CN104630502A - Method for recovering nickel, cobalt, iron and silicon from limonite by combined leaching process - Google Patents
Method for recovering nickel, cobalt, iron and silicon from limonite by combined leaching process Download PDFInfo
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- CN104630502A CN104630502A CN201410845398.9A CN201410845398A CN104630502A CN 104630502 A CN104630502 A CN 104630502A CN 201410845398 A CN201410845398 A CN 201410845398A CN 104630502 A CN104630502 A CN 104630502A
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Abstract
The invention discloses a method for recovering nickel, cobalt, iron and silicon from limonite by a combined leaching process. The method comprises the following steps: washing and grading the limonite to obtain high-silicon magnesium ore and low-silicon magnesium and high-iron ore; adding high-silicon magnesium ore slurry after heating and concentrated sulfuric acid into a double-spiral material pushing reactor; dissolving reaction materials in water, then performing solid-liquid separation, and washing filtration residues to obtain normal-pressure leaching residues, a normal-pressure leaching solution and a washing solution; respectively heating low-silicon magnesium and high-iron ore slurry and the normal-pressure leaching solution, then adding into a pressurization pipeline reactor for pressurization and leaching, hydrolyzing Fe<3+> in the normal-pressure leaching solution to release acid, and leaching the low-silicon magnesium and high-iron ore; reducing the temperature, and performing solid-liquid separation to obtain pressurized leaching residues and a pressurized leaching solution; removing impurities in the pressurized leaching solution, and then recovering nickel and/or cobalt; washing the pressurized leaching residues with a soda ash solution, and then drying to obtain fine iron powder; and performing treatment on the normal-pressure leaching residues to obtain silicon dioxide and fine sand. The method disclosed by the invention has the advantages of short leaching time, high nickel leaching rate, low acid consumption and effective recovery of iron and part of silicon.
Description
Technical field
The present invention relates to the hydrometallurgical processes technical field of limonite, be specifically related to a kind of method being reclaimed nickel, cobalt, iron and silicon by combined leaching process from limonite.
Background technology
Laterite is by nickeliferous peridotites at the torrid zone or the nickel oxide ore that goes bad through extensive long-term weathering leaching of subtropical zone, and owing to there is the difference of geographical position, weather condition and rate of decay, laterite type is all over the world incomplete same.Efflorescence generally produces bedded deposit, wherein also exists completely or sedentary product the most thoroughly near surface, along with degree of depth increase fades to the lighter sedentary product of degree, and finally terminates as unweathered rock at certain darker depth.Most of nickel that height waste mantle is contained usually is trickle to be distributed in pyrrhosiderite particle in small, broken bits.This layer is commonly referred to limonite, and it generally contains silicon and the magnesium of a high proportion of iron and low ratio.Nickel contained by the layer that weathering is lighter is generally contained in various magnesium silicate minerals more, such as serpentine.A lot of other may be had in incomplete zone of weathering to contain the silicate minerals of nickel.The height of part weathering is commonly referred to saprolite or noumeite containing magnesium ribbon.Its iron generally containing low ratio and a high proportion of silicon and magnesium.In some mineral deposits, also have the another kind of main band containing nontonite clays be usually between limonite and saprolite, be called transition ore deposit." low-grade laterite " refers to the laterite not having saprolite ore deposit, the laterite be namely made up of limonite and transition ore deposit.Under normal circumstances, limonite is the chief component of red soil nickel ore, accounts for the 65%-75% of laterite total amount; Saprolite accounts for 15%-25%; Transition ore deposit accounts for 10%.From red soil nickel ore, reclaim nickel, the where the shoe pinches of cobalt is, usually not by the useful component of the abundant enriching nickel of physics mode before carrying out chemical treatment separating metal useful component (as nickel and cobalt), namely cannot carry out enrichment by the technology of ore dressing, this makes the processing cost of red soil nickel ore very high.And due to different mineral and chemical constitution in limonite and saprolite ore deposit, these ores are unsuitable for using same treatment technology to process usually.Finding the method for the cost reducing process red soil nickel ore in decades always.
The treatment process of current red soil nickel ore can be divided into thermal process and the large class of wet processing two usually.Fire metallurgy process is applicable to process saprolite ore deposit.This technique can only produce ferronickel usually, can not Call Provision, and its application is restricted.Hydrometallurgical processes is applicable to process limonite.Hydrometallurgical technology comprise high pressure acidleach and reducing roasting _ ammonia leaching and occur in recent years as normal pressure acidleach, heap leaching method etc.Heap Leaching leaching yield is lower, is only applicable to the laterite processing high Mg content; Reduction roasting-ammonia leaching technique due to energy consumption higher, technical process is long and less to be used; Normal pressure acidleach technological operation is simple, does not need to use expensive autoclave, but it is comparatively large that mineral will be made to dissolve then required sour consumption completely, and containing each metal ion species in leach liquor, makes the follow-up separation circuit that macerates become complicated.High pressure acidleach (HPAL) technique uses sulfuric acid to leach red soil nickel ore under high temperature (250 DEG C) and high pressure (50MPa).Under high temperature, condition of high voltage, the metalliferous mineral in ore almost dissolves completely.The iron dissolved is hydrolyzed to rapidly rhombohedral iron ore (Fe under adopted high temperature
20
3) precipitation, nickel, cobalt etc. stay in the solution, and the leaching residue of iron content and silicon is by a series of washing concentrating after cooling, namely concentrated in so-called counter-current decantation washing (CCD) loop and be separated from the solution of nickeliferous, cobalt.Therefore the main purpose of extract technology is reached--nickel is separated with iron.
The advantage of high pressure Ore Leaching (HPAL) technique is: nickel, cobalt leaching yield are high; Speed of response is fast, the reaction times is short; Iron does not consume sulfuric acid in theory in acidleach process and hydrolysate is rhombohedral iron ore (Fe
20
3) precipitation.But the shortcoming of high pressure Ore Leaching (HPAL) technique is also very outstanding: be first that it needs the autoclave of complicated high temperature, high pressure and relevant equipment, its I&M is all very expensive; Two is that the sulfuric acid of high pressure acidleach (HPAL) processes expend is more than the sulfuric acid needed for the non-ferrous metal components stoichiometrically dissolved in ore.Because most sulfate ion provided by sulfuric acid is connected to form hydrogen sulfate ion (HSO under high pressure acidleach condition
4 -).That is sulfuric acid dissociation under high pressure acidleach condition discharges a proton (H+).Leach liquor cooling and in and time, hydrogen sulfate ion resolves into sulfate radical (SO
4 2-) and another proton.Because after this proton (acid) is inabundant for leaching, and cause excessive sulfuric acid in subsequent disposal to be carried out with and consume neutralizing agent; Three is raw materials that HPAL technique is only limited to that process is mainly limonite class, because the existence of saprolite can cause rolling up of sulfuric acid consumption.This is because the Mg content of magnesium in saprolite is higher caused; Four be HPAL technique in the easy fouling of operational process mesohigh still, need periodic shut down to clear up, working rate is low; Five is leach the quantity of slag greatly, and is the mixing slag of silicon and iron, can not cost-effectively develop.
U.S. Patent No. 4,097,575 describe the improvement to HPAL technique, be included in the high pressure that limonite occurs in described autoclave to leach, the discharge that high pressure leaches be used in less than about 820 DEG C roastings, and the stronger saprolite ore deposit roasting sand of the reactive behavior of sulfuric acid in and excessive acid, the nickel contained in saprolite ore deposit in this N-process dissolves in a large number.The advantage of this technique is that it utilizes the sulfuric acid added in limonite pressure leaching process better, decrease the consumption for the treatment of the Wingdale of autoclave discharge liquid or the neutralization reagent of other costlinesses, and obtain the ability that the limonite component in red soil nickel ore body and saprolite component are processed.But this technique still needs the leaching using expensive autoclave for limonite, and needs to carry out calcination process to saprolite ore deposit, and this treatment process is all very expensive in fund input and running cost.
U.S. Patent No. 6,379,636 B2 describe U.S. Patent No. 4, and 097, the further improvement of the technique described in 575, eliminates saprolite calcination steps, and acid excessive during saprolite raw ore is used for and in autoclave discharge solution.In addition, can add more acid in relief liquor can leaching content with what increase saprolite.But this technique still needs to use expensive autoclave.
In order to avoid using expensive autoclave, developing the laterite nickel resources of saprolite and limonite simultaneously, there has been proposed the normal pressure acidleach technology that some improve.If publication number is the patent of invention of CN101273146A, propose the two step normal pressure leach extraction methods in lixiviate saprolite ore deposit after simultaneously lixiviate limonite and saprolite ore deposit or first lixiviate limonite, this method has the advantage not using autoclave, but propose in the flow process described in this application when processing to remove Fe and/or A1 to infusion solution, to need to add in neutralizing agent and residual acid in leach liquor, most of iron is deposited as ferric hydroxide, and this can cause loss and the slurry filtration difficulty of the valuable elements such as nickel cobalt.And for example publication number is the patent of invention of CN101541985A, proposes the method for the mixture in a kind of normal pressure leaching limonite and saprolite ore deposit, but its iron precipitated product is jarosite, containing sulfate radical in jarosite, therefore can increase the acid consumption of leaching process; And jarosite is a kind of compound of thermodynamic instability, can sulfuric acid be discharged when heap sum is deposited, thus cause environmental pollution.For another example publication number is the patent of invention of CN101006190A, the method of the mixture proposing a kind of concentrated acid process limonite and saprolite ore deposit then water leaching nickel cobalt, the deposition of iron thing that this method produces is ferric oxide except jarosite or oxyhydroxide, but the extraction time of this application needs 12-48h, extraction time is longer, cause process cycle longer, production cost rises.
For another example publication number is the patent of invention of CN102206749A, propose one and first use sulfuric acid leaching limonite, use a leach liquor lixiviate saprolite ore deposit again, rear section (or all) secondary leach liquor return the circulation normal-pressure leaching method once leaching limonite again, the method possesses can process the higher advantage of limonite and saprolite ore deposit and nickel cobalt leaching yield simultaneously, but technical process is comparatively complicated, the shortcoming of sulfuric acid consumption higher (mean value is about 0.7g acid/1.0g ore deposit), and saprolite ore deposit used amount is more than 1.5 times of limonite amount, form with the mine belt of laterite and contradict.For another example publication number is the patent of invention of CN101001964A, propose and a kind ofly first under normal pressure (100 DEG C-105 DEG C), leach limonite with enough sulfuric acid, then use the normal pressure leaching ore pulp of limonite and saprolite ore pulp to leach the method extracting nickel, cobalt under middle pressure (about 0.5MPa, 150 DEG C).The advantage of the method is: can process limonite and saprolite ore deposit simultaneously; Avoid using expensive autoclave and achieve the higher nickel leaching yield in saprolite ore deposit with relatively simple pressure exerting device under middle pressure condition.But the method exists following shortcoming and defect: first the time of normal pressure leaching limonite is longer, be generally more than 4 hours, therefore required normal pressure leaching equipment is huge; Two is that acid consumption is higher, total acid/ore=0.6/1, although this acid consumes index far below normal pressure acidleach far above high pressure acidleach; Three are saprolite ore deposit used amounts is 1 times of limonite amount, and this mine belt that is same and laterite forms and contradicts, it is well known that in red soil nickel ore bed, and limonite amount: saprolite ore deposit measures >=2: 1.
In a word, in the patent of invention of above-mentioned laterite nickel ore hydrometallurgical, the shortcoming of the high pressure acid leaching process of high pressure acidleach (HPAL) technique and improvement is: need the autoclave of complicated high temperature, high pressure and relevant equipment, its I&M is all very expensive; The sulfuric acid of HPAL processes expend is more than the sulfuric acid needed for the non-ferrous metal components stoichiometrically dissolved in ore; HPAL technique is only limited to the raw material that process is mainly limonite class; HPAL technique is in the easy fouling of operational process mesohigh still, and need periodic shut down to clear up, working rate is low.The shortcoming of the normal pressure acid leaching process of normal pressure acid leaching process and improvement is: sulfuric acid consumption is high; Nickel, cobalt leaching yield are low; Long reaction time, required equipment is huge.It is that to leach the quantity of slag large that high pressure acidleach comprises common drawback that the high pressure acid leaching process of improvement and normal pressure acid leaching process comprise the normal pressure acid leaching process of improvement, and is the mixing slag of silicon and iron, and the main component iron of laterite can not cost-effectively be developed.Although be referred to the recycling of leached mud in the patent of invention of CN102206749A, but because the silicon-dioxide in slag and ferric oxide, pyrrhosiderite etc. are the fine particles of reaction generation, their mutual " growths " together, be difficult to by methods such as simple magnetic separation, they are separated, therefore the economic benefit of above-mentioned leached mud exploitation is very poor, useless solid process can only be worked as, even must work as danger waste residue for the leached mud that nickel leaching yield is lower and process.
Because saprolite only accounts for about 30% of red soil nickel ore total amount, and belong to the rich ore in laterite mineral deposit due to saprolite, usually all adopt thermal process to produce ferronickel, what therefore laterite processing enterprise can obtain is the limonite that nickel grade is lower.
Summary of the invention
The object of the invention is to solve the technical problem existed in prior art, providing a kind of and by combined leaching process sulfuric acid normal pressure leaching carried out to the high silicon magnesium ore deposit composition in limonite and with normal pressure leaching liquid, low silicon magnesium height iron ore composition carried out to the method for the recovery nickel of pressure leaching, cobalt, iron and silicon.
In order to achieve the above object, the present invention is by the following technical solutions: a kind of method being reclaimed nickel, cobalt, iron and silicon by combined leaching process from limonite, comprise the following steps: (a) obtains high silicon magnesium ore deposit and low silicon magnesium height iron ore to limonite washing classification, add water obtained high silicon magnesium ore pulp in high silicon magnesium ore deposit; B high silicon magnesium ore pulp is heated to 60 DEG C-100 DEG C by (), the vitriol oil is heated to 150 DEG C-200 DEG C, adds the high silicon magnesium ore pulp after heating and the vitriol oil, react to dissolve solubility non-ferrous metal and soluble iron in duplex pusher reactor; C () carries out water-soluble rear solid-liquid separation to reaction mass and residue washing obtains normal pressure leaching slag (A), normal pressure leaching liquid (B) and washings (E); D () makes low silicon magnesium high ferro ore pulp with washings (E) and low silicon magnesium height iron ore, add in capstan reactor after low silicon magnesium high ferro ore pulp and normal pressure leaching liquid (B) are heated to 95 DEG C-100 DEG C respectively, pressure be 1.5MPa-4.0Mpa, temperature be the condition of 150 DEG C-240 DEG C under pressure leaching 0.5-1.5 hour, the Fe in normal pressure leaching liquid (B)
3+be hydrolyzed to hematite precipitation and discharge acid and leach low silicon magnesium height iron ore again; E () is reduced temperature and carry out solid-liquid separation after 80 DEG C, obtain pressure leaching slag (C) and pressureleaching solution (D); By namely there being method to reclaim nickel and/or cobalt f () removes non-nickel cobalt impurity to pressureleaching solution (D) after; G () obtains Iron concentrate to pressure leaching slag (C) soda ash solution washing post-drying; H () obtains silicon-dioxide and fine sand to normal pressure leaching slag (A) through screening process.
Further, in described step (a), the granularity in high silicon magnesium ore deposit is+80 orders, and the granularity of low silicon magnesium height iron ore is-80 orders.
Further, in described step (a), the mass ratio of high silicon magnesium ore deposit and water is 1:1.2-1:1.
Further, in described step (b), the mass ratio of high silicon magnesium ore pulp and the vitriol oil is 20:9-22:9, and the reaction times is 1-12 minute.
Further, time water-soluble in described step (c), the mass ratio of reaction mass and water is 29:30-1:1.
Further, proportioning when washings (E) and low silicon magnesium height iron ore make low silicon magnesium high ferro ore pulp in described step (d) is 2L:1Kg.
Further, in low silicon magnesium high ferro ore pulp, adding normal pressure leaching liquid (B) in described step (d) makes reaction mass final ph be 0.5-1.5.
Further, in described step (g), the massfraction of soda ash solution is 10%, and bake out temperature is 120 DEG C-150 DEG C.
Further, in described step (c), normal pressure leaching slag (A) is white residue, and its dioxide-containing silica is 65%-90%.
Further, obtain pressure leaching slag (C) in described step (e) for rhombohedral iron ore slag, wherein iron level is 58%-65%.
Wherein, the first step is in limonite washing classification process, obtains the thicker high silicon magnesium ore deposit part of particle diameter and the thinner low silicon magnesium height iron ore part of particle diameter.Second step is in high silicon magnesium ore deposit acidleach process, the vitriol oil of high silicon magnesium ore pulp and q.s fully mixes fast, the heat of dilution that water in the vitriol oil and high silicon magnesium ore pulp produces makes temperature of charge raise to impel metal (nickel, cobalt, iron, magnesium, chromium, aluminium etc.) in high silicon magnesium ore deposit and sulfuric acid rapid reaction generation metal sulfate, simultaneously a large amount of reaction heat makes temperature of charge be increased to 95 DEG C-120 DEG C further and ensures that reaction is carried out fully and completely, and silicon-dioxide and the unreacted iron of minute quantity and non-ferrous metal are formed and leach residue.3rd step is the water-soluble of normal pressure acidleach material and solid-liquid separation process, for some time placed by the normal pressure leaching material of second step, loose cellular solid-state lotion is formed in temperature-fall period, add the water that can ensure that metal sulfate all dissolves and stir, metal sulfate is all dissolved and enters solution, after carrying out solid-liquid separation and residue washing, obtain normal pressure leaching slag (A), normal pressure leaching liquid (B) and washings (E).4th step is the process that normal pressure leaching immersion goes out low silicon magnesium height iron ore, and normal pressure leaching liquid and low silicon magnesium height iron ore slurry are added pressure leaching in capstan reactor, the Fe in filtrate
3+be hydrolyzed to hematite precipitation and discharge acid and leach low silicon magnesium height iron ore again, during reaction, pressure is 1.5MPa-4.0Mpa, temperature is 150 DEG C-240 DEG C, can not only ensure that the hydrolysate of iron ion is that rhombohedral iron ore also has fast hydrolysis rate and higher nickel cobalt leaching yield and leaching velocity.5th step is lowered the temperature by pressure leaching material and obtains pressure leaching slag (C) and pressureleaching solution (D) after carrying out solid-liquid separation, wherein pressure leaching slag (C) main component is rhombohedral iron ore, iron level is very high, and pressureleaching solution (D) nickel concentration is higher and iron/nickel ratio is lower.
Hinge structure of the present invention has following beneficial effect:
1, achieve and a kind ofly by combined leaching process sulfuric acid normal pressure leaching carried out to the high silicon magnesium ore deposit composition in limonite and with normal pressure leaching liquid, low silicon magnesium height iron ore composition carried out to the recovery nickel of pressure leaching, cobalt, the method of iron and silicon, eliminate the shortcoming of existing high pressure Ore Leaching technique, obtain the nickel higher than known normal pressure leaching technique and the cobalt rate of recovery simultaneously and reclaim speed faster, the acid consumption lower than existing high pressure acidleach, particularly in technological process, very naturally easily the main component ironworking of limonite is become Iron concentrate, part silicon is recovered as higher-grade silica product, waste residue amount is made to be reduced to about 5 percent of raw ore amount.Compared with high pressure Ore Leaching (HPAL) technique, pressure leaching of the present invention carries out under 1.5MPa-4.0Mpa, than mild condition many of high pressure acidleach 4.5MPa-5.0MPa, compared with normal pressure acidleach, the normal pressure leaching time of the present invention is 1-12 minute, and existing normal pressure leaching time is generally 240 minutes to 2400 minutes, corresponding normal pressure pickling equipment investment of the present invention is much smaller than existing normal pressure pickling equipment investment.
2, sulfuric acid consumption of the present invention not only consumes far below the acid of existing normal pressure acidleach, and consume lower than the acid of existing high pressure acidleach, the acid consumption of existing normal pressure acidleach is 2.57-3.33 times that the present invention's acid consumes, and the acid consumption of existing high pressure acidleach is 1.39-1.71 times of the present invention's acid consumption.Under high pressure acidleach condition, most sulfate ion provided by sulfuric acid is connected to form hydrogen sulfate ion (HSO
4 -), that is sulfuric acid dissociation under high pressure acidleach condition discharges a proton (H+), leach liquor cooling and in and time, hydrogen sulfate ion resolves into sulfate radical (SO
4 2-) and another proton, because after this proton (acid) is inabundant for leaching, and cause excessive sulfuric acid in subsequent disposal to be carried out and and consume neutralizing agent.And in method of the present invention, although need to consume more sulfuric acid and iron reaction generation ferric sulfate in the high silicon magnesium ore deposit normal pressure leaching stage, then do not need separately to add sulfuric acid in the low silicon magnesium height iron ore pressure leaching stage, but rely on Fe
3+the proton (acid) being hydrolyzed to hematite precipitation release leaches low silicon magnesium height iron ore, avoiding problems because of hydrogen sulfate ion (HSO
4 -) and cause the defect that acid-utilising rate is low, and significantly can reduce the consumption of follow-up neutralizing agent.In addition, existing high pressure acid leaching process ore pulp and the vitriol oil is directly added autoclave leach, and in autoclave, regional area sulfuric acid concentration is very high, is easy to generate the fouling such as ferric subsulfate and alum, and the pressure leaching stage of the present invention does not have adding of the vitriol oil, the generation of foulant can be avoided.
3, it is large that existing high pressure acid leaching process and normal pressure acid leaching process leach the quantity of slag, its leached mud is the mixing slag of silicon and iron, can not cost-effectively develop, specifically, due to the silicon-dioxide in leached mud and ferric oxide, pyrrhosiderites etc. are the fine particles that reaction generates, their mutual " growths " together, be difficult to by methods such as simple magnetic separation, they are separated, therefore the economic benefit that the leached mud utilizing existing high pressure acid leaching process and normal pressure acid leaching process to obtain develops is very poor, useless solid process can only be worked as, even must work as danger waste residue for the leached mud that nickel leaching yield is lower to process.And the main component iron in ore deposit and part silicon very naturally can be able to cost-effective recycling easily by method of the present invention in technological process.According to method of the present invention, in the normal pressure leaching stage, in high silicon magnesium ore deposit, iron and non-ferrous metal and sulfuric acid reaction generate vitriol and enter solution, silicon forms silicon-dioxide and becomes leaching residue, the 30-50% that the normal pressure leaching quantity of slag only has high silicon magnesium ore deposit to measure after solid-liquid separation, the 8-15% accounting for limonite total amount, in normal pressure leaching slag, dioxide-containing silica reaches 80-85%; In the pressure leaching stage, the Fe in normal pressure leaching liquid
3+all generate rhombohedral iron ore with the iron in low silicon magnesium height iron ore and a small amount of silicon becomes leaching residue, after solid-liquid separation, in pressure leaching slag, iron level is up to 58-65%, and namely simple process can be used as Iron concentrate and sell.
4, nickel leaching yield of the present invention is not only far above the nickel leaching yield of existing normal pressure acidleach, and higher than the nickel leaching yield of existing high pressure acidleach.The nickel leaching yield of existing normal pressure acidleach is 70-85%, and the nickel leaching yield of existing high pressure acidleach is 90-93%, and nickel leaching yield of the present invention is more than 95%.
Accompanying drawing explanation
fig. 1 is schematic flow sheet of the present invention.
Embodiment
Use in following embodiment 1
#ore is from laterite mineral deposit, New Caledonia, and washing classification obtains 2
#with 3
#ore; 4
#ore is from Philippines's laterite mineral deposit, and washing classification obtains 5
#with 6
#ore.The main component of ore is in table 1.2
#ore and 5
#ore is broken and be ground to granularity for+80 orders, 3 before for experiment
#ore and 6
#ore is broken and be ground to granularity for-80 orders before for experiment.
The main component table of table 1 ore
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1
Get 2 after 500Kg washing classification
#high silicon magnesium ore deposit (doing) adds 500Kg water and makes high silicon magnesium ore pulp, preparing 450Kg massfraction is the vitriol oil of 98%, high silicon magnesium ore pulp is heated to 60 DEG C, the high silicon magnesium ore pulp after heating and the vitriol oil synchronously to add the opening for feed of duplex pusher reactor by the vitriol oil with mortar pump and vitriol oil pump after being heated to 200 DEG C, high silicon magnesium ore pulp and the vitriol oil are forced into rapid reaction in duplex pusher reactor and, to dissolve solubility non-ferrous metal and soluble iron, react and reaction mass is released duplex pusher reactor after 1 minute after short mix.Be cooled to less than 60 DEG C, the reaction mass simple crushing of loose cellular solid-state lotion is fallen back in leaching tank, add 1500Kg water, stirring carries out water-soluble in 30 minutes, water-soluble gained slurry is pumped in plate-and-frame filter press and carries out solid-liquid separation and residue washing, obtain normal pressure leaching slag (A1) 175Kg(do), normal pressure leaching liquid (B1) 1480L and washings (E1) 1130L.The composition of normal pressure leaching slag (A1), normal pressure leaching liquid (B1) and washings (E1) is in Table 1-1, table 1-2 and table 1-3.
Get 3 after 30Kg washing classification
#low silicon magnesium height iron ore (doing), add washings (E1) 60L and be mixed with low silicon magnesium high ferro ore pulp, add in the circulation tank of capstan reactor after low silicon magnesium high ferro ore pulp is heated to 95 DEG C, in the circulation tank of capstan reactor, add the normal pressure leaching liquid (B1) being heated to 95 DEG C again makes reaction mass final ph be 0.5, force (forcing) pump is opened after sealing circulation tank, open the hot oil heater of capstan reactor simultaneously, control temperature heats, be 1.5MPa at pressure, temperature is pressure leaching 50 minutes under the condition of 240 DEG C, Fe in normal pressure leaching liquid (B1)
3+be hydrolyzed to hematite precipitation and discharge acid and leach low silicon magnesium height iron ore again, from the circulation tank of capstan reactor, shift out reaction paste after being cooled to 85 DEG C carry out solid-liquid separation and wash filter residue, obtain pressure leaching slag (C1) 28Kg(to do), pressureleaching solution (D1) 76L and washings (F1) 46L, by namely there being method reclaim nickel and/or cobalt after removing non-nickel cobalt impurity to pressureleaching solution (D1).The composition of pressure leaching slag (C1), pressureleaching solution (D1) and washings (F1) is in Table 1-4, table 1-5 and table 1-6.
Get 300g pressure leaching slag (C1) and add that to fill 1000ml massfraction be in the beaker of the soda ash solution of 10%, be heated to 60 DEG C and stir 30 minutes, solid-liquid separation is also dried after washing leaching cake under temperature is 120 DEG C of conditions, obtains rhombohedral iron ore (G1) 290g.Rhombohedral iron ore (G1) composition is in Table 1-7.
Get 300g normal pressure leaching slag (A1) and carry out hydrocyclone separation technology, obtain-100 order silicon dioxide powder (H1) 148g and+100 order fine sand (I1) 146g.Silicon dioxide powder (H1) and fine sand (I1) composition are in Table 1-8 and table 1-9.
Calculate nickel, cobalt leaching yield, slag rate and acid consumption data as follows:
Normal pressure acidleach nickel leaching yield: 98.1%; Normal pressure acidleach cobalt leaching yield: 97.1%.
Pressure leaching nickel leaching yield: 95.4%; Pressure leaching cobalt leaching yield: 93.2%.
Amount to nickel leaching yield 96.1%; Cobalt leaching yield 94.2%.
Iron recovery >96%.
Sulfuric acid consumption: 180Kg sulfuric acid/t ore deposit.
Amount to slag rate: 70.0g white residue/1000g limonite.
Embodiment 2
Get 5 after 500Kg washing classification
#high silicon magnesium ore deposit (doing) adds 600Kg water and makes high silicon magnesium ore pulp, preparing 450Kg massfraction is the vitriol oil of 98%, high silicon magnesium ore pulp is heated to 100 DEG C, the high silicon magnesium ore pulp after heating and the vitriol oil synchronously to add the opening for feed of duplex pusher reactor by the vitriol oil with mortar pump and vitriol oil pump after being heated to 150 DEG C, high silicon magnesium ore pulp and the vitriol oil are forced into rapid reaction in duplex pusher reactor and, to dissolve solubility non-ferrous metal and soluble iron, react and reaction mass is released duplex pusher reactor after 12 minutes after short mix.Be cooled to less than 60 DEG C, the reaction mass simple crushing of loose cellular solid-state lotion is fallen back in leaching tank, add 1550Kg water, stirring carries out water-soluble in 30 minutes, water-soluble gained slurry is pumped in plate-and-frame filter press and carries out solid-liquid separation and residue washing, obtain normal pressure leaching slag (A2) 220Kg(do), normal pressure leaching liquid (B2) 1490L and washings (E2) 1100L.The composition of normal pressure leaching slag (A2), normal pressure leaching liquid (B2) and washings (E2) is in Table 2-1, table 2-2 and table 2-3.
Get 6 after 40Kg washing classification
#low silicon magnesium height iron ore (doing), add washings (E2) 80L and be mixed with low silicon magnesium high ferro ore pulp, add in the circulation tank of capstan reactor after low silicon magnesium high ferro ore pulp is heated to 100 DEG C, in the circulation tank of capstan reactor, add the normal pressure leaching liquid (B2) being heated to 100 DEG C again makes reaction mass final ph be 1.5, force (forcing) pump is opened after sealing circulation tank, open the hot oil heater of capstan reactor simultaneously, control temperature heats, be 4.0MPa at pressure, temperature is pressure leaching 30 minutes under the condition of 150 DEG C, Fe in normal pressure leaching liquid (B2)
3+be hydrolyzed to hematite precipitation and discharge acid and leach low silicon magnesium height iron ore again, from the circulation tank of capstan reactor, shift out reaction paste after being cooled to 85 DEG C carry out solid-liquid separation and wash filter residue, obtain pressure leaching slag (C2) 34Kg(to do), pressureleaching solution (D2) 94L and washings (F2) 55L, by namely there being method reclaim nickel and/or cobalt after removing non-nickel cobalt impurity to pressureleaching solution (D2).The composition of pressure leaching slag (C2), pressureleaching solution (D2) and washings (F2) is in Table 2-4, table 2-5 and table 2-6.
Get 300g pressure leaching slag (C2) and add that to fill 1000ml massfraction be in the beaker of the soda ash solution of 10%, be heated to 60 DEG C and stir 30 minutes, solid-liquid separation is also dried after washing leaching cake under temperature is 150 DEG C of conditions, obtains rhombohedral iron ore (G2) 296g.Rhombohedral iron ore (G2) composition is in Table 2-7.
Get 300g normal pressure leaching slag (A2) and carry out hydrocyclone separation technology, obtain-100 order silicon dioxide powder (H2) 142g and+100 order fine sand (I2) 148g.Silicon dioxide powder (H2) and fine sand (I2) composition are in Table 2-8 and table 2-9.
Calculate nickel, cobalt leaching yield, slag rate and acid consumption data as follows:
Normal pressure acidleach nickel leaching yield: 99.0%; Normal pressure acidleach cobalt leaching yield: 95.1%.
Pressure leaching nickel leaching yield: 94.7%; Pressure leaching cobalt leaching yield: 92.2%.
Amount to nickel leaching yield 95.37%; Cobalt leaching yield 93.7%.
Iron recovery >96%.
Sulfuric acid consumption: 180Kg sulfuric acid/t ore deposit.
Amount to slag rate: 88.0g white residue/1000g limonite.
Embodiment 3
The normal pressure acid leaching stage of the present embodiment is identical with embodiment 1, in the pressure leaching stage by 3
#new noise made in coughing or vomiting low silicon high ferro magnesium ore deposit has changed 6 into
#philippines's low silicon magnesium height iron ore.
Get 6 after 30Kg washing classification
#low silicon magnesium height iron ore (doing), add washings (E1) 60L and be mixed with low silicon magnesium high ferro ore pulp, add in the circulation tank of capstan reactor after low silicon magnesium high ferro ore pulp is heated to 95 DEG C, in the circulation tank of capstan reactor, add the normal pressure leaching liquid (B1) being heated to 95 DEG C again makes reaction mass final ph be 1.0, force (forcing) pump is opened after sealing circulation tank, open the hot oil heater of capstan reactor simultaneously, control temperature heats, be 2.0MPa at pressure, temperature is pressure leaching 60 minutes under the condition of 223 DEG C, Fe in normal pressure leaching liquid (B1)
3+be hydrolyzed to hematite precipitation and discharge acid and leach low silicon magnesium height iron ore again, from the circulation tank of capstan reactor, shift out reaction paste after being cooled to 85 DEG C carry out solid-liquid separation and wash filter residue, obtain pressure leaching slag (C3) 29Kg(to do), pressureleaching solution (D3) 76L and washings (F3) 44L, by namely there being method reclaim nickel and/or cobalt after removing non-nickel cobalt impurity to pressureleaching solution (D3).The composition of pressure leaching slag (C3), pressureleaching solution (D3) and washings (F3) is in Table 3-1, table 3-2 and table 3-3.
Get 300g pressure leaching slag (C3) and add that to fill 1000ml massfraction be in the beaker of the soda ash solution of 10%, be heated to 60 DEG C and stir 30 minutes, solid-liquid separation is also dried after washing leaching cake under temperature is 130 DEG C of conditions, obtains rhombohedral iron ore (G3) 296g.Rhombohedral iron ore (G3) composition is in Table 3-4.
Get 300g normal pressure leaching slag (A1) and carry out hydrocyclone separation technology, obtain-100 order silicon dioxide powder (H1) 148g and+100 order fine sand (I1) 146g.
Calculate nickel, cobalt leaching yield, slag rate and acid consumption data as follows:
Pressure leaching nickel leaching yield: 94.6%; Pressure leaching cobalt leaching yield: 93.4%.
Amount to nickel leaching yield 95.5%; Cobalt leaching yield 94.5%.
Iron recovery >96%.
Sulfuric acid consumption: 180Kg sulfuric acid/t ore deposit.
Amount to slag rate: 70.0g white residue/1000g limonite.
Embodiment 4
The normal pressure acid leaching stage of the present embodiment is identical with embodiment 2, in the pressure leaching stage by 6
#philippines's low silicon magnesium height iron ore has changed 3 into
#new noise made in coughing or vomiting low silicon magnesium height iron ore.
Get 40Kg1
#after washing classification 3
#low silicon magnesium height iron ore (doing), add washings (E1) 80L and be mixed with low silicon magnesium high ferro ore pulp, add in the circulation tank of capstan reactor after low silicon magnesium high ferro ore pulp is heated to 100 DEG C, in the circulation tank of capstan reactor, add the normal pressure leaching liquid (B1) being heated to 100 DEG C again makes reaction mass final ph be 1.5, force (forcing) pump is opened after sealing circulation tank, open the hot oil heater of capstan reactor simultaneously, control temperature heats, be 3MPa at pressure, temperature is pressure leaching 45 minutes under the condition of 185 DEG C, Fe in normal pressure leaching liquid (B1)
3+be hydrolyzed to hematite precipitation and discharge acid and leach low silicon magnesium height iron ore again, from the circulation tank of capstan reactor, shift out reaction paste after being cooled to 85 DEG C carry out solid-liquid separation and wash filter residue, obtain pressure leaching slag (C4) 38Kg(to do), pressureleaching solution (D4) 94L and washings (F4) 55L, by namely there being sulfide precipitation method reclaim nickel and/or cobalt after removing non-nickel cobalt impurity to pressureleaching solution (D4).The composition of pressure leaching slag (C4), pressureleaching solution (D4) and washings (F4) is in Table 4-1, table 4-2 and table 4-3.
Get 300g pressure leaching slag (C4) and add that to fill 1000ml massfraction be in the beaker of the soda ash solution of 10%, be heated to 60 DEG C and stir 30 minutes, solid-liquid separation is also dried after washing leaching cake under temperature is 140 DEG C of conditions, obtains rhombohedral iron ore (G4) 293g.Rhombohedral iron ore (G4) composition is in Table 4-4.
Get 300g normal pressure leaching slag (A2) and carry out hydrocyclone separation technology, obtain-100 order silicon dioxide powder (H2) 142g and+100 order fine sand (I2) 148g.
Calculate nickel, cobalt leaching yield, slag rate and acid consumption data as follows:
Pressure leaching nickel leaching yield: 93.9%; Pressure leaching cobalt leaching yield: 92.8%.
Amount to nickel leaching yield 95.3%; Cobalt leaching yield 93.2%.
Iron recovery >96%.
Sulfuric acid consumption: 180Kg sulfuric acid/t ore deposit.
Amount to slag rate: 88.0g white residue/1000g limonite.
Embodiment 5 (reference examples)
The normal pressure acid leaching stage of the present embodiment is identical with embodiment 1, in the pressure leaching stage by 4
#new noise made in coughing or vomiting low silicon magnesium height iron ore has changed 4 into
#philippines's limonite.
Get 30Kg4
#philippines's limonite (doing), add washings (E1) 60L and be mixed with limonite slurry, add in the circulation tank of capstan reactor after limonite slurry being heated to 95 DEG C, in the circulation tank of capstan reactor, add the normal pressure leaching liquid (B1) being heated to 95 DEG C again makes reaction mass final ph be 1.0, force (forcing) pump is opened after sealing circulation tank, open the hot oil heater of capstan reactor simultaneously, control temperature heats, be 2.0MPa at pressure, temperature is pressure leaching 60 minutes under the condition of 223 DEG C, Fe in normal pressure leaching liquid (B1)
3+be hydrolyzed to hematite precipitation and discharge acid and leach limonite again, from the circulation tank of capstan reactor, shift out reaction paste after being cooled to 85 DEG C carry out solid-liquid separation and wash filter residue, obtain pressure leaching slag (C5) 29Kg(to do), pressureleaching solution (D5) 76L and washings (F5) 47L, by namely there being sulfide precipitation method reclaim nickel and/or cobalt after removing non-nickel cobalt impurity to pressureleaching solution (D5).The composition of pressure leaching slag (C5), pressureleaching solution (D5) and washings (F5) is in Table 5-1, table 5-2 and table 5-3.
Get 300g pressure leaching slag (C5) and add that to fill 1000ml massfraction be in the beaker of the soda ash solution of 10%, be heated to 60 DEG C and stir 30 minutes, solid-liquid separation is also dried after washing leaching cake under temperature is 120 DEG C of conditions, obtains rhombohedral iron ore (G5) 297g.Rhombohedral iron ore (G5) composition is in Table 5-4.
Calculate nickel, cobalt leaching yield, slag rate and acid consumption data as follows:
Pressure leaching nickel leaching yield: 94.8%; Pressure leaching cobalt leaching yield: 92.4%.
Amount to nickel leaching yield 95.4%; Cobalt leaching yield 93.7%.
Iron recovery >96%.
Sulfuric acid consumption: 180Kg sulfuric acid/t ore deposit.
Amount to slag rate: 70.0g white residue/1000g limonite.
In above embodiment, embodiment 1 and the embodiment 2 high silicon magnesium ore deposit in the limonite of same mineral deposit and the combination of low silicon magnesium ore deposit; Embodiment 3 and the embodiment 4 high silicon magnesium ore deposit in the limonite of different mineral deposits and the combination of low silicon magnesium ore deposit; As a comparison, the embodiment 5 high silicon magnesium ore deposit in limonite and the combination of limonite raw ore.From analytical data, the technical indicator such as nickel (cobalt) leaching yield, sulfuric acid consumption etc. of five embodiments is all better, but what adopt due to embodiment 5 is high silicon magnesium ore deposit in limonite and the combination of limonite raw ore, therefore the iron level of pressure leaching slag is only 54.64%, the rhombohedral iron ore iron content about 54% reclaimed, and the iron level of the pressure leaching slag that other four embodiments obtain is all more than 63%, the rhombohedral iron ore iron level of recovery is all about 63%, and iron recovery is more than 96%.Amount to slag rate about 80.0g white residue/1000g limonite, about slag rate is down to 40g white residue/1000g limonite after reclaiming silicon-dioxide.
Claims (10)
1. from limonite, reclaimed a method for nickel, cobalt, iron and silicon by combined leaching process, it is characterized in that: comprise the following steps:
A () obtains high silicon magnesium ore deposit and low silicon magnesium height iron ore to limonite washing classification, add water obtained high silicon magnesium ore pulp in high silicon magnesium ore deposit;
B high silicon magnesium ore pulp is heated to 60 DEG C-100 DEG C by (), the vitriol oil is heated to 150 DEG C-200 DEG C, adds the high silicon magnesium ore pulp after heating and the vitriol oil, react to dissolve solubility non-ferrous metal and soluble iron in duplex pusher reactor;
C () carries out water-soluble rear solid-liquid separation to reaction mass and residue washing obtains normal pressure leaching slag (A), normal pressure leaching liquid (B) and washings (E);
D () makes low silicon magnesium high ferro ore pulp with washings (E) and low silicon magnesium height iron ore, add in capstan reactor after low silicon magnesium high ferro ore pulp and normal pressure leaching liquid (B) are heated to 95 DEG C-100 DEG C respectively, pressure be 1.5MPa-4.0Mpa, temperature be the condition of 150 DEG C-240 DEG C under pressure leaching 0.5-1.5 hour, the Fe in normal pressure leaching liquid (B)
3+be hydrolyzed to hematite precipitation and discharge acid and leach low silicon magnesium height iron ore again;
E () is reduced temperature and carry out solid-liquid separation after 80 DEG C, obtain pressure leaching slag (C) and pressureleaching solution (D);
By namely there being method to reclaim nickel and/or cobalt f () removes non-nickel cobalt impurity to pressureleaching solution (D) after;
G () obtains Iron concentrate to pressure leaching slag (C) soda ash solution washing post-drying;
H () obtains silicon-dioxide and fine sand to normal pressure leaching slag (A) through screening process.
2. a kind of method being reclaimed nickel, cobalt, iron and silicon by combined leaching process from limonite according to claim 1, be is characterized in that: in described step (a), the granularity in high silicon magnesium ore deposit is+80 orders, and the granularity of low silicon magnesium height iron ore is-80 orders.
3. a kind of method being reclaimed nickel, cobalt, iron and silicon by combined leaching process from limonite according to claim 1, be is characterized in that: in described step (a), the mass ratio of high silicon magnesium ore deposit and water is 1:1.2-1:1.
4. a kind of method being reclaimed nickel, cobalt, iron and silicon by combined leaching process from limonite according to claim 1, it is characterized in that: in described step (b), the mass ratio of high silicon magnesium ore pulp and the vitriol oil is 20:9-22:9, the reaction times is 1-12 minute.
5. a kind of method being reclaimed nickel, cobalt, iron and silicon by combined leaching process from limonite according to claim 1, be is characterized in that: time water-soluble in described step (c), the mass ratio of reaction mass and water is 29:30-1:1.
6. a kind of method being reclaimed nickel, cobalt, iron and silicon by combined leaching process from limonite according to claim 1, be is characterized in that: proportioning when washings (E) and low silicon magnesium height iron ore make low silicon magnesium high ferro ore pulp in described step (d) is 2L:1Kg.
7. a kind of method being reclaimed nickel, cobalt, iron and silicon by combined leaching process from limonite according to claim 1, be is characterized in that: in low silicon magnesium high ferro ore pulp, add normal pressure leaching liquid (B) in described step (d) and make reaction mass final ph be 0.5-1.5.
8. a kind of method being reclaimed nickel, cobalt, iron and silicon by combined leaching process from limonite according to claim 1, be is characterized in that: in described step (g), the massfraction of soda ash solution is 10%, and bake out temperature is 120 DEG C-150 DEG C.
9. a kind of method being reclaimed nickel, cobalt, iron and silicon by combined leaching process from limonite according to claim 1, it is characterized in that: in described step (c), normal pressure leaching slag (A) is white residue, and its dioxide-containing silica is 65%-90%.
10. a kind of method being reclaimed nickel, cobalt, iron and silicon by combined leaching process from limonite according to claim 1, it is characterized in that: obtain pressure leaching slag (C) in described step (e) for rhombohedral iron ore slag, wherein iron level is 58%-65%.
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