein sulfide mineral separates with oxide mineral and forms respectively unique stove sulfonium and molten slag layer.These layers are emitted individually on different heights in stove.PGM often follow the sulfonium phase and in the melting step rate of recovery reach 95%.Yet minor contaminants element (As, Se, Te, Bi, Cd, Hg, Pb) is also followed described sulfonium phase (matte phase), has the rate of recovery of change.Step of converting is after the melting step, and wherein FeS removes from stove sulfonium (matte).Between transition phase, air (has or without O 2enrichment) be injected into converter (transmodulator) thus in FeS is oxidized to FeO and SO 2.Some oxidations of melting base metal sulfide and slight desulfurization, also may betide in conversion process.Final product from smelting operation is called converter matte mostly.Converter matte not only contains contaminant species (As, Se, Te, Bi, Pb), also contains the artifact of conversion operation and because slag carries or carry secretly the mineral that exist.This generally includes SiO 2with spinel oxides as magnetite and awaruite (or other similar Ni/Cu/Fe oxide compounds).The Cr of trace 2o 3, CaO, the MgO(source that also has slag to carry) also be present in converter matte.
Converter matte can carry out granulation or atomization, and delivers to base metal removal/refinement step, wherein sulfide mineral (being mainly Ni, Cu and Fe sulfide) thus leach to produce 40% the resistates (based on dry weight) containing PGM.
In other practice, thereby converter matte can separate the PGM in alloy phase by Slow cooling with base metal sulfide.After Slow cooling, alloy-sulfide piece is crushed, and described alloy is recovered in thick magnetic part, and base metal sulfide is recycled in non magnetic concentrate.Thereby the complete physical sepn between these two phases is seldom the feasible described alloy phase that makes processes with bronsted lowry acids and bases bronsted lowry the Symbiont of removing the base metal pollutent usually under well-oxygenated environment.Subsequently, PGM alloy concentrate directly sends to PMR.
Although BMR technological process main purpose is to remove sulfide mineral, described refining often comprises and is intended to deliver to noble metal refining (PMR) removes before the circulation process of some pollutents from the BMR salvage stores.This comprises that multiple circulation process is to remove Se, Te, Pb, SiO 2and ferric oxide/nickel composite.These circulation process are generally used for and tend to is the BMR place of vitriol basic craft course.Therefore can process better the pollutent that easily from sulfate liquor matrix, more easily moves into or shift out in BMR.On the contrary, the pollutent that uses muriate, nitrate or cyanide solution matrix to be easy to remove can be removed better at the PMR place.
Produced PGM(and comprised Pt, Pd, Rh, Ru, Ir, Os in noble metal refinery), and the final step of Au and Ag.This precious metal fine fodder from BMR leaches usually in chlorine and hydrochloric environment, for dissolving platinum metals.Then will become containing the solution separating of PGM its composition metal by many processes (may comprise and repeat precipitation and dissolution process, solvent extraction, any in the scope of ion-exchange or molecular recognition technology).
The typical feed grade of the PMR of platinum industry is about 40%～75%, but is generally 65%(Pt, Pd, Rh, Ru, the summation of Ir and Au).Residue content is As, Pb, Se, Te, Bi, SiO 2, Fe/Ni oxide compound, metallization/sulfuration Fe, the BMS(base metal sulfide that do not leach), stable vitriol/oxyhydroxide of forming during the BMR technological process-vitriol, CaO, MgO, Cr 2o 3composite mix or compound with crystal water.This part of pollutent list is reported in the various flows of PMR technological process, and tends to produce resistates in the PMR technological process.These resistatess need to adopt relevant treatment cost, inventory time etc. again to process.These pollutents also may have a negative impact to the total yield of precious metal with by the pipeline time that metal is paid market.
At present, all pollutents that are contained in the main feed material stream of PMR, processed by hydrometallurgy procedure of processing (having the circulation process that BMR or PMR technological process are introduced).Most of refinings all have the fire metallurgy process step on recirculation/resistates/processing with foreign materials material, but also do not have ready-made pyrometallurgy method tracked (slot) to be used for after removing most of described Cu, Ni and S and make described material dissolution process main feed material before for the PMR technological process to flow.
Summary of the invention
According to the present invention, a kind of method is provided, wherein be rich in platinum metals (PGM) resistates (usually be greater than by mass 40% precious metal be PGM) and usually contain the base metal that is less than by weight 10% in described resistates, the experience high-temperature roasting is to remove pollutent, volatile element (for example, Se, Te, As, S, Bi, Os) and obtain product of roasting normally.
Preferably, above-mentioned product of roasting is used for forming slag phase and alloy phase with the fusing assistant melting, and is used for evaporating vitriol and heavy metal as Pb, Te, and by stable oxide compound as SiO 2remove to described slag phase with the oxide compound of Fe, Ni, Co, Cu, Cr, Te, Bi, and after this described alloy and described slag are separated.
Thereby above-mentioned alloy phase can carry out subsequently melting and with gas or atomization of liquid method carry out atomization form can be dissolved in the water and in the refining of hydrometallurgy PMR(precious metal) the meticulous alloy particle processed in technological process.
Principle of the present invention is allowed by the pyrometallurgy method, removes the pollutent of relative broad range by the rare character (tolerance oxidation and low-vapor pressure) of at high temperature using described PGM material.The enrichment of PGM allows to form PGM alloy phase (without adding trapping agent) that can atomization.The method proposed can produce 90% or higher 6 kinds of PGE(Pt, Pd, Rh, Ru, Ir and Au comprising alloy), wherein remaining pollutent is mainly metallized Fe, Ni and Cu.
Maturing temperature needs enough height, with the necessary compound of vaporizing (as TeO 2, SeO 2, TeO 2, As 2o 3and Os 4o 6) and decompose stable compound (as vitriol), and may need temperature higher than 500 ℃ and lower than 1000 ℃, preferably 600 ℃ to lower than 900 ℃, most preferably 700 ℃～850 ℃.At lower temperature, described PGM(is Pd, Ru, Rh and Ir particularly) vapour pressure of tending to occur oxidation and described PGM oxide compound is greater than the several orders of magnitude of pure metal.For fear of PMG oxide compound vaporization (especially Ru), maturing temperature can keep below 900 ℃.Calcination steps comprises and adds oxygenant, as the oxidisability roasting of air.Generally, every 100 gram resistatess add 100～150g, preferably the air of 130～150g.
Although all volatile components are oxide compounds, therefore need aerial oxidisability roasting, the oxidation state of element and mineralogy are in conjunction with determining roasting condition.Before or after described oxidisability roasting, thereby the reductibility roasting can also be the necessary correct oxidation state that forms some element.Described reductibility roasting can be at 550 ℃～650 ℃, usually approximately at the temperature of 600 ℃, with reductive agent, as coal or refinery coke, implemented.
Described melting step should be a little more than the liquidus temperature of alloy phase (wherein all solids disappears and becomes the minimum temperature of fusing fully) to decompose stable compound (as vitriol), by Pb(and other heavy metals) remove to gas phase and allow that stable oxide compound is (as SiO 2, Cr 2o 3and spinel) be dissolved in slag mutually in, common described melting step, at 1300 ℃～1600 ℃, is implemented at the temperature of preferably 1400 ℃～1500 ℃.
Preferably, under reductive condition, usually by adding as reductive agent as carbon, for example, by every 100g feed material add 5～15g carbohydrate as flour carry out as described in melting.
Synthetic slag can also add in described melt, utilizes low melting point and viscosity with the following: Ca or Mg oxide compound, silicate, aluminate, alkalimetal oxide, preferably CaO-SiO 2-Al 2o 3-Na 2o, fusing assistant system, for example, described fusing assistant can contain 10%～40% SiO by weight 2, 5%～15% Al by weight 2o 3, 30%～50% CaO and 15%～25% Na by weight by weight 2o.The charging of every 100g product of roasting, adding of slag can be changed to the 100g slag from 20g, but usually adds 50g slag/100g product of roasting charging will allow that slag can be by stable spinel type compound dissolution in described roasting feed material.
Described melting step can be implemented without adding trapping agent.
If realize melting with induction, the graphite acceptor container of ceramic lining should be preferably used as crucible.
Preferably, described melting is implemented with three steps:
1) reductibility melting step;
2) reduce pressure, preferably reduce described absolute pressure extremely lower than 0.5atm, common about 0.1atm, continue 10～30min to remove Pb, Te and/or other heavy metals; And/or
3) add oxygenant as K 2nO 3, Na 2o 2, O 2gas, air, NaNO 3or MnO 2, preferred NaNO 3with guarantee by pollutent as Fe and Ni be dispensed to well as described in the slag phase.
The atomization of described alloy can complete by gas or liquid cooling.High-pressure water jet is the method for the good foundation of atomization, and can obtain very meticulous particle (D50 be approximately 10～20 μ m) if necessary.The atomization that adopts liquid (for example water) to carry out forms rapidly cooling metastable phase and has inhomogeneous (normally hollow) particle that allows rapidly-soluble high surface area.Also likely use high-pressure inert gas (as N 2or Ar) jet, or centrifugal gas cooling becomes approximately 40 μ m of D50 by described alloy atomization.Particle is more spherical, and unlike cooling quick in water.Material is processed, and solubility behavior and metal metering (metal accouting) will promote the decision to atomization type used.
Method of the present invention can be inserted in:
After the Slow cooling technological process,
Among base metal reclaims (BMR) technological process, or
Between BMR technological process and PMR technological process.
" Slow cooling " method refers to the wherein method with the PGM of separation in alloy phase from base metal sulfide by the sulfonium Slow cooling.
" BMR method " for example refers to, from removing most of described base metal and sulphur (> 95% in charging (, the hydrometallurgical processes process based on vitriol)) any method.
The examples of locations of the inventive method will be direct melting concentrate from the BMR technological process after the pressure leaching for removing Cu.This will eliminate for removing last remaining BMS, SiO 2, Fe/Ni oxide compound, metallization/sulfuration Fe, Pb and amphoteric element the part of existing BMR.
" PMR method " refers to hydrometallurgy processing treatment step, wherein from the PGM concentrate, separates and recovery PGM.
The accompanying drawing explanation
Fig. 1 is the schema of the inventive method.
Embodiment
The present invention relates to a kind of pyrometallurgy method, it has with single treatment step removes a large amount of pollutents to the PMR(precious metal and reclaims from material feeding) ability of technological process, remove very selectively pollutent (but not PGM, except Os) simultaneously.Because many pollutents can be removed in single step, current BMR(base metal reclaims) and the PMR technical process can be simplified potentially, and save relevant cost.
Described a kind of method, wherein pollutent (includes but not limited to As, Pb, Se, Te, Bi, SiO2, Fe/Ni oxide compound, metallization/sulfuration Fe, the base metal sulfide of not leaching (leaching), stable vitriol/oxyhydroxide-vitriol, CaO, MgO, Cr 2o 3) by the pyrometallurgy method, from the PMR feed material, remove fully or partly.The pyrometallurgy method is by calcination steps, and then the melting step forms.Calcination steps removes volatile element for example, to gas phase (, Se, Te, Os, S, Bi, As).The melting step is decomposed stable compound (as vitriol), by Pb(and other heavy metals) remove to gas phase, and allow stable oxide compound (as SiO 2, Cr 2o 3and spinel) be dissolved in slag mutually in.The melting step forms alloy and the slag phase that can cast with physical sepn.Alloy phase melting and carry out atomization again, thus contribute to the alloy of PMR technological process to dissolve.
Following table 1 comprises the typical material feeding that the method that can propose by the present invention is processed.The mineralogy material forms and mineral assemblage is the key that understanding method is optimized.
Table 1: the example that enters the feed material in technological process
Figure BDA00003622014400071
Figure BDA00003622014400081
Calcination steps
The core of calcination steps is that volatile oxidn (is mainly SeO 2, TeO 2, As 2o 3, Os 4o 6and SO 2) formation.Air is enough strong oxygenants of realizing this purpose.Except utilizing air not having under relevant cost, it also contains 79% N 2, it plays allows that enough gas volumes remove volatile matter (TeO especially 2) vital role.
For studied feed material, about 140g air/100g feed material is necessary for reaching sufficient removal.Except the longer and roasting cost of roasting time increases, for thering is higher gas flow (volume), can exert an influence hardly.
For described oxidisability calcination steps, approximately the temperature of 800 ℃ just can be moved.Some Ru losses, will, for decomposing stable vitriol, still will occur (as RuO in higher temperature more than 900 ℃ 3and RuO 4).Under maturing temperature, Ru, Rh, Ir and Pd all form the vapour pressure of oxide compound and these oxide compounds for being greater than several orders of magnitude of pure metal (except Pd).
Described maturing temperature should be optimized for the character of described feed material.As an example, other that circulate from the Se/Te precipitation in BMR leach resistatess in approximately 750 ℃ of beginning meltings, and maturing temperature is limited to 700 ℃.Although the removal of Te is not good in described roasting circulation, described Te can remove fully in decompression is smelted.
Roasting can complete in fluidized-bed (circulation bed fluid reactor or bubbling bed reactor), rotary drum stoving oven, multiple hearth furnace or static bed (a plurality of trays in manually being written into retort furnace).High-level efficiency fluid bed reactor preferably, but particle diameter, required through-rate and to the needs of batch processing will play a key effect aspect the choice of technology.In the situation that studied material, carry out one slightly coalescent to control particle suspension.To decompose/be dissolved to the slag phase for micro-coalescent tackiness agent in the melting step process.The heat of roasting can be supplied with by electric power/gas or burning.
For studied material, owing to removing with air, roasting also is not so good as to pass through the effective like that of modeling and forecasting.This may be real, because at nonvolatile arsenate (As 5+) and difficult with the sperrylite of oxidation, exist down, the material of supposing in described feed material forms and is incorrect.In order to remove As, be necessary to be reduced into trivalent As.Can complete the prereduction roasting 600 ℃ of left and right with coal or refinery coke.If the reducing/oxidizing roasting of two steps is necessary, it is better in single container, can completing the simple batch reaction changed of gas.
With reference to figure 1, BMR feed material 10, reductive agent 12 and rare gas element 14 are fed in the reductibility calcination steps 16A in stoving oven 16.After this, air supply 18 to offer same stoving oven 16 by oxidisability calcination steps 16B after the reductibility calcination steps.
In the typical rate of recovery value of the gas phase of 800 ℃ of lower roastings can see following table 2.Nearly all Se, As, Os, Te and most of S can be volatilized.
Table 2: during 800 ℃ of lower roastings, element is removed efficiency to the typical case of gas phase
Element Remove to gas phase (quality %)
Pb 0.0%
Au 0.0%
Pt 0.0%
Ir 0.0%
Os 100.0%
Te 95.0%
Ag 0.0%
Pd 0.0%
Rh 0.0%
Ru 0.0%
Se 100.0%
As 90.0%
Cu 0.0%
Ni 0.0%
Co 0.0%
Fe 0.0%
S 90.9%
The waste gas formed during roasting should be hunted down and offer gas sweetening/metal recovery step 22, because described gas can contain objectionable impurities (as oxide compound and the SO of Se, As, Os 2).This will discuss in more detail below.
The melting step
Be the melting step after roasting, and will, from the oxidation material 24 of stoving oven 16, together with reductive agent 28, rare gas element 30 and fusing assistant 32, be supplied to smelting furnace 26.Melting allows to form alloy phase and slag phase.Described slag will absorb SiO mutually 2, the oxide compound of Fe, Ni, Co, Cu, Cr, Te, Bi etc., vitriol/oxygen vitriol will decompose and allow the slag middle oxide compound produced that absorbs mutually simultaneously.PGM is concentrated in alloy phase, and, by the atomized alloy phase, PGM has enough reactive behavioies, to enter PMR refining circulation by existing dissolving circulation.
In this embodiment of the invention, smelting furnace 26 is induction furnaces, although AC and DC technology also can be used.Induction fusing can contribute to batchwise operation by heating and cooling in crucible is arranged, and allows more easily to carry out the pressure change step than AC or DC stove simultaneously.The PRELIMINARY RESULTS of induction fusing shows, need to transfer heat to described material via the acceptor crucible, because can not realize direct coupling for the material of described roasting.Recommend graphite as the acceptor crucible, because it can contribute to temperature up to 1800 ℃, and without any problem, and heating and cooling very rapidly.This research shows, graphite really occurs to interact with described melt and should use ceramic crucible (preferably high magnesia content) the described graphite of lining and contact with described melt.
Melting should be carried out under the liquidus temperature a little more than alloy (minimum temperature that all solids becomes and melts fully).The liquidus temperature of described alloy phase is the alloying action driving by the relative concentration of different PGM metals and described base metal (as Cu and Ni) and Fe.PGM content higher (particularly as Ru higher melt metal), liquidus temperature is just higher.Leach resistates for studied BMR, Ru is that the metal and the described liquidus temperature that finally are dissolved in described alloy are 1430～1450 ℃.The temperature that it is found that 1450～1500 ℃ is applicable to test job.Temperature more than 1500 ℃ can cause Pd to a certain degree loss (under 1500 ℃ 0.3%), because Pd has the highest vapour pressure of PGM metals.
Smelting operation can be described as 3 different steps best, 1) reductibility melting step 26A a little, 2) by Pb, the Te of reduction pressure and the removal 26B of other heavy metals, and 3) thereby oxygenant adds 26C to be guaranteed pollutent (comprising some Fe and Ni) is assigned to described slag phase well.Because melting completes as the batch process process, described 3 steps can be regulated continuously from charging to casting.In the end after oxidation step, then cast.
Because the vapour pressure of PGM oxide compound (Ru, Ir and the Rh on less degree) is enough lost between heating period causing greatly, should be together with synthetic slag 32(, described slag is not natural slag, but the slag of being made by its component) add together gentle reductive agent 28 and mixed with the feed material of described roasting before melting.Described reductive agent can be carbohydrate (as whole meal flour), and should be the rank of the feed material of about 5g～10g flour/100g roasting.Too the condition of reductibility will force most of Fe and Ni to alloy phase.Once, in alloy phase, these elements will be difficult to carry out to a great extent selective oxidation.Rare gas element 30 is supplied in smelting furnace 26, and can maintain inert gas atmosphere in whole smelting operation process on described melt.
After all materials all melt, can reduce the pressure of atmosphere on described melt.This can be by vacuumizing to contribute to carry out with vacuum pump in Bing Gai chamber, closing presure chamber.Pb often at PMR(especially at Rh between refining period) in produce special problem.Due to required Pb standard, removing step to the Pb of gas phase need to be included in melting operation.Approximately 95% Pb removal (together with Te and some other heavy metals) can come very effectively to reach by described absolute pressure is reduced to about 0.1atm.Pb is as PbO and Pb gasification.After for some time of 10～30min, can break vacuum under lower pressure.Approximately 50% silver loses to gas phase (its experience reduces pressure).
Opening vacuum chamber and making after melt recovers standard atmosphere pressure, thus can to add in described slag oxygenant 34 guarantee by pollutent be assigned to best described slag mutually in.Can also realize the limited oxidation of the Cu of Fe, Ni and less degree by adding oxygenant.The product charging of about 2.5g oxygenant/100g roasting is added can be raised to 92% from 87% by final alloy PGM grade.NaNO 3and MnO 2can both be used as oxygenant, but preferred NaNO 3.
Be important to note that the standard for some element will cause the melting step complicated on device.If the dosis tolerata of the Pb in alloy, Ni etc. can reduce, pressure decreased step and oxidation step can be exempted.The reductibility melting still can produce the alloy of the 6PGE grade that has approximately 85% a little.
Following table 3 has shown under the product that adds 7g flour/100g roasting the typical rate of recovery to described alloy phase of the melting step of whole product of roasting under 1450 ℃.If those skilled in the art can recalculate quality addition required while using alternative carbohydrate.
Table 3: after 800 ℃ of lower roastings for 1450 ℃ of lower meltings to the typical rate of recovery of described alloy phase.The product charging that adds 7g flour/100g roasting
Element The rate of recovery to alloy phase
Bi 29.35%
Te 1.46%
As 2.45%
Pb 0.22%
Au 99.58%
Pt 100.00%
Ir 99.99%
Ag 36.42%
Pd 99.75%
Rh 100.00%
Ru 99.42%
Cu 64.16%
Ni 26.39%
Co 7.93%
Fe 3.70%
Cr 0.00%
Ca 0.00%
S 0.00%
Si 0.00%
Al 0.00%
Mg 0.00%
Need in melt, add synthetic slag, be used for absorbing undesired oxide compound from melt.Recommendation CaO-SiO 2-Al 2o 3-Na 2the O system is as fusing assistant, because it has low melting glass (forming approximately 1150 ℃ of liquidus temperatures for recommended slag), low viscosity (about 0.4log(pool under 1450 ℃)), the low-down ability that absorbs the good capacity of all oxides and absorb magnesium oxide-based lining.The indication slag forms (from the angle of adding) as shown in Table 4 below:
Table 4: the fusing assistant composition ratio proposed
Figure BDA00003622014400121
Figure BDA00003622014400131
Recommend fusing assistant to add the product feed material that speed is the total fusing assistant of about 50g/100g roasting.This adds speed is very important for enough receptivities of allowing the spinel that absorbs otherwise exist with solid form.For example, because there is spinel in conversion operation (, magnetite and awaruite), but some also can form (due to the existence of Mg, Fe, Ni, Al and Cr) during roasting.
When smelting operation finishes, described slag has low-down viscosity (be calculated as 0.13log(pool)) (due to for example, from described melt (, FeO, Fe 2o 3, NiO, MgO) in the ability of additionally fluxing of the oxide compound that absorbs).
Off gas treatment from the roasting circulation process
The roasting circulation process will produce gas stream 20 heat, concentrated, and it will comprise environment and the harmful a large amount of gaseous matter of human body.Owing to from baking operation, almost can't avoiding some particle suspension in gas phase, need the particle separation step is included in such gas circulation flow process.Ideally, this particle removal step should be carried out, and simultaneously gas is still the gaseous matter of (dew point/more than desublimation point) of heat.Ceramic candle type filter is an example of spendable hot particle removal equipment.The particle of removing from gas can turn back in stoving oven 16 24.
In order to remove most of obnoxious flavour material from waste gas, it will be possible in wet type circulation process (being preferably based on alkalescence), washing.In addition, it is also possible reclaiming some valuable gaseous matter (Se, Te, Os) by selectivity condensation/desublimation.This may need reduction and carry out the frigorimeter area of condensation thereon.
If need the reductibility calcination steps, need to design for it existence of inflammable gas material.Off gas treatment will be made laws, and existing Infrastructure and described potential market/metal values are ordered about.
It is also possible processing torrefaction waste gas and process melting waste gas in the cycles of washing flow process (particle reclaims rear) of existing apparatus.
Off gas treatment from the melting circulation process
Waste gas from smelting operation 36 must be extracted and be processed on described stove, and be processed in off gas treatment operation 38.Off gas treatment may need or may not need particle removal and washing.Described exhaust flow can merge with the exhaust flow of baking operation, or can merge with the circulation process of existing apparatus.
The melt of roasting and the melt of oxidisability-cast molding in mold
To be cast in mold 42 from molten alloy and the slag 40 of smelting furnace 26.Induction furnace (with less AC and DC stove) thus usually can tilt described melt is poured in mold by enough hydraulic efficiency plant.Bottom tapping is also possible for batchwise operation.
Casting can be at fixed mould, or the overflow ladle mould of segregation drive completes in arranging.Once solidify, can shift out the content of mould.PGM is not the solvency action in mutually at slag to the main loss mechanism of slag, but in suspension (carrying secretly) and the cold junction effect of the alloy particle in mutually at slag during the casting process process.Thereby the very important aspect of casting is to make described slag become suitable fluid to contribute to from described slag the quantitative alloy sedimentation to molten alloy pool.Uniqueness between slag and alloy and smooth surface is for being essential with separating neatly easily, and is easy to realize.
In the situation that use fixing AC or DC smelting furnace technology to carry out melting, bleed outlet can be maintained at (but tilt operation also can operate on small-sized AC and DC stove) in the refractory liner that can open as required and clog.Thereby slag and alloy can be released and effectively remove the suspensoid of alloy from different height during pouring operation.The advantage of this way is, described slag will more lack precious metal and this will limit the material locked in technological process.
Manual separation slag and alloy
Separation alloy and slag in simple hand technological process 44.Described slag can knock out alloy phase simply mechanically.If complete casting under good control, should be quite smooth and separate and be easy to be affected in the surface between described slag and alloy.Alloy pig and slag bear manually sorting subsequently and in batches with further processing treatment.Described alloy pig is should be very clean and alloy phase does not almost carry slag, because this slag will enter the PMR technological process together with described alloy after atomization.
Slag goes back to smelting furnace
The slag 46 separated from alloy will comprise some PGM, be mainly owing to carrying secretly with little suspended particle form due to alloy.PGM at described slag in mutually can for example, by the described slag of processing treatment and reclaiming again in described smelting furnace device stove (be referred to as existing smelting operation,, the selected melting completed before described step of converting and described BMR).The base metal sulfide material of discharging by described slag will play the PGM of trapping agent effect and recovery will be again by described conversion process process.The rate of recovery that typical smelting operation has > 98%, so secondary should have the opportunity to very effectively reclaim any loss by (two roads) slag.
The atomization melt
It is very necessary that the alloy of described separation 48 is dissolved in described precious metal refining.In order with alloy, effectively to realize this purpose, described surface-area needs enough large, and described surface need to have enough reactive behavioies.52 one-tenth fine powders of described alloy atomization just can be realized this target.
For the liquid stream of atomized alloy, described alloy is melting 50 again.The induction furnace technology is this situation that is best suited for so far because the coupling and transferring energy directly alloy carry out.This makes described melting process very fast and is effective.Someone is recommended in the described alloy of melting in alumina crucible, but also can use graphite.50 ℃ of temperature (liquidus temperature) when melt temperature should be not liquid higher than all alloys.The magnitude that required atomization melt temperature is 1500～1550 ℃.Inert gas atmosphere should be maintained on crucible to avoid described alloy and crucible generation oxidation.
For controlled alloy liquid stream (controlling with mass rate and flow direction) is provided in described high pressure gas or water spray, can use graphite furnace.This graphite furnace can heat to prevent that by ruhmkorff coil any material from freezing in described stove again.Inert gas atmosphere should be maintained at whole graphite to prevent described alloy and crucible generation oxidation.Described stove receives and waits in line (queue) liquid metal and enters described high pressure gas/water jet.Furnace can be controlled in 1500 ℃.
Extraction hood should be positioned on induction furnace in order to remove flue gas.From the gas of this melt can with other gas streams, such as from described roasting and/or preliminary melting step, the gas for washing merges.Should not exist for remove any needs of particle from this gas stream.
Atomization
The atomization 52 of described alloy can complete by gas or liquid cooling.If use liquid, preferably water, and rare gas element, such as N 2or Ar, also preferably as gas cooling medium.High-pressure water jet is the method for having set up of atomization, and can obtain very meticulous particle (if necessary, D50 approximately 10～20 μ m).The particle that the atomization of using liquid (such as water) to complete forms rapidly cooling metastable phase and has inhomogeneous (the usually hollow) of allowing rapidly-soluble high surface area.For estimated material, during cooling form at least 2 phases, contain most of high-melting-point PGM(Rh, Ir, Ru and Pt) height melting phase and the Fe, the Ni that contain some Pd and most of surplus and the second-phase of Cu.
Use the high pressure gas jet, or centrifugal gas cooling come the described alloy of atomization to D50 approximately 40 μ m be also possible.Particle is more spherical and cooling not as rapid in water.Material processing, solubility behavior and metal metering (metal accounting) all will affect determining of adopted atomization type.
If make water, the water jet of recommendation under 60～160bar pressure.Between atomization period, the ratio of described water and alloy (w/w) can be 5～10.Management of water/alloy ratio will allow that described alloy slip is pumped directly to dissolution vessel.If this can't complete, will need filtration step to remove water from described slip.
Be dissolved in the PMR circulation process
The alloy of atomization can directly be committed to dissolution process process 54, although described dissolution rate can force, described container is carried out to better temperature control.It is found that the reactive behavior of described alloy is slightly higher than normal PMR feed material, and after chlorine is opened, use described alloy solution heating faster.Yet, temperature is controlled and redox-potential be controlled at laboratory scale on normal PMR feed material similar level on can realize.
The processing method variant does not limit the present invention
The present invention is not subject to following any one restriction or constraint:
The mode that is prepared converter matte by the smelting furnace sulfonium, or any technology or processing and treating method before producing converter matte.
Mode (described mode base metal physically or is chemically removed) by the concentrated PGM of converter matte
Method steps in described BMR (if PGM is by described BMR)-as an example, for Ni+Cu, remove the choice of technology between atmosphere and pressure leaching.
Fang method Bu Zhou – in described PMR is as an example, in the choice of technology repeated between precipitation and dissolution process, solvent extraction, ion-exchange or molecular recognition technology.
Stove subtype – AC, DC or induction furnace are for preliminary melting.Induction furnace is best (heating rate, by the efficiency of direct coupling) for atomization
Molten smelting method – comprises or pressure release is controlled, and comprises or get rid of in slag adding oxygenant
The type of crucible/refractory materials
Atomization Lei Xing – gas or liquid are as heat-eliminating medium
The Lei Xing – gravity overflow type of arrangement of casting mould, single large mold etc.
Slag purification Fang Fa – can be returned in existing smelting operation and maybe can introduce independent slag purification melt and discard slag
The static bed of the Lei Xing – of stoving oven, rotation type, many thoraxes, fluiddized-bed roasting
The necessity of reductibility roasting before or after the Lei Xing – oxidisability roasting that roasting requires
The type that gas sweetening used and solid reclaim
Reclaim precious metals from exhaust flow, such as the Method type (if use) of Se, Te and Os
The major advantage of the inventive method is that it can be applicable to any existing precious metal refining, and wherein said feed material contains pollutent, includes but not limited to As, Pb, Se, Te, Bi, Cd, Hg, SiO 2, Fe/Ni oxide compound, metallization/sulfuration Fe, the BMS(base metal sulfide that do not leach), CaO, MgO, Cr 2o 3.
Can predict following advantage list by method of the present invention:
Can be reduced in the amount of the resistates produced in the PMR technological process.Can save the cost of processing with foreign materials/reprocessing resistates material.
Amount from the effluent of PMR technological process can reduce along with the relevant reduction of PGM loss in described effluent.
Because PGM in resistates has not too closely improved first rate of recovery of passing through in described PMR circulation process and can obtain effluent stream in conjunction with (less tie-up).
The described PMR processing treatment time can be reduced (from having more reactivity and tentatively being leached to faster the pollutant removal step).The capacity that this has reduced the tank farm stock in the technological process and has improved described PMR.
Be that pollutent exists the exercisable challenge in relevant PMR (especially to be fed to the periodic high SiO of described PMR 2and Pb) can be solved.Described melting step can be stablized PMR charging grade by removing the pollutent that does not have the control step in all the other processes of the method.
Described BMR and/or PMR method can be simplified by walking around hydrometallurgy pollutant removal step.This also will eliminate this step of avoiding and produce effluent stream (having lower relevant PGM loss).Can reach manpower and cost savings by the pollutant removal technological process of avoiding.
The charging content of described PMR is little.
Present patent application requires the right of priority of ZA2011/00894, and its content is as a reference incorporated herein.

Claims (35)

1. a method, wherein comprise base metal be rich in platinum metals (PGM) resistates through high-temperature roasting to remove the pollutent that comprises Se, Te, As, S, Bi, Os, and obtain product of roasting.
2. method according to claim 1, wherein in described resistates, being greater than by mass 40% precious metal is PGM.
3. method according to claim 1 and 2, wherein said resistates contains the base metal that is less than by weight 10%.
4. according to the described method of any one in claim 1～3, wherein said maturing temperature higher than 500 ℃ lower than 1000 ℃.
5. method according to claim 4, wherein said maturing temperature is from 600 ℃ to lower than 900 ℃.
6. method according to claim 5, wherein said maturing temperature is 700 ℃～850 ℃.
7. according to the described method of any one in the claim of front, wherein said calcination steps comprises the oxidisability roasting that adds oxygenant.
8. method according to claim 7, wherein said oxygenant is air.
9. method according to claim 8, wherein every 100g resistates adds 100～150g air.
10. method according to claim 9, wherein every 100g resistates adds 130～150g air.
11., according to the described method of any one in claim 7～10, wherein said calcination steps carries out the reductibility roasting before or after being included in described oxidisability roasting.
12. method according to claim 11, wherein said reductibility roasting is carried out at the temperature of 550 ℃～650 ℃.
13. method according to claim 12, wherein said reductibility roasting is approximately being carried out at the temperature of 600 ℃.
14., according to the described method of any one in claim 11～13, wherein in described reductibility roasting, add reductive agent.
15. method according to claim 14, wherein said reductive agent is coal or refinery coke.
16. a method, thereby wherein as product of roasting as described in the method limited in any one in claim 1～15, at the temperature of 1300 ℃～1600 ℃, with the fusing assistant melting, form slag phase and the alloy phase separated.
17. method according to claim 16, wherein said product of roasting carries out melting at the temperature of 1400 ℃～1500 ℃.
18., according to the described method of claim 16 or 17, wherein said melting is carried out under reductive condition.
19. method according to claim 18 wherein adds reductive agent in described melting step.
20. method according to claim 19, wherein said reductive agent is carbohydrate.
21. method according to claim 20, wherein said reductive agent is flour.
22. method according to claim 21, wherein every 100g feed material adds the flour of 5g～15g.
23., according to the described method of any one in claim 16～22, wherein said slag is synthetic slag.
24., according to the described method of any one in claim 16～23, wherein said fusing assistant is Ca or Mg oxide compound, silicate, aluminate, base metal oxide fusing assistant.
25. method according to claim 24, wherein said fusing assistant is CaO-SiO 2-Al 2o 3-Na 2the O fusing assistant.
26. method according to claim 25, wherein said fusing assistant contains 10%～40% SiO by weight 2, 5%～15% Al by weight 2o 3, 30%～50% CaO and 15%～25% Na by weight by weight 2o.
27., according to the described method of any one in claim 16～26, it is 20g～100g slag/100g product of roasting charging that wherein said slag adds.
28. method according to claim 27, wherein said slag is incorporated as about 50g slag/100g product of roasting charging.
29., according to the described method of any one in claim 16～28, wherein said melting step is carried out not adding under trapping agent.
30., according to the described method of any one in claim 16～29, wherein with induction, realize the melting in the graphite receptor container with ceramic lining.
31., according to the described method of any one in claim 16～30, wherein said melting is carried out with three steps:
1) reductibility melting step;
2) reduce pressure, preferably reduce for some time of lasting 10～30 minutes of absolute pressure to remove Pb, Te and/or other heavy metals; And/or
3) add oxygenant as K 2nO 3, Na 2o 2, O 2gas, air, NaNO 3or MnO 2, preferred NaNO 3thereby guarantee pollutent as Fe and Ni be dispensed to well as described in the slag phase.
32. method according to claim 31, wherein reduce described absolute pressure lower than 0.5atm.
33. method according to claim 32, wherein reduce described absolute pressure to about 0.1atm.
34. a method, thus wherein as alloy product as described in the method that limits in any one in claim 16～33, be melted and with gas or atomization of liquid method carry out atomization form can be dissolved in the water and in the refining of hydrometallurgy PMR(precious metal) the meticulous alloy particle processed in method.
35. can be implemented as follows according to the method limited in any one in the claim of front:
After the slow cooling method,
At base metal, reclaim in (BMR) method, or
Between BMR method and PMR method.
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