CN101525690A - Method for separating and recovering nickel, cobalt, magnesium, iron and silicon from nickel-bearing laterite - Google Patents
Method for separating and recovering nickel, cobalt, magnesium, iron and silicon from nickel-bearing laterite Download PDFInfo
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- CN101525690A CN101525690A CN200910113991A CN200910113991A CN101525690A CN 101525690 A CN101525690 A CN 101525690A CN 200910113991 A CN200910113991 A CN 200910113991A CN 200910113991 A CN200910113991 A CN 200910113991A CN 101525690 A CN101525690 A CN 101525690A
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Abstract
A method for separating and recovering nickel, cobalt, magnesium, iron and silicon from nickel-bearing laterite is disclosed; nickel, cobalt, magnesium and iron therein are leached out by using high-temperature peracid, leachate is pre-neutralized via serpentine powder, after the pre-neutralization, the leachate is neutralized by magnesite powder for de-ironing, and the scum is delivered for ironmaking after being dewatered by smoke gases in a fluidized bed furnace for making sulfuric acid, the de-ironed clear nickel liquid uses magnesite powder to precipitate nickel carbonate, and the precipitated liquid is concentrated and crystallized to obtain magnesium sulfate heptahydrate. The leached slag mainly contains silicon and can be used for making white carbon black. The invention can sufficiently recover and utilize nickel, cobalt, magnesium, iron and silicon in the nickel-bearing laterite, and the invention is simple in technology, low in energy consumption and pollution-free on environment.
Description
One, technical field
The present invention relates to a kind of Wet-smelting method of red soil nickel ore, particularly the method for Separation and Recovery nickel cobalt, magnesium, iron and silicon from red soil nickel ore.
Two, background technology
Red soil nickel ore is divided into two types, a kind of is the limonite type, and iron height, nickel are low, and silicon, magnesium are lower, but cobalt contents is higher, by traditional method, this ore should adopt wet method smelting process to handle, but general hydrometallurgy is low to the leaching yield of nickel cobalt, if adopt high pressure to leach, magnesium wherein scabs easily, causes operational difficulty, and autoclave is not long work-ing life.Another kind is a noumeite, and nickel content is higher, thinks that in the past this ore should adopt pyrometallurgical smelting process to handle, but the blast furnace smelting in the pyrometallurgical smelting, because technology falls behind, environment there is reason such as pollution be eliminated, so most at present electrosmelting that adopts.Electrosmelting needs high temperature, the also bad solution of energy consumption height, furnace building material, and furnace life is short.Yet there are no the report of more satisfactory low-grade red soil nickel ore smelting technology.
Three, summary of the invention
The object of the present invention is to provide a kind of from red soil nickel ore the method for Separation and Recovery nickel cobalt, magnesium, iron and silicon, this method can be handled the red soil nickel ore of the low magnesium of high ferro or high magnesium of low iron or the high magnesium of high ferro effectively, not only can high efficiente callback nickel cobalt wherein, iron wherein can also be used for ironmaking, all generate sal epsom with dissolving the magnesium that, silicon can be used for producing white carbon black.
The present invention achieves the above object by the following technical programs: a kind of from red soil nickel ore the method for Separation and Recovery nickel cobalt, magnesium, iron and silicon, this method comprises the steps:
Adopting the main component of raw material red soil nickel ore is (wt%): Ni 0.8~3.0, and Co 0.02~0.2, and Fe 10~50, and MgO 0.5~50, SiO
210~50, Cr
2O
31~5, all the other earth or other mineral for sneaking in the mining comprise aluminium copper-manganese calcium.
A, with described raw material with 2~8mol/L H
2SO
4, the solid-to-liquid ratio by 1: 2~8 at 80~95 ℃, leached 1~4 hour, obtained leach liquor through press filtration,
B, with snake stone flour pre-neutralization described leach liquor, add the snake stone flours down in 80 ℃~95 ℃, react 0.5~1 hour, liquid after the pre-neutralization,
C, liquid is used in the magnesite breeze and deironing after the described pre-neutralization, under 50 ℃~90 ℃, the stepwise dilution deironing, add the water of 1/3rd grooves the first time in first iron removal trough, use clean nickel liquid later on, stir, add the magnesite breeze, slowly add iron-containing liquor, keep ferric ion at pH 1.5~2.0 slow hydrolytic precipitations, when terminal point is pH 2.5, it is anti-molten to begin that throw out is added sulfuric acid, molten always to pH 2, continues reaction 5~10min, press filtration, filtrate pumps into the header tank of second iron removal trough, flows into second iron removal trough again, and the same working method of the employing and first iron removal trough is carried out deironing, second iron removal trough control deironing terminal point is pH3.5~3.8, check that solution not during iron content, filters immediately, filtrate is pressed into clean nickel liquid storage tank, after twice deironing, obtain clean nickel liquid and deironing filter residue
D, usefulness magnesite breeze precipitation nickelous carbonate, under 60 ℃~85 ℃, in heavy nickel groove, add clean nickel liquid, stir, adds excessive magnesite reaction, check that supernatant liquor does not have the color of nickel and reaches pH8~8.3 to be and to sink the nickel terminal point, stop to stir, treat that the nickelous carbonate throw out is deposited to 1/3rd of groove, filter nickelous carbonate throw out and heavy nickel filtrate
E, described nickelous carbonate throw out is purified, earlier described nickelous carbonate throw out filter is done, sulfuric acid dissolution is used in the back, and it is not tolerant to remove by filter acid, and filtrate is settled out nickel hydroxide with sodium hydroxide, and filtration washing obtains nickel hydroxide, sends to refining,
F, will precipitate supernatant liquor that nickelous carbonate obtains and heavy nickel filtrate and adopt concentration tank to carry out condensing crystal to obtain magnesium sulfate heptahydrate, dry with whizzer and promptly get the magnesium sulfate heptahydrate product,
G, deironing filter residue that the c step is obtained be through compressing and washing, and after being washed till water outlet and not having the color of nickel,, dewaters with fluidized bed roasting system vitriolic fluidizing furnace flue gas drying to below the moisture 15wt% with the high-pressure air blow pressure again, and the gained scum is sent to ironmaking.
Outstanding advantage of the present invention is:
1, nickel cobalt magnesium iron that leaching is come out in the red soil nickel ore and the silicon stayed in the slag can comprehensive reutilizations.
2, adopt the high temperature peracid to leach red soil nickel ore, nickel cobalt extraction yield height, magnesium iron aluminum bronze chromium manganese is also dissolved simultaneously, but nickel ferro-cobalt aluminum bronze chromium manganese is not taken away sulfate radical in leach liquor deironing and heavy nickel stage, sulfate radical is just walked to generate sal epsom by magnesium ribbon, sulfuric acid is used for dissolving all soluble metal elements in theory, but during owing to the hydrolysis of nickel ferro-cobalt aluminum bronze chromium manganese, emit equimolar sulfuric acid again and removed to dissolve equimolar magnesium, elements such as iron have played individual intermediate axle beam effect here, that is to say, in fact dissolve nickel ferro-cobalt aluminum bronze chromium manganese and all do not consume sulfuric acid, overwhelming majority sulfuric acid is to be used for dissolved magnesium generation sal epsom, therefore leaches and is not afraid of consumption acid height, till the leaching yield with nickel cobalt magnesium iron reaches satisfaction.
3, adopt nickeliferous snake stone flour that the leach liquor of high acidity is carried out pre-neutralization or directly snake stone flour and red soil nickel ore are leached simultaneously, enlarged the resource that reclaims useful nickel ferro-cobalt magnesium, wherein the dissolved sulfuric acid that also do not consume of nickel ferro-cobalt also is to come dissolved magnesium by the acid that hydrolysis is emitted.Want to improve the leaching yield of nickel cobalt in the snake stone flour and the stripping quantity of iron magnesium, nickeliferous snake stone flour and red soil nickel ore can be joined the ore deposit by arbitrary proportion and leach simultaneously, even individual curing snake stone flour can.
If 4 adopt in the snake stone flours and deironing, iron can not be eliminated, because molten iron is separated and emitted acid and remove to dissolve the iron of self again, move in endless cycles like this, forever endless.If adopt the neutralization of lime or limestone powder, will generate calcium sulfate, not only make sulfuric acid cause loss, and sulphur has been brought in the scum, scum just can not be used for ironmaking.In order to make scum can be used in ironmaking, and can make full use of sulfuric acid, so selected the neutralizing agent of magnesite breeze as deironing, this is first bright spot of the present invention.
5, for magnesium can be reclaimed with the form of sal epsom, in the solution that sal epsom is all concentrated, just can not come coprecipitated nickel hydroxide with sodium hydroxide or yellow soda ash, otherwise cause in the Adlerika of whole technology and sneak into sodium sulfate, make the technology that reclaims magnesium just become more complicated, it is very high that production cost can become.So must adopt the magnesite breeze to precipitate nickelous carbonate, this has just guaranteed that in the solution of total system all be sal epsom, thereby has guaranteed the quality that scum is used to smelt iron, and has also guaranteed the quality product of sal epsom, and this is second bright spot of the present invention.
With the nickel cobalt magnesium iron aluminium chromium manganese of sulfuric acid dissolution, except generation calcium sulfate was taken away sulfate radical, having only magnesium was to be with sulfate radical SO
4 =Generate sal epsom.Calculate according to molecular formula, 1 ton of sulfuric acid of every input will produce 2.5 tons of magnesium sulfate heptahydrates in the leaching, 1.4 tons of magnesium sulfate monohydrates, 1.2 tons of anhydrous magnesium sulfates.Drop into 1 ton of sulfuric acid, just reclaim magnesium this, approximately can obtain the sal epsom product of 4~8 tons of sulfate values.Direct condensing crystal sal epsom has replaced yellow soda ash and has changed into magnesiumcarbonate, has also reduced the cost recovery of magnesium.Iron can attach recovery, and silicon has obtained highly enriched, and being convenient to produce silicon is product.So it is good that the present invention handles the economic benefit of red soil nickel ore.
6, the present invention has adopted the technology of two sections deironing, total iron amount in the system can not increase, again dissolved once if each deironing all has 50% iron to return, return so and the iron amount of discharging of opening a way is invariable, just the sulfuric acid consumption has strengthened, the consumption of magnesite has increased, thereby make the meltage of magnesium also more, in isopyknic solution, the concentration of sal epsom has improved, the energy consumption of condensing crystal sal epsom has reduced, and the output of sal epsom has also just improved more.So iron ion is returned in pickling, not only reduced the loss of nickel, also reduced the production cost of sal epsom, this is the 3rd bright spot of the present invention.
7, the present invention has adopted the method for stepwise dilution deironing different with traditional method for removing iron.Traditional method for removing iron has the siderotil method, goethite process, hematite process, they all be unable to do without high temperature even High Temperature High Pressure, they all be unable to do without finally will become ferric ion, and especially goethite process at first will be reduced into divalence with ferric ion, then again under the situation of the high power consumption of high temperature, oxidation of divalent iron ion is become trivalent, turn from side to side so repeatedly and just obtain the good scum of strainability.Method for removing iron of the present invention, neither need high temperature, also no matter the iron ion in the solution is trivalent or divalence, can carry out the deironing operation, and simple to operate, easily control, the strainability of the scum that obtains and not second to pyrrhosiderite slag and iron vitriol slag, even also want better, this is the 4th bright spot of the present invention.
8, technology of the present invention is simple, and the device processes ability is big.Adopt peracid to leach under normal pressure, the short period of time just can reach the nickel cobalt magnesium iron aluminium chromium manganese in the red soil nickel ore dissolving of satisfaction.The strainability of various solid products is all good, only needs press filtration to compress and wash, just can residue washing is clean, do not need to build thickening pond, and so the device fabrication expense is few, initial cost is low.
9, production run cost of the present invention is low, and energy expenditure is low.Only need to drop into chemical reagent sulfuric acid, magnesite breeze and snake stone flour all are that purposes and cheap additive are arranged, and reagent cost is very low.Leaching is general high temperature peracid process, but the time is short.Deironing and heavy nickel can utilize the waste heat of an operation or carry out under lower temperature.Since the magnesium ion concentration height in the solution, condensing crystal magnesium sulfate heptahydrate, the few and conservation measures in addition of power consumption.Though the content height of scum crystal water can utilize fluidized bed roasting system vitriolic flue gas to make scum slough crystal water fully, so the energy expenditure of the whole technology of the present invention is low.
10, deironing terminal point of the present invention is pH3.5~3.8, and Fe, Al remove together, and Cu, Cr, Mn stay in the nickel liquid.The precipitation terminal point of nickel is pH8~8.3, Cu, Cr, Mn, Ni, Co coprecipitation.Nickelous carbonate is controlled at pH5~6 with the terminal point of sulfuric acid solution, Cu, Cr stay in the sour molten residue, residue returns, Cu, the Cr accumulation that in solution, circulates, when waiting to run up to finite concentration, the terminal point pH of the molten nickelous carbonate of acid is reduced to 2.5~3, and Cu, Cr, Mn, Ni enter solution together, separate with magnesite breeze insolubles.The Cu, the Cr that enter in the solution can separate with Ni, Mn by the precipitator method, and just have only Mn, the Ni that enter P204 extraction deep impurity-removing have at last separated, and can make the operation of P204 extraction process simpler.Remaining Cu, Cr separate also not difficult.So processing condition of the present invention make the separation of various impurity elements become easier.
Five, specific embodiment
Below by embodiment technical scheme of the present invention is described in further detail.
Of the present invention from red soil nickel ore the method for Separation and Recovery nickel cobalt, magnesium, iron and silicon, this method comprises the steps:
1, sulfuric acid leaches
Get red soil nickel ore raw material 270 grams, main component is (wt%): Ni 1.82, Co 0.043, Fe 19.80, Mg 7.97.Add 628g/L H at 1: 3 by solid-to-liquid ratio
2SO
4, under 90 ℃, leached 2h, use the B suction filtration, obtain leaching filtrate 930ml and filter cake 527 grams, the moisture 61.54wt% of filter cake does the quantity of slag 203 grams, and dried slag contains Ni 0.13wt%.Press raw ore 270 grams, contain Ni 1.82wt% meter, the leaching yield of nickel is 94.63wt%.
2, with the described leaching of snake stone flour pre-neutralization filtrate
Get the filtrate 930ml of the 1st step, add the 200 gram pre-neutralizations of snake stone flour, under 95 ℃, reaction 40min, filtration washing, get pre-neutralization filtrate 900ml and filter cake 188 grams, the moisture 35.79wt% of filter cake, dried slag weigh 121 grams, and dried slag contains Ni 0.1wt%, contain Ni 1.42wt% by the snake stone flour, the leaching yield 95.74wt% of nickel.
3, with the deironing of magnesite breeze precipitation
Elder generation joins 15g magnesite breeze in the 200ml water and stirs, and under 75 ℃, adds 125ml pre-neutralization filtrate by 10g magnesite breeze, pre-neutralization filtrate is slowly joined in the solution of magnesite, adds 625ml pre-neutralization filtrate, 50g magnesite breeze altogether.Regulate pH to 5~6 with the magnesite breeze, check that solution does not have Fe
+++Promptly stop, begin to filter, obtain 2350ml deironing filtrate.That analyzes the scum filter cake contains (wt%): Fe31.46, and Ni 3.23.
4, nickel falls in the scum pickling
Get the scum filter cake 100g of the above-mentioned Ni of containing 3.34wt%, add 200ml water and size mixing, under 80 ℃, transfer to pH 1.5 with sulfuric acid, stir about 30 minutes, filter filter cake 58g, analyze filter cake and contain Ni 0.11wt%, flush away the quantity of slag of 42wt%, also washed out the nickel of 98wt%.So the measure of two sections deironing is taked in decision on technology.First segment endpoint is in pH1.5~2, and the low ferronickel slag of output is the open circuit slag, and second segment endpoint obtains the clean nickel liquid of iron-free in pH3.5~3.8, and nickelic scum returns and dissolves deironing again.
5, with magnesite breeze precipitation nickelous carbonate
Get 1 liter of the clean nickel liquid that contains Ni 3g/L, add the magnesite breeze under 50 ℃ of stirrings, become limpidly up to supernatant liquor, heavy nickel step is finished, filter, thick nickelous carbonate filter cake component content (wt%): Ni 20.21, and Co 0.20.
6, thick nickelous carbonate sulfuric acid dissolution, sodium hydroxide transforms purifies
With thick nickelous carbonate filter cake sulfuric acid dissolution, the elimination insolubles, the insolubles retrieval system, filtrate is used the industrial sodium hydroxide coprecipitated nickel hydroxide, filters, and gets the nickel hydroxide filter cake, sends to refining.
7, get the heavy later Adlerika condensing crystal of nickel of magnesite breeze, obtain magnesium sulfate heptahydrate, its component content is (wt%): Mg 10.46, Ni 0.0012, and the content of nickel in the magnesium sulfate heptahydrate product seldom illustrates when sinking nickel, nickel magnesium good separating effect, the precipitate recovery rate height of nickel.
Claims (1)
1, a kind of from red soil nickel ore the method for Separation and Recovery nickel cobalt, magnesium, iron and silicon, this method comprises the steps:
Adopting the main component of raw material red soil nickel ore is (wt%): Ni 0.8~3.0, and Co 0.02~0.2, and Fe 10~50, and MgO 0.5~50, SiO
210~50, Cr
2O
31~5, all the other earth or other mineral for sneaking in the mining comprise aluminium copper-manganese calcium,
A, with described raw material with 2~8mol/L H
2SO
4, the solid-to-liquid ratio by 1: 2~8 at 80~95 ℃, leached 1~4 hour, obtained leach liquor through press filtration,
B, with snake stone flour pre-neutralization described leach liquor, add the snake stone flours down in 80 ℃~95 ℃, react 0.5~1 hour, liquid after the pre-neutralization,
C, liquid is used in the magnesite breeze and deironing after the described pre-neutralization, under 50 ℃~90 ℃, the stepwise dilution deironing, add the water of 1/3rd grooves the first time in first iron removal trough, use clean nickel liquid later on, stir, add the magnesite breeze, slowly add iron-containing liquor, keep ferric ion at pH 1.5~2.0 slow hydrolytic precipitations, when terminal point is pH 2.5, it is anti-molten to begin that throw out is added sulfuric acid, molten always to pH 2, continues reaction 5~10min, press filtration, filtrate pumps into the header tank of second iron removal trough, flows into second iron removal trough again, and the same working method of the employing and first iron removal trough is carried out deironing, second iron removal trough control deironing terminal point is pH3.5~3.8, check that solution not during iron content, filters immediately, filtrate is pressed into clean nickel liquid storage tank, after twice deironing, obtain clean nickel liquid and deironing filter residue
D, usefulness magnesite breeze precipitation nickelous carbonate, under 60 ℃~85 ℃, in heavy nickel groove, add clean nickel liquid, stir, add excessive magnesite reaction, checking that supernatant liquor does not have the color of nickel and reaches pH8~8.3 is heavy nickel terminal point, stops to stir, and treats that the nickelous carbonate throw out is deposited to emit supernatant liquor three of groove/a period of time, keep throw out, after the operation of heavy nickel is carried out 4 to 8 times, filter nickelous carbonate throw out and heavy nickel filtrate
E, described nickelous carbonate throw out is purified, earlier described nickelous carbonate throw out filter is done, sulfuric acid dissolution is used in the back, and it is not tolerant to remove by filter acid, and filtrate is settled out nickel hydroxide with sodium hydroxide, and filtration washing obtains nickel hydroxide, sends to refining,
F, will precipitate supernatant liquor that nickelous carbonate obtains and heavy nickel filtrate and adopt concentration tank to carry out condensing crystal to obtain magnesium sulfate heptahydrate, dry with whizzer and promptly get the magnesium sulfate heptahydrate product,
G, deironing filter residue that the c step is obtained be through compressing and washing, and after being washed till water outlet and not having the color of nickel,, dewaters with fluidized bed roasting system vitriolic fluidizing furnace flue gas drying to below the moisture 15wt% with the high-pressure air blow pressure again, and the gained scum is sent to ironmaking.
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