CN101191151A - Process for extraction of nickel, cobalt, and other base metals from laterite ores by using heap leaching and product containing nickel, cobalt, and other metals from laterite ores - Google Patents
Process for extraction of nickel, cobalt, and other base metals from laterite ores by using heap leaching and product containing nickel, cobalt, and other metals from laterite ores Download PDFInfo
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Abstract
The invention discloses a technics for extracting nickel, cobalt and other metals from a laterite ore through heap leaching and the product gained by the technics, characterized in that the technics includes smashing (I), agglomeration (II), accumulating(III) and heap leaching(V), wherein the last step is a reverse-current, continuous and heap-leaching system which has two or more steps and two phases. One phase is made up of ore (solute), and the other is made up of infusion solution or dissolvent. The two phases respectively provide supply on the contrary ends in the steps and flow in different directions. In the last step when the lixiviation is finished, the dissolvent is removed and a new step is started as a first position where a new ore (solute) is lixiviated from a solvent solution. Wherein, the solvent solution is introduced in the last step, is percolated and flows all the steps until gets to the first step, and is carried out separation if it contains the target metals (PLS).
Description
Technical field
The present invention includes a kind of technology of from laterite (laterite) ore, extracting Ni, Co, Zn, Fe and Cu, it with respect to those technologies well known by persons skilled in the art have still less investment and lower running cost.According to process using of the present invention heap leaching (heap leaching) method, it is meant from the laterite solid mixture of piling up carries out the technology that soluble component is extracted in diafiltration by acidic solution.
Background technology
Usually, extractive metallurgy is defined as extracting from contain metal ores and/or material by physics and chemical process the technology and the science of metal.Extractive metallurgy can be divided into three main branches: hydrometallurgy, pyrometallurgy and electrometallurgy.
Hydrometallurgy is to extract the technology of metal by water law physical chemistry technology; Pyrometallurgy relates to the dry method physical chemistry technology under the high temperature; And electrometallurgy relates to is electrolysis process.Usually, electrometallurgy and other two kinds of technologies are used in combination, and adopt the electrolysis in the water-bearing media in the hydrometallurgy, adopt the electrolysis in the melting media in the pyrometallurgy.
Extractive metallurgy also relies on different unit operations to carry out with the enrichment that improves metal and/or separates, comprising: comminuting method (broken and grinding), physics concentration method (magnetic, gravity and electrostatic separation), physical chemistry concentration method (flotation) and solid-liquid isolation method (thickening, filtration and drying).
Hydrometallurgy was carried out with three different, successive physical chemistry stages: the metal (leaching) that (a) contains in the selective dissolution solid phase; (b) purification and/or enrichment contain the aqueous solution (precipitation, gluing, ion-exchange or solvent extraction) of metal target; And (c) optionally reclaim metal (electrolytic metallurgy, electrorefining and hydrogen reducing).
Over nearly more than 50 years, the application of hydrometallurgy route in metal recovery significantly increases, and this increase and higher-grade mineral reserve are about to exploitation totally, and ore grade becomes more and more lower true closely related as a result, and ore complexity more, and this just needs the pre-concentration stage.In addition, compare with traditional fire metallurgy process, this alternative method is less and the fund cost demand is also less to the influence of environment.
Extract soluble part by solvent in insoluble solids fraction and be commonly referred to as leaching, this is the technology of a substance transfer.Taggart apud Arbiter, at Copper Hydrometallurgy-Evolutionand milestones, Hydrometallurgy-Fundamentals, Technology andInnovation, 1993, in the 549-565 page or leaf, it is defined as the operation that effectively contacts between the ore that will leach and the solvent.
Leaching can be carried out in envrionment conditions or under high temperature and/or high pressure.Processing condition depend on the chemical reaction of generation.In all cases, purpose all be produce can be from solution the ion or the metal complex of selective extraction.
Any reagent that remains in extract technology as solvent should meet the following conditions at least, referring to Guptaet al. at Hydrometallury in Extraction Process, the description in rolling up 1,39 page:
● it should enough dissolve ore apace, makes this technology in viable commercial, and should be preferably chemically to the gangue mineral inertia.
● it answers cost effectively and can obtain in a large number apace.
● if possible, it should be able to be regenerated in the subsequent technique in the stage of leaching.
Except being used to leach the water of muriate or solvable vitriol, many different solvents have been used to different leachings and have used, shown in the example in the following table 1:
Leach the classification of reagent
Table 1
Acid, as sulfuric acid, hydrochloric acid and nitric acid at dissolution process, as the most commonly used in leaching.Wherein, sulfuric acid uses the most extensive and cost is minimum.
Just as is known to the person skilled in the art, according to Chemical Engineer ' the s Handbook of Perry and Chilton, the system that leaches is characterised in that and leaches circulation (in batches, continuously or alternate in batches multiple), flows to (following current, adverse current or mixed type), stage type (single phase, multistage or difference stage) and the way of contact (diafiltration or dispersible solid).
In multistage, contracurrent system (Foust et allii, Principles of Unit Operations, 1960,43-49 page or leaf), two-phase enters the opposite end in series of stable stage, as shown in Figure 1.These flow with opposite directions.By this way, can improve the solute concentration in the L phase product, and use more a spot of solvent can obtain higher solute and reclaim.
For contact method, leaching can be divided into original position leaching, heap leaching or pile up and leach, (leaching by diafiltration) and (under normal atmosphere and pressure) agitation leach.
Can confirm by Fig. 2, according to Esteban Domic at Hidrometalurgia Fundamentos, procesosy aplicaciones, 2001, common unitary operating method may be relevant with the available main leaching method of concentrate with present milling of ores.
Original position leaches the position that is infusion solution directly is applied to ore place in the mineral reserve, does not need it is extracted.
Heap leaching may be one of the most ancient method, and it is to be used for the most ancient method that copper reclaims.It is used to the recovery of copper in Spain since the 1700's.In this leaching method, general with the vitriol oil ore is made group earlier, then it to be piled up, and infusion solution is applied to the top of ore storage, this solution, and is collected in the bottom of ore storage from the top diafiltration by action of gravity.Spill device or swing sprinker and infusion solution is used at the top of ore storage and distributed by dripping.Rinse-system is defined as the function that has the evaporation and can obtain water.The solution that contains metal target enters purification/extraction stage subsequently.Ore to fragmentation can adopt heap leaching, ROM (raw ore) is then adopted to pile up leach.It is closely similar to pile up leaching and aforesaid technology, and it is the ore of the extremely low-grade that contains metal target is handled, and this grade is usually less than the economic cut-off grade of main technique line, and this ore is called as the mineralising waste material.In heap leaching technology, the ore deposit heap can be dynamic or fixed.Under the situation of dynamic ore deposit heap (being also referred to as interrupted ore deposit heap), the ore after wherein leaching is transferred to the place that is used for the final processing of mine tailing, and the bottom of ore deposit heap can be utilized once more.Under the situation of fixing ore deposit heap or static ore deposit heap, new ore deposit heap is formed on the top of ore deposit heap in front, utilizes or need not existing impermeable district.
Drill traverse goes out (in static groove) and comprises one group of groove that is generally square cross section, and broken ore wherein is housed and uses infusion solution so that it flows up or down, thus the submergence ore layer.This is very dynamic system, is suitable for leaching the ore with fast dissolution kinetics.Usually, leaching cycle is 6-12 days.
Agitation leach under normal atmosphere or pressure requires ore by fine grinding, and by gas injection or mechanical stirring solid matter is distributed in the groove in the infusion solution therein to carry out this agitation leach.Compare with other method, because the turbulent flow in smaller particles size (bigger specific area) and the groove, extraction time is shorter, and this eddy current provides higher diffusion between reagent and ore.
Drill traverse go out and agitation leach between have two main difference.The first, in agitation leach, liquid is external phase; The second, the leaching of this form occurs under the turbulent-flow conditions, and drill traverse to flow more common in going out be laminar flow.Therefore, there is big difference between the mass transfer rates of this leaching of two types.Under the turbulent flow contact conditions, can obtain higher mass transfer rates.
As the method for extracting gold (cyanide process in the alkaline medium), copper, uranium, nickel (sulphur in the acidic medium leaches) and other mineral, the application of heap leaching is improved in recent years, reason is that it can handle those by the ordinary method ore of infeasible extremely low-grade economically, and because it is a kind of replacement scheme of the extremely slow preparation of ore of those dissolution kineticses.
The heap leaching of copper is well-known.In history, greatly before 300 years in Spain, this initiative method has been used in Rio Tinto ore deposit.
In the heap leaching of copper, with ore reduction, make group with the vitriol oil then, be deposited in subsequently on impervious bottom of suitable preparation, the height change of ore deposit heap is very big, and scope is 1.5m-30m.Infusion solution (dilute sulphuric acid) is sprayed at the upper surface of ore deposit heap, and passes ore under oozing by action of gravity.Collection contains the carrying solution (laden solution) of dissolved copper, and it is sent in the copper recovery process, and it is a kind of typical solvent extraction and electrolytic metallurgy operation.This is a kind of well-known technology, and this cover unit operation heap beach leaching/solvent extraction/electrolytic metallurgy has been used more than 40 year with commercial size.
The kind of ore no matter, wherein the operational path that carries out the dissolution phase of metal target by heap leaching all needs the fragmentation of ore/grind the stage.For this technology, this ore deposit heap has and has excellent contact between good penetration and ore and the solution is basic.Report as document US 5077021, contain excessive clay pit or fine powder (usually, material is less than 0.15mm) ore in such technology, have problems because they often in some zone of ore deposit heap, diafiltration is slowed down or even stop, the result causes stopping up.It is generally acknowledged and stop up, when fine powder and/or clay pit enter some zone in the heap of ore deposit, thereby produce section with remarkable different infiltration rate because material segregation (segregation) causes.Because this influence, solution begins to be flow through by the less passage of resistance, produces the preferred flow passage.The appearance of these preferred flow passages makes and occurs in the heap not leaching the zone, thereby reduces the recovery of metal target.When very seriously forming " slurry ", will cause stopping up by the fine particle and/or the clay pit that discharge.Therefore, must be permeable for this technology by removing fine powder and/or clay pit or their groups of making being made bed (bed).As the preparation of waiting to pile up the ore deposit, the heap leaching of the broken group's of making stage afterwards for any ore all is basic, also is inherent, and no matter it is gold, uranium, vanadium, silver, copper, zinc or nickel, oxide compound or sulfide ore.
Known to each technician of this area, nickel ores can be divided into two kinds of main types according to its composition, just sulfide and laterite (latter is also referred to as oxidized form).The sulfide mineral reserve that stem from the subterranean layer under the Saprolitic area (clay is rich in this district) account for the about 20% of Western nickel reserves, and mainly are found in Australia, secondly are Canada, China, South Africa and Zimbabwe.Always about 55% of nickel output from sulfide ore.
Laterite ore appears at the more zone on top layer.Mineral reserve mainly are positioned at Brazil, Cuba, Australia, New Caledonia and Philippines, average grade be approximately 1.95% and the grade of ferric oxide greater than 24%, and have cobalt and magnesium.Laterite ore accounts for about 80% of known nickel reserves.
Growing interest to ore output and extraction cost reduction impels the nickel ores of utilizing the laterite resource more.Two factors that help to improve these ore utilizations are: sulfide nickel storage relates to high extraction cost, and the nickel grade of laterite ore is higher than sulfide ore, thereby has higher efficient, and is as shown in table 2 below:
| Ore (1,000 ton) | Grade (%) | Nickel (1,000 ton) | ％ | |
| Sulfide | 10,594 | 0.58 | 62 | 31 |
| Laterite | 10,382 | 1.34 | 140 | 69 |
| Total amount | 20,976 | 0.96 | 202 | 100 |
Table 2
The source:
E Metalurgia, in May, 2000
Can handle laterite soil by hydrometallurgy route or pyrometallurgy route.Usually, these technologies relate to high energy expenditure, and are the same with the situation of matte smelting, and fusion is produced and the ammonia extract technology to carry out Fe-Ni, and this technology makes that the processing of low-grade ferronickel vanadine ore is uneconomical.The high pressure sulfur-bearing leaches and relates to lower energy consumption, but to equipment with owing to corrosive atmosphere all needs more with high investment.
At present, ammonia leaching and the leaching of sulfuric acid pressure are two kinds of main hydrometallurgical technologies that reclaim nickel and cobalt from laterite.Except relating to corrosive relatively chemical treatment and high fund input, they all depend critically upon the cost of fuel and sulfuric acid/sulphur separately.
Although the relative more conventional techniques of sulfuric acid pressure extract technology can not produce big advantage aspect fund cost, it allows to obtain nickel with big economic advantages aspect running cost.Though require big industrial scale, this technology allows high-caliber cobalt to reclaim, and is the enough energy of operation cycle generation.
The high price of nickel and cobalt also impels industry to seek alternative technology so that reduce running cost, thereby keeps the commercial profit of nickel and cobalt under lower price level.
In recent years nickel is produced the development that huge concern has caused a collection of new technology route that laterite ore is handled, for example heap leaching.As everyone knows, heap leaching is a kind of investment and the low operation of running cost, and mainly is widely used in copper, uranium and Gold Ore.
Although be widely used, the conventional art that extracts metal from laterite ore may cause this technology infeasible economically, and this mainly is because the mutability of the price of required fuel of described technology and acid.
For nickel industry, a technical milestone has been represented in the use that leach in laterite on the heap beach, because it not only makes the exploitation of little or low-grade mineral reserve feasible economically, and with respect to above-mentioned traditional technology it is the possibility of investing greatly the preparation of ore that reduces.
Although after deliberation and open at other document, for example patented method GR1001555, GR1003569T, US6312500, WO2004/031422 and WO2005/005671, yet what propose in the processing condition that the heap leaching notion that wherein provides proposes and system configuration and the present patent application is different fully, will become apparent by describing this.
The earliest research relevant with the application is undertaken by S.Agatzini, and obtains Greece patent GR100155.The document has been put down in writing two kinds of heap leaching technology of the ore that is applied to contain low ore grade nickel.Technology I has considered a kind of route selection, and wherein infusion solution can recirculation, just is applied to ore and repeatedly contacts, and the concentration of nickel no longer increases in observing this process flow fluid.Reach this stable after, prepare new solution and be applied to ore.The solvent that uses is a sulfuric acid, and the starting point concentration of this acid solution is 1N.Think that infiltration rate is about 4-33L/h/m
2, be preferably 12.5-25L/h/m
2As what discussed in this technology, usually, the solution that obtains from extract technology is dilute solution, and concentration of metal is low and highly depend on stage of the kind and the technology of ore.Technology II at essentially identical technology described in the technology I, and comprise infusion solution be applied in each circulation back infusion solution is being carried out the step that pH value is regulated before the ore deposit heap again.PH value is corrected to initial value.When no longer increasing, the nickel concentration in the solution thinks that leaching process finishes.The solution of gained can be used to leach another material by identical mode subsequently, up to reach required nickel concentration in solution.This technology with continuous recirculation that it is emphasized that proposition can not suppress to leach, unless the element-specific in solution reaches capacity, can observe the precipitation of lysigenic deposit form in the case.According to this technology, in the extract technology process of the heap beach of red soil nickel ore, aluminium is sedimentary at first metal in the saturated back of solution.
Feature and document GR1001555 that patent GR1003569T describes are much at one described, with the water that contains various chemical ingredientss, use from the water of industry/municipal wastewater or with in addition seawater replace ortho-water, it claims the not influence of extraction to nickel, and can increase the recyclable amount of Mg in the percolate, Ca and Na in addition.
Document US 6312500 has been introduced a kind of heap leaching technology that is used to contain the nickel laterite ores of a large amount of clay materials, being defined as in a large number more than 25% clay wherein.If necessary, ore reduction to required size, less than 25.0mm, is preferably 19.0mm-3.35mm.Owing to have fine powder in the ore, this technology comprised the stage of making group with sulfuric acid before the ore deposit heap forms.Can operate the group of making in any unit at conventional equipment or can carrying out this element.As selection, after the group of making, ore is disposed (cure).The disposal time is not waited from 1 hour by 3 days.Leave in the open place of out of door and carry out this stage by making nodulizing stone.To make the long-pending ore deposit heap that forms of nodulizing clitter then, the height of ore deposit heap can for 60cm to about 9m.Can form two or more ore deposit heaps.Acid solution is applied to the top of ore deposit heap with the speed of 10-20L/h/m2.Below extract technology itself is narrated.The new sulphuric acid soln that is at least 10g/L with concentration leaches first ore deposit heap.If the pH value of effusive infusion solution is greater than 2 (perhaps free acidity is less than 1g/L), then this solution can be directly used in the recovery of nickel.If pH value is less than 2, then this liquid can be used for ore deposit heap 2.Except liquid, new sulphuric acid soln (concentration is at least 10g/L) is applied to ore deposit heap 2 from ore deposit heap 1.Also carry out the free acidity analysis to pile 2 effusive liquid from the ore deposit.If pH value greater than 2 or free acidity less than 1g/L, this liquid also can be used for the recovery of nickel so.Under these acidity levels, do not need this liquid is carried out subsequently neutralization stage, because nickel can directly extract from solution, for example by ion-exchange.Most liquid is directly used in the extraction of nickel, but still some is used for the 3rd ore deposit heap.Can carry out this technology to many ore deposits heap.
Although claim this method among the patent WO2004/031422 not especially at nickel, this element is included in one of its claim.This patent requires reply ore to make group, contains sulfuric acid and dissolved sulfurous gas in the desired infusion solution, and this solution is purified recovery train for use in nickel, and the sulfuric acid concentration in the described infusion solution is about 785g/L.In this invention, before infusion solution being applied to ore deposit heap to wherein adding sulfurous gas.
Summary of the invention
The present patent application of being discussed with above mention other is different, the present invention proposes a kind of continous treatment process, wherein ore leaches and carries out in contracurrent system, this system comprises at least two stages, each stage is by ore deposit heap part or ore deposit heap representative.
The objective of the invention is to develop a kind of very competitive selection of from laterite ore, extracting nickel, cobalt, zinc and copper and other base metal, its investment and running cost are all low than the technological line that other has been established, and can solve the problem of extracting nickel from low grade ore and/or little mineral reserve economically.
Another object of the present invention is significantly to reduce the sulfuric acid consumption of this system, reach the level of milling of ores 350kg per ton acid, difference according to the mineralogy composition, the extraction yield of nickel changes at 70%-90%, except that short leaching cycle being provided and helping the water balance of system, and provide with respect to the improvement metal target of gangue and extracted selectivity, and significantly reduced the cumulative volume of solution.
The present invention includes a successive technology, wherein carrying out ore at least in the contracurrent system that adopts 2 stages leaches, it all is that this technology can be used for containing the ore of a large amount of natural fine powders by ore deposit heap part or ore deposit heap representative that per stage leaches, and also is to handle (＞0.5mm) the selection of thick part.Described heap leaching is the optimal selection of extracting nickel, cobalt and zinc and other base metal from laterite, the investment of this technology and running cost are all low than the technological line that other has been established, and can solve the problem of extracting nickel from low grade ore and/or little mineral reserve economically.
The present invention includes a kind of technology of from laterite ore, extracting nickel, cobalt and other metal by heap leaching, this technology comprises fragmentation (I), the group of making (II), piles up (III) and heap leaching (IV) stage, the last stage is continuously, adverse current, dynamic heap leaching system, this system comprises two-phase, one is made up of ore (solute), another is by infusion solution or solvent composition, and they are provided and flow with opposite direction in the opposite end of this series of stages.When the leaching of final stage stops, its solute is removed and is beginning the new stage by the first location place that will form by the new ore (solute) that solvent solution leaches, this solvent solution is introduced into from final stage, diafiltration or the stage of flowing through all fronts arrive first stage up to it, and when this solvent solution carries metal target (the female infusion solution of PLS-) it are separated.
Description of drawings
Fig. 1 is the synoptic diagram of multistage, contracurrent system.
Fig. 2 is the schema that the operating method of display unit may be relevant with main leaching method.
Fig. 3 is the schema of the technology of the illustrative solution that obtains the enrichment metal target.
Fig. 4 is the synoptic diagram in explanation adverse current heap leaching stage.
Fig. 5 has shown a kind of high porosity ore that reagent enters that helps leaching.
Fig. 6 has shown that the nickel in 3 samples of embodiment 1 distributes.
Fig. 7 has shown the particle size distribution in 3 samples of embodiment 1.
Fig. 8 is the graphic representation that the nickel of 3 samples of embodiment 1 extracts.
Fig. 9 is the graphic representation that the nickel from saprolitic ores extracts among the embodiment 2.
Figure 10 is the graphic representation that the nickel from iron content or limonite ore extracts among the embodiment 2.
Figure 11 has shown the leaching stage of extract technology among the embodiment 2.
Figure 12 has shown that the nickel to four types of acquisitions of 4 meters high cylinder tests extracts curve.
Figure 13 has shown the extraction curve that different leaching circuits are selected.
Figure 14 has shown the influence that particle size is extracted nickel.
Embodiment
The present invention includes a kind of by utilizing heap leaching from laterite ore, to extract the technology of nickel, cobalt and other metal, comprise and wherein in the contracurrent system that adopts two stages, carry out the continuous processing that ore leaches at least, it all is by ore deposit heap part or ore deposit heap representative that per stage leaches, this technology is applicable to the ore that contains a large amount of natural fine powders, also is the (＞0.5mm) selection of processing of rough part.Described heap leaching itself is to extract the optimal selection together with other base metal of nickel, cobalt, zinc from laterite ore, the investment of this technology and running cost are all low than the technological line that other has been set up, and can separate the inferior problem of extracting nickel from low grade ore and/or little mineral reserve economically.
It at this appended Fig. 3 the block diagram of whole flow process of the technology of the illustrative solution that obtains the enrichment metal target; At this appended Fig. 4 synoptic diagram that then is the adverse current heap leaching stage.
The present invention includes the hydrometallurgical process route that is used to handle nickel laterite ores, wherein the dissolution phase of metal values is to be undertaken by heap leaching.
At this appended Fig. 3 is that the signal of whole flow process of technology of obtaining the solution of enrichment metal target shows, usually, the route of suggestion by broken (I), the group of making (II), pile up (III) and heap leaching (IV) stage is formed.
Raw ore ROM (O) is carried out fragmentation, so that make its particle size be suitable for this technology.According to the character of ore, implement broken so that obtain to be suitable for the particle size of this technology reaching in the needed stage.Usually, the maximum particle size that obtains in secondary breaking is the about 50.0mm of about 25.0mm-, and the maximum particle size that obtains in tertiary crushing is the about 6.30mm of about 12.5mm-.Two stage crushings are just enough concerning the highly porous ore (big specific area) that contains a large amount of fine powders.Under the situation of fine and close and more unmanageable (competent) ore, can adopt three grades even level Four broken so that bigger reaction surface is provided.The generation of fine powder is minimized.
Shown a kind of high porosity ore that reagent enters that helps leaching at this appended Fig. 5.
Next, the product after the fragmentation is sent into by travelling belt made single group unit (II).If necessary, in transport process, can in ore, add entry, for example very dried and contain under the situation of a large amount of fine powders at ore.Can (for example spray) interpolation of on travelling belt, adding water and water in several ways and can reduce the formation of dust, thereby create better Working environment.In addition, it is highly important that it can reduce the loss of nickel, because this element is the characteristics of laterite in the enrichment of thin part.The group of making in traditional equipment, for example cylinder or rotating disk or even the equipment of any generation expected result.
In this stage, determine the sulfuric acid (vitriol oil or sulphuric acid soln) that in ore, adds and the amount of water according to the amount (what be lower than 0.074mm can account for 30-70%) of fine powder, and add sour and water dosage enough produce the agglomerate humidity of aequum.The humidity of agglomerate pre-determines in small-scale test, and this humidity depends on the physics and the mineralogy of ore.Because the existence of ultra-fine part, can add binding agent, this binding agent can be inorganic or organic, synthetic or natural or or even mineral sources (mineralorigin), wilkinite for example is as long as these reagent are inert to the acid in the infusion solution.In the group's of making product, should there be fine powder, promptly any ore part less than 1.70mm.
It is worthy of note, because the high-content of basic component, for example MgO or CaO, the ore of natural alkalescence has high neutralising capacity, and saprolite (saprolitic) ore is exactly this situation.Therefore, the group of making is except known benefit, and the important part of this stage in the route of suggestion also is the pre-neutralization stage as ore.Consider the ore kind of main consumption acid in the technology particle size measurement, thereby determine the vitriolic add-on.This neutralization reaction in this stage has been quickened the beginning that metal target is extracted.In this stage, do not add acid and just water make (having or do not have binding agent), can be observed the delay that metal target (particularly nickel and cobalt) is extracted, though observe whole extraction circulation is not had great effect.Usually, magnesium, iron, aluminium and calcium all are main consumption acid elements.
After the group of making (II), ore is piled up (III), form the final ore deposit heap that highly is preferably 4m for the about 7m of about 2m-.
Suggestion leaching system (IV) is that dynamically pile in the ore deposit of (or interrupted), and is adverse current, multistage, and the number in stage is 2 or more, is preferably 3 stages.System described here follows the notion that Foust et allii that background technology mentions in describing provides in Principles of Unit Operations.As leaching unit operation, two-phase is made up of the ore (solute) and the sulphuric acid soln (solvent) of its metal values to be extracted (mainly being nickel and cobalt).This two-phase is supplied with and is flowed with opposite directions in the opposite end of a series of equilibrium stages.With and stream line or parallel flow compare, adopt this technology can obtain the concentration of higher nickel and cobalt and shorter leaching cycle and use in liquid product quantity of solvent still less.
To final stage or at the new infusion solution of applied on top---the sulphuric acid soln that concentration does not wait between the about 200g/L of about 50g/L-of the ore deposit in the stage 3 under 3 stage system situations heap, and be collected in separately in separately the storage tank from the diafiltration solution in per stage, and be used for subsequent stage according to the flow direction.
Solution from stage 2 and 3 is named as intermediate solution 2 (ILS2) and intermediate solution 3 (ILS3) respectively, by that analogy.
---female infusion solution (PLS)---residual acidity of having is the about 30g/L of about 10-to be loaded with the final solution of metal target.
Last at extract technology (IV), in the end the stage,, wash ore with new water or process water perhaps in the stage 3 of 3 stage system.After the flushing, the ore after leaching is transported to the nothing infiltration and prepares to be used to leach the last sedimentary zone of residue.Need be appreciated that, because this is a successive technology, in case final stage or for example the ore in the stage 3 leach and stop, the ore in the stage 2 will be sent to the stage 3, and the ore in stage 1 will be sent to the stage 2, and new part (or ore deposit heap) will enter the stage 1.
As target of the present invention, heap leaching technology can be used for containing the ore of a large amount of natural fine powders, and also can be used as the selection that raw granulate fraction (for example particle size is greater than 0.5mm) is handled.In a kind of situation in back, fine fraction will carry out the conventional processing by autoclave, perhaps carry out atmosphere and leach the perhaps combination of two kinds of extract technologies.
The present invention also considers the final product that contains nickel, cobalt and other metal that obtains by heap leaching technology (IV) from laterite ore, the solution of perhaps having reported that is loaded with metal target (PLS) that technology obtains according to the present invention.
The different choice that mother solution (PLS) is handled is assessed, for example from the generation of the verticality (verticalization) of the generation of the outflow solution-mixed precipitation in stage 1 or technology up to metallic nickel.
Precipitate the iron that mother solution is existed and the extraction of aluminium stage by stage by adding alkaline reagents.Subsequently, the solution of not iron content and aluminium or iron and aluminium are delivered to the extraction (6) of carrying out nickel and cobalt at the solution of acceptable degree at the most, can extract or reclaim this nickel and cobalt by multiple technologies, for example precipitation, solvent extraction or even ion-exchange.By solvent extraction or ion exchange resin, produce metallic nickel; By precipitation, produce the mixed oxyhydroxide or the sulfide of containing of nickel, cobalt, zinc and other base metal.
The application has mentioned certain operational condition, for example ore deposit stack height, ore particles size and sulfuric acid concentration or the like, but do not limit their exclusiveness, and point out that these conditions can change in each heap leaching stage, and do not damage the net result of technology.
Although describe and preferred operating procedure be described, need point out it is that the variant of this technology is possible and feasible, do not depart from the scope of the present invention.
Leach from the laterite ore ore dressing remainder that leaches route by the HPAL/ atmosphere (＞0.5mm) applicability in order to assess the heap beach, get 3 samples, its chemical analysis is shown in following table 3, and highly for these samples being tested in the cylinder of 1m.
The chemical analysis of charging sample
| Middle class | Al(％) | Co(％) | Cr(％) | Cu(％) | Fe(％) | Mg(％) | Mn(％) | Ni(％) | Si(％) | Ti(％) | Zn(％) |
| |
0.83 | 0.03 | 0.58 | 0.02 | 9.65 | 1.55 | 0.21 | 0.31 | 33.65 | 0.05 | 0.02 |
| |
0.72 | 0.03 | 0.67 | 0.03 | 8.54 | 9.52 | 0.11 | 0.46 | 25.10 | 0.03 | 0.03 |
| |
2.37 | 0.09 | 0.78 | 0.06 | 10.20 | 6.42 | 0.37 | 1.36 | 24.70 | 0.24 | 0.05 |
Table 3
Shown that at this appended Fig. 6 the nickel in these samples distributes.Nickel mainly is in layered silicate (serpentinite and chlorite).
The particle size of sample is decided to be 100% and is lower than 1.27mm.The distribution of particle size is as appended shown in Figure 7 at this.Other executive condition of these tests is as follows: infiltration rate is 10L/h/m
2, vitriolic concentration is 20g/L in the infusion solution; The dosage of acid is ore 20kg per ton in the group of making; Open line test.
These preliminary test shows are carried out the ability that nickel extracts by the heap leaching unit operation.Yet the graphic representation that extracts at the nickel shown in this appended Fig. 8 shows that these system needs are more sour, for example the infusion solution of the acid by having greater concn.Low acid concentration may be slow dynamic (dynamical) factor.In 100 days operation, sample 1,2 and 3 nickel extract and reach 34%, 58% and 69% respectively.
In 1 meter high cylinder and 4 meters high cylinders, test, so that the influence that the entry evaluation height extracts nickel.These tests are that the sample from four kinds of different lithology (lithdogy) is carried out, and also having one is the composite sample of each rock type (lithotype).All samples all are crushed to particle size 100% less than 12.5mm.Infiltration rate is constant and be 10L/h/m
2Sulfuric acid concentration in 1 meter high cylinder in the infusion solution is 20-200g/L, and is 50g/L in 4 meters high cylinders.
Under different acidity conditions, the nickel of different ore kinds extracts curve and proves that this variable is influential to technology.High more acid concentration can cause fast more kinetics.
Nickel extraction meeting changes according to mineralogy.Concerning technology, tolerate most (refractory), thereby the mineral that can obtain the extraction of minimum level nickel are the mineral that contain a large amount of nickel in the ironic hydroxide.This tolerance of form that occurs for nickel is understandable, because nickel needs more energy in the system to overcome the high bonding energy of these oxyhydroxide in the crystalline structure of ironic hydroxide.Nickle atom is difficult for entering infusion solution.
Shown the extraction curve of the test in 1 meter high column form object at this appended Fig. 9 (in the saprolitic ores nickel extract) and Figure 10 (nickel in iron content or the limonite ore extracts), to two kinds of extraction curves of assessing ore type.
The test of carrying out in paxillae can be assessed the maximum expected nickel extracted amount that reaches.Because all types of ores all day reach stable in 100 circulations, suppose that this time is whole cycles, and the concentration of acid changed once in per 20 days, from 20 to 200g/L then from 200 to 20g/L.Acid concentration is proved again to the influence of technology.In having the test that improves acidity value, variation has taken place in the bending that can observe curve when acidity increases.In having the test that reduces acidity value, it is not obvious to observe this influence.
In these tests, determined three main stages in the extract technology of assessment: neutralization, elementary leaching and secondary leach, as in this appended (leaching stage) shown in Figure 11.In the fs, main reaction relates to diffluent ore, especially contains the material of magnesium, so this process is regarded as neutralization.There are three kinds of different kinetics, depend on how nickel distributes in ore: the nickel that the sheet interlayer (between sheet) of layered silicate absorbs is than the easier extraction of nickel of (in the sheet) in these same mineral structures, thereby this can produce the extracted amount bigger than the nickel that contains in the ironic hydroxide.
Different this behaviors of leaching the zone have shown the importance of assessment according to the circuit of counter-current principle.
The nickel that has shown four types of acquisitions that 4 meters high cylinders are tested at this appended Figure 12 extracts curve.
Three kinds of different choice that leach circuit are assessed, and it extracts curve as appended shown in Figure 13 at this: open circuit, have the adverse current circuit (circuit with ILS) of three phases, and have PLS recirculation and the gauged route of acid concentration.
For the ILS circuit, the whole cycle is considered to 150 days, and three phases respectively is 50 days.Linear flow route (ILS) shows it itself is the optimal selection of the ore of assessing, because it has significantly shortened leaching cycle, and has reduced the cumulative volume and the acid consumption of solution, shown in following table 4.
| Route type | Leaching cycle (my god) | The extraction of nickel (%) | The extraction of cobalt (%) | H 2SO 4Consumption (kilogram/ore per ton) |
| ILS | 150 | 84 | 70 | 280 |
| Open | 270 | 87 | 72 | 560 |
| Having recirculation and acidity proofreaies and correct | 270 | 84 | 70 | 250 |
Table 4
Same sample in 4 meters high cylinders is tested, with of the influence of assessment particle size the nickel extraction.Other condition of technology, for example the concentration of infusion solution, infiltration rate, the group's of making condition all remain unchanged.Can observe, in ore the naturally occurring fine powder, to highly porous sample, the overall dimension of 12.5mm or 50.0mm is not extracted nickel and is produced remarkably influenced, as in this appended (impact evaluation that particle size is extracted nickel) shown in Figure 14.
Claims (19)
1. from laterite ore, extract nickel by heap leaching, the method of cobalt and other metal, it is characterized in that comprising fragmentation (I), the group of making (II), pile up (III) and heap leaching (IV) stage, this final stage is an adverse current, successive, the heap leaching system, this system has two or more stages, there is two-phase, form by ore (solute) for one, another is by infusion solution or solvent composition mutually, they are supplied with in this series of stages opposite end respectively, and flow in the opposite direction, when the leaching of final stage stops, its solute is removed, and beginning the new stage by the first location place that will form by the new ore (solute) that solvent solution leaches, this solvent solution is introduced by final stage, diafiltration or flow through all the preceding the stage arrive the fs up to it, if it is loaded with metal target (PLS) then separates.
2. as claimed in claim 1ly from laterite ore, extract the method for nickel, cobalt and other metal, it is characterized in that, can in a plurality of stages, carry out fragmentation (I) on demand to obtain to be suitable for the particle size of this method by heap leaching.
3. the method for from laterite ore, extracting nickel, cobalt and other metal by heap leaching as claimed in claim 2, it is characterized in that, the maximum particle size that obtains in two-stage crushing is the about 50.0mm of about 25.0mm-, and the maximum particle size that obtains in three grades of fragmentations is the particle of the about 6.30mm of about 12.5mm-.
4. as claimed in claim 1ly extract the method for nickel, cobalt and other metal by heap leaching from laterite ore, it is characterized in that, it is preceding optional to wherein adding water to be admitted to the group's of making stage (II) at crushed product.
5. as claimed in claim 1ly from laterite ore, extract the method for nickel, cobalt and other metal, it is characterized in that, in the group's of making stage (II), add water and optional interpolation acid or other additive, for example binding agent etc. by heap leaching.
6. as claimed in claim 5ly from laterite ore, extract the method for nickel, cobalt and other metal, it is characterized in that the sulfuric acid in the vitriol oil or the solution and the additive capacity of water are enough to reach the group's of making humidity by heap leaching.
7. as claimed in claim 5ly from laterite ore, extract the method for nickel, cobalt and other metal, it is characterized in that described binding agent can be inorganic or organic, synthetic or natural, or even be derived from mineral, for example wilkinite by heap leaching.
8. describedly from laterite ore, extract the method for nickel, cobalt and other metal as claim 1 or 5, it is characterized in that, do not exist in the product of the group of making damaging the fine powder of diafiltration technology by heap leaching.
9. as claimed in claim 1ly from laterite ore, extract the method for nickel, cobalt and other metal, it is characterized in that described ore deposit heap is preferably dynamic or interrupted type by heap leaching.
10. describedly from laterite ore, extract the method for nickel, cobalt and other metal as claim 1 or 9, it is characterized in that the ore of accumulation (III) forms highly to be piled for the ore deposit of the about 7m of about 2m-by heap leaching.
11. as claimed in claim 1ly from laterite ore, extract the method for nickel, cobalt and other metal, it is characterized in that described heap leaching system (IV) is made up of three phases by heap leaching.
12. as claimed in claim 1ly from laterite ore, extract the method for nickel, cobalt and other metal by heap leaching, it is characterized in that, contain sulphuric acid soln in the new infusion solution.
13. as claimed in claim 12ly from laterite ore, extract the method for nickel, cobalt and other metal, it is characterized in that its concentration is 50g/L-200g/L by heap leaching.
14. as claimed in claim 1ly from laterite ore, extract the method for nickel, cobalt and other metal, it is characterized in that in the end new infusion solution is introduced at the upper surface in stage or top by heap leaching.
15. as claimed in claim 1ly from laterite ore, extract the method for nickel, cobalt and other metal by heap leaching, it is characterized in that, collect respectively to be used for the follow-up stage from the diafiltration solution (ILS) in each stage and according to the flow direction.
16. as claimed in claim 1ly from laterite ore, extract the method for nickel, cobalt and other metal, it is characterized in that the residual acidity that exists in female infusion solution (PLS) is the about 30g/L of about 10-by heap leaching.
17. as claimed in claim 1ly from laterite ore, extract the method for nickel, cobalt and other metal, it is characterized in that, when in the end the extract technology in stage finishes, with the ore of new water or process water flushing leaching, then as residue by heap leaching.
18. the method for from laterite ore, extracting nickel, cobalt and other metal by heap leaching as claimed in claim 1, it is characterized in that the solution (PLS) that is loaded with metal can carry out follow-up technology so that separate for example metal of nickel, cobalt, zinc, aluminium and iron etc.
19. as the described product that contains nickel, cobalt and other metal of any claim in front from laterite ore, it is characterized in that, it obtains by heap leaching technology (IV), perhaps comprises the solution that is loaded with metal target (PLS) that obtains by by described technology.
Applications Claiming Priority (6)
| Application Number | Priority Date | Filing Date | Title |
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| BR05058287 | 2005-11-28 | ||
| BR0505828-7 | 2005-11-28 | ||
| BRPI0505828 | 2005-11-28 | ||
| BR06056431 | 2006-10-30 | ||
| BRPI0605643-1A BRPI0605643A (en) | 2006-10-30 | 2006-10-30 | process for removing nickel, cobalt and other metals from lateritic ores by leaching into piles and product containing nickel, cobalt and other metals from lateritic ores |
| BR0605643-1 | 2006-10-30 |
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| CN110195157A (en) * | 2019-07-05 | 2019-09-03 | 福州大学 | Low Grade Copper Ore briquetting-the biological dump leaching process crushed based on high-pressure roller mill |
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| CN110195157A (en) * | 2019-07-05 | 2019-09-03 | 福州大学 | Low Grade Copper Ore briquetting-the biological dump leaching process crushed based on high-pressure roller mill |
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