CN104805283A - Method for processing laterite-nickel ore by combination of atmospheric pressure acid leaching and medium pressure leaching - Google Patents
Method for processing laterite-nickel ore by combination of atmospheric pressure acid leaching and medium pressure leaching Download PDFInfo
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Abstract
The invention aims to provide a laterite-nickel ore hydrometallurgy process with low acid consumption and high leaching rate and relates to a processing method for carrying out sulfuric acid atmospheric pressure leaching on saprolite and carrying out pressure leaching on limonite with an atmospheric pressure leaching agent by the same process. Saprolite and limonite are processed by the same process, and by the atmospheric pressure acid leaching and medium pressure leaching combined process, the defect that costs and high maintenance fees are high because an existing high pressure acid leaching process requires an autoclave and related equipment is overcome, and the technical problem that the existing acid leaching process has high acid consumption and is only limited to processing of limonite materials is solved. The process provided by the invention has beneficial effects as follows: the process provided by the invention has higher nickel and cobalt recovery rate than an atmospheric pressure leaching process and is easy to effectively separate leaching residues.
Description
Technical field
the present invention relates to the hydrometallurgical processes of red soil nickel ore, in same technique, sulfuric acid normal pressure leaching carried out to saprolite in particular to a kind of and utilize normal pressure leaching liquid to carry out the treatment process of pressure leaching to limonite.
Background technology
Laterite also claims red soil nickel ore, it is the nickel oxide ore gone bad through extensive long-term weathering leaching in the torrid zone or subtropical zone by nickeliferous peridotites, 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.
Usually, people's subjectivity laterite mineral deposit is divided into three layers from top to bottom, i.e. limonite ore bed, transition ore deposit ore bed and saprolite (vegetable mould) ore bed.Limonite is height waste mantle, and its particle is trickle, and nickel, silicon, Mg content are lower, but iron level is higher.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, and wherein nickel, silicon, Mg content are higher, and corresponding iron level is lower.In some mineral deposits, also have that another kind of to be usually between limonite and saprolite main containing nontonite clays band, be called transition ore deposit, in transition ore deposit, the content of each composition is between therebetween.
Generally, limonite is the chief component of red soil nickel ore, accounts for 65% ~ 75% of laterite total amount; Saprolite accounts for 15% ~ 25%; Transition ore deposit accounts for 10%.
The where the shoe pinches reclaiming nickel (cobalt) from laterite nickel is, usually not by these useful components of the abundant enrichment 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 causes 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 red soil nickel ore can be divided into thermal process and the large class of wet processing two.
Fire metallurgy process is applicable to process saprolite ore deposit, and 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 techniques such as normal pressure acidleach, dump leaching.
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 than more according to the sulfuric acid needed for the non-ferrous metal components in stoichiometry dissolving 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 in causing excessive sulfuric acid must carry out when subsequent disposal 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, can not cost-effectively develop.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.
Summary of the invention
The object of this invention is to provide the method that the high normal pressure acidleach of a kind of less acid-consuming, leaching yield and middle pressure leach the process red soil nickel ore that combines
The present invention is achieved through the following technical solutions above-mentioned purpose:
Normal pressure acidleach and middle pressure leach a method for the process red soil nickel ore that combines, comprise the following steps:
A, making by being ground to-80 object saprolite ore deposits the ore pulp that solid content is 40%-60%, saprolite ore pulp and the vitriol oil being added in steel lining alloy reaction tank and reacting, to dissolve most solubility non-ferrous metal and soluble iron;
B, the reaction mass in above-mentioned a step and water to be dissolved with the mass ratio of 1:0.8 ~ 1:1.5, and solid-liquid separation obtains normal pressure leaching slag A and normal pressure leaching liquid B;
C, limonite make the ore pulp that solid content is 40%-60%, the normal pressure leaching liquid B of above-mentioned b step gained and limonite ore pulp are added capstan reactor, at 150 DEG C ~ 240 DEG C, pressure leaching under 1.5MPa ~ 4.0MPa condition, after leaching 0.5 ~ 1.5h, carry out solid-liquid separation, obtain pressure leaching slag C and pressureleaching solution D;
D, by the pressureleaching solution D clarification of above-mentioned step c gained, reclaim nickel, cobalt by sulfide or precipitation of hydroxide.
Wherein in step a, the vitriol oil and saprolite ore deposit are that the amount of 0.8:1 ~ 1.2:1 adds with mass ratio.
Wherein step a reacts at ambient pressure, reaction times 1 ~ 12min.
Wash to obtain washings E to the normal pressure leaching slag A in step b and the pressure leaching slag C in step c, washings E is for the preparation of limonite ore pulp.
The add-on wherein controlling normal pressure leaching liquid B and limonite ore pulp in step c makes the final pH value of reaction mass between 0.5 ~ 1.5.
Temperature of reaction wherein in rate-determining steps a is between 95 DEG C ~ 120 DEG C.
Wherein in step b, in normal pressure leaching slag A, dioxide-containing silica is 65% ~ 90%.
Wherein obtaining iron level in pressure leaching slag C in step c is 58% ~ 65%.
Wherein in step c, temperature is preferably 210 DEG C ~ 240 DEG C.
The first step is in saprolite acidleach process, the vitriol oil of saprolite ore pulp and q.s fully mixes fast, the heat of dilution that water in the vitriol oil and ore pulp produces makes temperature of charge raise to impel metal (nickel, cobalt, iron, magnesium, chromium, aluminium etc.) in saprolite ore deposit and sulfuric acid rapid reaction generation metal sulfate, the stopping property of invar lining alloy retort is good, preheating can not be shifted to an earlier date to saprolite ore pulp and the vitriol oil before reaction, also can ensure that a large amount of reaction heat makes temperature of charge reach between the temperature 95 DEG C ~ 120 DEG C of thoroughly reaction.The vitriol oil and saprolite ore deposit add with the ratio of 0.8:1 ~ 1.2:1, react 1 minute to 12 minutes, and the unreacted iron of silicon-dioxide, minute quantity and non-ferrous metal form acidleach residue.
Second 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 the first step, loose cellular solid-state lotion is formed in temperature-fall period, add minimum but the water that metal sulfate all dissolves can be ensured and stir, metal sulfate is all dissolved, carry out solid-liquid separation and obtain normal pressure leaching slag A and normal pressure leaching liquid B, and washings E is washed to obtain to normal pressure leaching slag A.
3rd step is the process that normal pressure leaching immersion goes out limonite.Prepare limonite ore pulp with above-mentioned washings E, namely washings is recycled, to reduce the waste of Mineral resources; Normal pressure leaching liquid B and limonite ore pulp are added in capstan reactor, pressure leaching under middle pressure condition, the Fe in filtrate
3+be hydrolyzed to hematite precipitation and discharge acid (H+) to leach limonite; Adopt capstan reactor to compare autoclave and can realize continuous prodution, continuous output, it is high to produce integrated efficiency.Wherein the add-on of normal pressure leaching liquid and limonite ore pulp should according to making the final pH value of reaction mass be the ratio control of 0.5 ~ 1.5.It is rhombohedral iron ore and fast hydrolysis rate and higher nickel cobalt leaching yield and leaching velocity that temperature of reaction is high enough to the hydrolysate reaching iron ion, enough be low to moderate and make the operating pressure reached in the scope that pressurized reactor that is simple, low cost can bear under the prerequisite of the leaching yield obtaining higher nickel (and cobalt), be generally 150 DEG C ~ 240 DEG C, preferably 210 DEG C ~ 240 DEG C, extraction time is 0.5 hour ~ 1.5 hours.Lowered the temperature by pressure leaching material and carry out solid-liquid separation and obtain pressure leaching slag C and pressureleaching solution D, wherein the main component of pressure leaching slag C is rhombohedral iron ore, and iron level is very high, and pressureleaching solution D nickel concentration is higher and iron/nickel ratio is lower.
4th step comprises pressure leaching filtrate purifying, reclaims nickel, cobalt by sulfide or precipitation of hydroxide or other recovery method.
The invention has the beneficial effects as follows:
1, while realizing processing saprolite ore deposit and limonite in same technique, normal pressure acidleach and middle pressure is adopted to leach the technique that combines, overcome existing high pressure acid leaching process and need autoclave and relevant device, cause the defect of cost, maintenance cost costliness, and solve this acid leaching process acid amount and consume high and be only limitted to process the technical problem of limonite class raw material, there is the nickel higher than normal pressure leaching technique, the cobalt rate of recovery, easily effectively separation is carried out to leached mud and wait beneficial effect.
2, compared with high pressure Ore Leaching (HPAL) technique, pressure leaching of the present invention carries out under press strip part in 1.5MPa ~ 4.0Mpa, the mild condition of higher pressure acidleach, the cost of investment of corresponding pressure exerting device and much lower than high pressure acidleach of working cost, and simple to operate.Carry out under lower pressure (about 0.5MPa) condition although CN101001964A patent discloses pressure leaching, this technology is in order to obtain comparatively ideal nickel, cobalt leaching yield, and extraction time needs 1 ~ 2 hour, is 2 times of the present invention's time used.
3, compared with normal pressure acidleach, the normal pressure leaching time of the present invention is 1 ~ 12 minute, and normal pressure leaching time is 4 ~ 40 hours at present, and namely normal pressure pickling equipment investment of the present invention is obviously much smaller than existing normal pressure pickling equipment investment.
4, the most important thing is that sulfuric acid consumption of the present invention not only consumes far below the acid of normal pressure acidleach, and consume lower than the acid of high pressure acidleach.Under normal circumstances, use similar laterite, the acid consumption of normal pressure acidleach is that 600 ~ 900Kg sulfuric acid/1000Kg does ore deposit; The acid consumption of high pressure acidleach is that 300 ~ 600Kg sulfuric acid/1000Kg does ore deposit; Acid consumption of the present invention is that 180 ~ 350Kg sulfuric acid/1000Kg does ore deposit.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, therefore this proton (H+) is inabundant for leaching, and in causing excessive sulfuric acid must carry out when subsequent disposal 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 saprolite normal pressure leaching stage, then do not need separately to add sulfuric acid in limonite pressure leaching stage, but rely on Fe
3+be hydrolyzed to hematite precipitation and release proton (H+) leach limonite, avoiding problems because of hydrogen sulfate ion (HSO
4 -) and cause the defect that acid-utilising rate is low, and the consumption of follow-up neutralizing agent can be avoided.
5, nickel leaching yield of the present invention is not only far above normal pressure acidleach, and reaches or higher than high pressure acidleach.Generally, use similar laterite, the nickel leaching yield of normal pressure acidleach is 70 ~ 85%, and the nickel leaching yield of high pressure acidleach is 90 ~ 95%, and nickel leaching yield of the present invention is more than 95%, reason is that the leaching yield of nickeliferous high saprolite under constant-pressure and high-temperature condition is up to more than 98%.
6, high pressure acid leaching process laterite ore pulp and the vitriol oil is directly added autoclave leach, and in autoclave, regional area sulfuric acid concentration is very high, easily generates 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 a large amount of foulant can be avoided.
7, the common drawback of the high pressure acid leaching process of existing high pressure acidleach and improvement and the normal pressure acid leaching process of normal pressure acid leaching process and improvement leaches the quantity of slag greatly, and be the mixing slag of silicon and iron, can not cost-effectively develop.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, cause Solid state fermentation cost to increase.And leached mud very naturally can be separated into available white residue and scum easily by processing method of the present invention in technological process; Because under normal circumstances, limonite accounts for 70% of laterite total amount, and saprolite accounts for 30%, and in limonite, silicone content is about 0.5 ~ 5%, in saprolite, silicone content is about 15 ~ 25%, and that is in laterite, most silicon tax is stored in the less saprolite ore deposit of content.According to processing method of the present invention, in the normal pressure leaching stage, in saprolite, iron and non-ferrous metal and sulfuric acid reaction are produced vitriol and are entered solution, silicon then forms silicon-dioxide and becomes leaching residue, after solid-liquid separation, the normal pressure leaching quantity of slag only has saprolite ore deposit to measure 30 ~ 50%, account for 8 ~ 15% of laterite total amount, and in slag, the content of silicon-dioxide is even higher up to 80 ~ 85%; In the pressure leaching stage, the Fe in normal pressure leaching liquid
3+rhombohedral iron ore is all generated and a small amount of silicon becomes leaching residue with the iron in limonite, after solid-liquid separation, in pressure leaching slag, iron level is even higher up to 58 ~ 65%, namely a large amount of silicon is separated in normal pressure leaching slag, and a large amount of iron is separated in pressure leaching slag, avoid the two mutual " growth " together, be easy to effectively be separated with scum white residue, improve the utilization ratio of ore deposit energy resource.
8, in the present invention, saprolite ore deposit amount is the 1/4-1/3 of limonite amount, meets limonite amount in red soil nickel ore bed: the mine belt distribution of saprolite ore deposit amount >=2: 1.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
Embodiment
To be described further the present invention and effect thereof with embodiment below.
Illustrate: 1, use in following examples 1
#, 2
#with 3
#ore from laterite mineral deposit, New Caledonia, 4
#with 5
#from Indonesia's laterite mineral deposit, the main component of ore is in table 1.2, saprolite ore deposit is broken and be ground to-80 orders before for experiment.
Embodiment 1
Get 500Kg(butt) be ground to-80 objects 2
#saprolite ore deposit 500Kg water joins in steel lining alloy reaction tank and makes saprolite ore pulp, and after stirring, control speed adds the 500Kg vitriol oil that concentration is 98%, 10 minutes used times of reaction.
In time being cooled to below 60 DEG C, water logging tank is joined by after the reaction mass simple crushing of loose cellular solid-state lotion, add 1500Kg water, stir about is after 30 minutes, gained slip is added plate-and-frame filter press and carries out solid-liquid separation and residue washing, obtain normal pressure leaching slag A1 180Kg(do), normal pressure leaching liquid B1 1550L and washings E1 1200L.The composition of normal pressure leaching slag A1 normal pressure leaching liquid B1 washings E1 is in Table 1-1, table 1-2 and table 1-3.
Get 30Kg(to do) 1
#limonite, add washings E1 60L and be mixed with limonite slurry, move into after being heated to 95 DEG C in the circulation tank of capstan reactor, then in the circulation tank of capstan reactor, add normal pressure acidleach liquor B 1 30L of 95 DEG C, the final pH value recording reaction mass is 0.5.Open force (forcing) pump after sealing circulation tank, open the hot oil heater of capstan reactor, adjustment pressure is 1.5Mpa simultaneously, and control temperature heats, and continues thermostatically heating and within 50 minutes, stop afterwards heating and cooling when temperature is increased to 225 DEG C.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(do), pressureleaching solution D1 76L and washings F1 46L.Subsequently to pressureleaching solution D1 clarification, regulate material PH between 4.0 ~ 5.0, except the impurity such as de-iron, chromium reclaims nickel, cobalt by adding magnesium oxide.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.
Based on the component content of residue, calculate nickel, cobalt leaching yield, slag rate and acid consumption data as follows:
Normal pressure acidleach nickel leaching yield: 97.78%; Normal pressure acidleach cobalt leaching yield: 96.40%.
Pressure leaching nickel leaching yield: 94.95%; Pressure leaching cobalt leaching yield: 93.34%.
Amount to nickel leaching yield 96.21%; Cobalt leaching yield 93.66%.
Sulfuric acid consumption: 250Kg sulfuric acid/t ore deposit.
Amount to slag rate: 90.0g white residue/1000g laterite.
Embodiment 2
Get 500Kg(butt) be ground to-80 objects 2
#saprolite ore deposit 500Kg water joins in steel lining alloy reaction tank and makes saprolite ore pulp, and after stirring, control speed adds the 450Kg vitriol oil that concentration is 98%, 10 minutes used times of reaction.
In time being cooled to below 60 DEG C, joining water logging tank by after the reaction mass simple crushing of loose cellular solid-state lotion, add 1500Kg water, stir about 30 minutes.Water-soluble gained slurry is pumped into plate-and-frame filter press and carries out solid-liquid separation and residue washing, obtain normal pressure acidleach filter residue A2 220Kg(do), normal pressure acidleach liquor B 2 1530L and washings E2 1300L.The composition of normal pressure acidleach filter residue A2, normal pressure acidleach liquor B 2 and washings E2 is in Table 2-1, table 2-2 and table 2-3.
Get 40Kg(to do) 4
#limonite, add washings E2 80L and be mixed with limonite slurry, move into after being heated to 95 DEG C in the circulation tank of capstan reactor, then in the circulation tank of capstan reactor, add normal pressure acidleach liquor B 2 30L of 95 DEG C, the final pH value recording reaction mass is 1.5.Open force (forcing) pump after sealing circulation tank, open the hot oil heater of capstan reactor, adjustment pressure is 2.5Mpa simultaneously, and control temperature heats, and continues thermostatically heating and within 55 minutes, stop afterwards heating and cooling when temperature is increased to 230 DEG C.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(do), pressureleaching solution D2 94L and washings F2 55L.Subsequently to pressureleaching solution D1 clarification, regulate material PH between 4.0 ~ 5.0, except the impurity such as de-iron, chromium reclaims nickel, cobalt by adding magnesium oxide.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.
Based on the component content of residue, calculate nickel, cobalt leaching yield, slag rate and acid consumption data as follows:
Normal pressure acidleach nickel leaching yield: 98.77%; Normal pressure acidleach cobalt leaching yield: 94.00%.
Pressure leaching nickel leaching yield: 95.67%; Pressure leaching cobalt leaching yield: 92.11%.
Amount to nickel leaching yield 96.60%; Cobalt leaching yield 92.29%.
Sulfuric acid consumption: 180Kg sulfuric acid/t ore deposit.
Amount to slag rate: 88.0g white residue/1000g laterite.
Embodiment 3
The normal pressure acid leaching stage of the present embodiment is identical with embodiment 1, in the pressure leaching stage by 1
new noise made in coughing or vomiting limonite has changed 4 into
#indonesia's limonite.
Get 30Kg(to do) 4
#limonite, add washings E1 60L and be mixed with limonite slurry, move into after being heated to 95 DEG C in the circulation tank of capstan reactor, then in the circulation tank of capstan reactor, add normal pressure acidleach liquor B 1 30L of 95 DEG C, the final pH value recording reaction mass is 0.8.Open force (forcing) pump after sealing circulation tank, open the hot oil heater of capstan reactor, adjustment pressure is 2.0Mpa simultaneously, and control temperature heats, and continues thermostatically heating and within 60 minutes, stop afterwards heating and cooling when temperature is increased to 225 DEG C.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(do), pressureleaching solution D3 76L and washings F3 44L ml.Subsequently to pressureleaching solution D1 clarification, regulate material PH between 4.0 ~ 5.0, except the impurity such as de-iron, chromium reclaims nickel, cobalt by adding magnesium oxide.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.
Based on the component content of residue, calculate nickel, cobalt leaching yield, slag rate and acid consumption data as follows:
Pressure leaching nickel leaching yield: 95.56%; Pressure leaching cobalt leaching yield: 92.07%.
Amount to nickel leaching yield 96.29%; Cobalt leaching yield 92.43%.
Sulfuric acid consumption: 250Kg sulfuric acid/t ore deposit.
Amount to slag rate: 90.0g white residue/1000g laterite.
Embodiment 4
The normal pressure acid leaching stage of the present embodiment is identical with embodiment 2, in the pressure leaching stage by 4
indonesia's limonite has changed 1 into
#new noise made in coughing or vomiting limonite.
Get 40Kg(to do) 1
#limonite, add washings E2 80L and be mixed with limonite slurry, move into after being heated to 95 DEG C in the circulation tank of capstan reactor, then in the circulation tank of capstan reactor, add normal pressure acidleach liquor B 1 30L of 95 DEG C, the final pH value recording reaction mass is 1.3.Open force (forcing) pump after sealing circulation tank, open the hot oil heater of capstan reactor, adjustment pressure is 4.0Mpa simultaneously, and control temperature heats, and continues thermostatically heating and within 50 minutes, stop afterwards heating and cooling when temperature is increased to 240 DEG C.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(do), pressureleaching solution D4 94L and washings F4 55L.Subsequently to pressureleaching solution D1 clarification, regulate material PH between 4.0 ~ 5.0, except the impurity such as de-iron, chromium reclaims nickel, cobalt by adding magnesium oxide.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.
Based on the component content of residue, calculate nickel, cobalt leaching yield, slag rate and acid consumption data as follows:
Pressure leaching nickel leaching yield: 94.51%; Pressure leaching cobalt leaching yield: 92.48%.
Amount to nickel leaching yield 96.08%; Cobalt leaching yield 92.66%.
Sulfuric acid consumption: 180Kg sulfuric acid/t ore deposit.
Amount to slag rate: 88.0g white residue/1000g laterite.
Embodiment 5
The normal pressure acid leaching stage of the present embodiment is identical with embodiment 1, in the pressure leaching stage by 1
#new noise made in coughing or vomiting limonite has changed 3 into
#new Ka Guodukuang.
Get 30Kg(to do) 3
#transition ore deposit, add washings E1 60L and be mixed with transition ore deposit ore pulp, move into after being heated to 95 DEG C in the circulation tank of capstan reactor, then in the circulation tank of capstan reactor, add normal pressure acidleach liquor B 1 30L of 95 DEG C, the final pH value recording reaction mass is 0.9.Open force (forcing) pump after sealing circulation tank, open the hot oil heater of capstan reactor, adjustment pressure is 3.0Mpa simultaneously, and control temperature heats, and continues thermostatically heating and within 60 minutes, stop afterwards heating and cooling when temperature is increased to 225 DEG C.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(do), pressureleaching solution D5 76L and washings F3 47L.Subsequently to pressureleaching solution D1 clarification, regulate material PH between 4.0 ~ 5.0, except the impurity such as de-iron, chromium reclaims nickel, cobalt by adding magnesium oxide.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.
Based on the component content of residue, calculate nickel, cobalt leaching yield, slag rate and acid consumption data as follows:
Pressure leaching nickel leaching yield: 94.90%; Pressure leaching cobalt leaching yield: 93.38%.
Amount to nickel leaching yield 95.75%; Cobalt leaching yield 93.57%.
Sulfuric acid consumption: 250Kg sulfuric acid/t ore deposit.
Amount to slag rate: 90.0g white residue/1000g laterite.
In above embodiment, embodiment 1 and embodiment 2 saprolite in same mineral deposit and limonite combination; Embodiment 3 and embodiment 4 saprolite in different mineral deposit and limonite combination; As a comparison, embodiment 5 saprolite and the combination of transition ore deposit.From analytical data, the technical indicator such as nickel (cobalt) leaching yield, sulfuric acid consumption etc. of five embodiments is all better, but due to embodiment 5 employing is saprolite and the combination of transition ore deposit, therefore the iron level of pressure leaching slag is only 45.2%, and the iron level of the pressure leaching slag that other four embodiments obtain is all more than 58%.
Claims (9)
1. normal pressure acidleach and middle pressure leach a method for the process red soil nickel ore that combines, it is characterized in that: comprise the following steps:
A, making by being ground to-80 object saprolite ore deposits the ore pulp that solid content is 40%-60%, saprolite ore pulp and the vitriol oil being added in steel lining alloy reaction tank and reacting, to dissolve most solubility non-ferrous metal and soluble iron;
B, the reaction mass in above-mentioned a step and water to be dissolved with the mass ratio of 1:0.8 ~ 1:1.5, and solid-liquid separation obtains normal pressure leaching slag (A) and normal pressure leaching liquid (B);
C, limonite make the ore pulp that solid content is 40%-60%, the normal pressure leaching liquid (B) of above-mentioned b step gained and limonite ore pulp are added capstan reactor, at 150 DEG C ~ 240 DEG C, pressure leaching under 1.5MPa ~ 4.0MPa condition, after leaching 0.5 ~ 1.5h, carry out solid-liquid separation, obtain pressure leaching slag (C) and pressureleaching solution (D);
D, by pressureleaching solution (D) clarification of above-mentioned step c gained, reclaim nickel, cobalt by sulfide or precipitation of hydroxide.
2. a kind of normal pressure acidleach according to claim 1 and middle pressure leach the method for the process red soil nickel ore that combines, and it is characterized in that: wherein in step a, the vitriol oil and saprolite ore deposit are that the amount of 0.8:1 ~ 1.2:1 adds with mass ratio.
3. a kind of normal pressure acidleach according to claim 1 and middle pressure leach the method for the process red soil nickel ore that combines, and it is characterized in that: wherein step a reacts at ambient pressure, reaction times 1 ~ 12min.
4. a kind of normal pressure acidleach according to claim 1 and middle pressure leach the method for the process red soil nickel ore that combines, it is characterized in that: wash to obtain washings (E) to the normal pressure leaching slag (A) in step b and the pressure leaching slag (C) in step c, washings (E) is for the preparation of limonite ore pulp.
5. a kind of normal pressure acidleach according to claim 4 and middle pressure leach the method for the process red soil nickel ore that combines, and it is characterized in that: the add-on wherein controlling normal pressure leaching liquid (B) and limonite ore pulp in step c makes the final pH value of reaction mass between 0.5 ~ 1.5.
6. leach the method for the process red soil nickel ore that combines according to the arbitrary described a kind of normal pressure acidleach of claim 1-5 and middle pressure, it is characterized in that: the temperature of reaction wherein in rate-determining steps a is between 95 DEG C ~ 120 DEG C.
7. leach the method for the process red soil nickel ore that combines according to the arbitrary described a kind of normal pressure acidleach of claim 1-5 and middle pressure, it is characterized in that: wherein in step b, in normal pressure leaching slag (A), dioxide-containing silica is 65% ~ 90%.
8. leach the method for the process red soil nickel ore that combines according to the arbitrary described a kind of normal pressure acidleach of claim 1-5 and middle pressure, it is characterized in that: wherein obtaining iron level in pressure leaching slag (C) in step c is 58% ~ 65%.
9. leach the method for the process red soil nickel ore that combines according to the arbitrary described a kind of normal pressure acidleach of claim 1-5 and middle pressure, it is characterized in that: wherein in step c, temperature is preferably 210 DEG C ~ 240 DEG C.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109837386A (en) * | 2019-03-13 | 2019-06-04 | 荆门市格林美新材料有限公司 | A kind of leaching method of lateritic nickel ore |
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| CN101133171A (en) * | 2005-02-14 | 2008-02-27 | Bhp比利通Ssm技术有限公司 | Process for enhanced acid leaching of laterite ores |
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| CN103614571A (en) * | 2013-10-09 | 2014-03-05 | 北京矿冶研究总院 | Combined leaching process of laterite-nickel ore |
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| CN101001964A (en) * | 2004-08-02 | 2007-07-18 | 斯凯资源有限公司 | Method for nickel and cobalt recovery from laterite ores by combination of atmospheric and moderate pressure leaching |
| CN101133171A (en) * | 2005-02-14 | 2008-02-27 | Bhp比利通Ssm技术有限公司 | Process for enhanced acid leaching of laterite ores |
| CN101768665A (en) * | 2008-12-30 | 2010-07-07 | 厦门紫金矿冶技术有限公司 | Method for reducing acid consumption during heap leaching and high-pressure leaching of nickel laterite ore |
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| CN109837386A (en) * | 2019-03-13 | 2019-06-04 | 荆门市格林美新材料有限公司 | A kind of leaching method of lateritic nickel ore |
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Inventor after: Yu Yanfen Inventor after: Wang Xiaochan Inventor after: Yao Fei Inventor after: Wang Yuanpu Inventor after: Tian Zhongyuan Inventor after: Wang Shaohua Inventor after: Sun Zhizhong Inventor after: Liu Yuqiang Inventor after: Zhang Shufeng Inventor after: Liu Ke Inventor after: Liu Zhaoxia Inventor after: Du Hao Inventor after: Sha Bin Inventor after: Liu Shihe Inventor before: Yu Yanfen Inventor before: Wang Shaohua Inventor before: Sun Zhizhong Inventor before: Liu Yuqiang Inventor before: Liu Zhaoxia Inventor before: Du Hao Inventor before: Sha Bin Inventor before: Wang Xiaochan Inventor before: Yao Fei Inventor before: Zhu Hui |
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Application publication date: 20150729 |