CN104789797A - A novel method of recovering nickel, cobalt, iron, silicon and magnesium from low-grade lateritic nickel ore - Google Patents
A novel method of recovering nickel, cobalt, iron, silicon and magnesium from low-grade lateritic nickel ore Download PDFInfo
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Abstract
A novel method of recovering nickel, cobalt, iron, silicon and magnesium from low-grade lateritic nickel ore is provided. The method includes preforming ore dressing by washing and grading to obtain coarse high-silicon high-magnesium ore and finer low-silicon low-magnesium high-iron ore; adding sufficient concentrated sulfuric acid into high-silicon high-magnesium ore pulp and reacting; performing solid liquid separation to obtain atmospheric-pressure leaching slag and atmospheric-pressure leachate; adding the atmospheric-pressure leachate and low-silicon low-magnesium high-iron ore pulp into a tubular reactor according to a ratio and performing pressure leaching; performing solid liquid separation; purifying and precipitating leachate of pressure leaching with magnesium oxide and filtering to obtain nickel (cobalt) hydroxide; evaporating the liquid after nickel precipitation and crystallizing to obtain magnesium sulfate heptahydrate; and washing pressure leaching slag and drying to obtain a fine iron powder product. The method is high in applicable range for lateritic nickel ore, high in nickel and cobalt leaching rates, small in atmospheric-pressure devices, short in time, high in efficiency, and low in sulfuric acid consumption. The pressure leaching adopts the middle- and low- pressure tubular reactor, and avoids the defect that autoclaves are expensive and liable to scale. The iron and the magnesium which are main components of the ore and a part of silicon can be economically and effectively recovered. Waste slag is low in amount and can be effectively utilized.
Description
Technical field
The invention belongs to field of metallurgy, is wet-leaching technique, relates to a kind of novel method reclaiming nickel, cobalt, iron, silicon and magnesium from low-grade laterite nickel ore.
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.
Under normal circumstances, 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 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 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.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 reduction 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
2o
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
2o
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.
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.
Summary of the invention
The object of the invention is the shortcoming eliminating or alleviate 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 high pressure acidleach.A kind of method of high efficiente callback nickel (cobalt), iron, silicon and magnesium from low-grade laterite nickel ore is provided.
Technical scheme: a kind of novel method reclaiming nickel, cobalt, iron, silicon and magnesium from low-grade laterite nickel ore, comprises the following steps: (a) obtains the thicker high silicon magnesium ore deposit of particle diameter and the thinner low silicon magnesium height iron ore of particle diameter to low-grade laterite nickel ore washing classification; B high silicon magnesium ore deposit adds water slurrying by (), high silicon magnesium ore pulp is heated to 60 DEG C ~ 100 DEG C, 98% vitriol oil is heated to 150 DEG C ~ 200 DEG C, the high silicon magnesium ore pulp of heating and 98% vitriol oil synchronously add duplex pusher reactor makes it reaction, to dissolve solubility non-ferrous metal and the soluble iron of the overwhelming majority; To adding water after the loose cellular object simple crushing generated and stirring pulping c () reacted material shifts out duplex pusher reactor after, then institute's pulping is carried out press filtration and obtain filter residue, normal pressure acidleach filtrate (B), washing filter residue obtains normal pressure acidleach filter residue (A) and washings (E); D () adds washings (E) slurrying to low silicon magnesium height iron ore, obtained low silicon magnesium high ferro ore pulp and normal pressure acidleach filtrate (B) are added in pipeline reactor, pressurization, heating is started after sealing, temperature 195 DEG C ~ 230 DEG C, pressure not higher than pressure leaching under 3.0Mpa condition, the Fe in normal pressure acidleach filtrate
3+be hydrolyzed to hematite precipitation and discharge Ore Leaching low silicon magnesium height iron ore; E () reduces pressure, temperature, taken out by reactant in pipeline reactor and carry out solid-liquid separation, obtain pressure leaching slag (C) and pressureleaching solution (D); F () pressureleaching solution (D) magnesium oxide removes non-nickel, cobalt impurity, precipitation, filtration, reclaim nickel, cobalt; G magnesium sulfate heptahydrate that the filtrate evaporative crystallization of () f arrives; H () gained pressure leaching slag (C) adds stirring in soda ash solution, then filters, dry namely obtain Iron concentrate to gained filter cake; (i) normal pressure acidleach filter residue (A) obtains higher-grade silica product and building sand through screening process.
After described step (a) ore grinding, high silicon magnesium ore deposit is+80 orders, and low silicon magnesium height iron ore is-80 orders.
Described step (b) high silicon magnesium ore deposit add water slurrying time ore deposit, quality than for 1:0.9 ~ 1:1.1, slurry is 1:0.45 ~ 1:0.5 with the mass ratio of 98% vitriol oil.
The reacted material of described step (c) and the mass ratio added water are 1:0.9 ~ 1:1.1.
Material reaction temperature in described step (b) duplex pusher reactor is 160 DEG C ~ 280 DEG C, and the reaction times is 1 minute to 12 minutes, preferably 5 minutes to 10 minutes.
In described step (c), the dioxide-containing silica of normal pressure acidleach filter residue (A) is 65% ~ 90%.
The iron level obtaining pressure leaching slag (C) in described step (e) is 58% ~ 65%.
The additional proportion of normal pressure acidleach filtrate (B) and low silicon magnesium high ferro ore pulp reaches 0.5 ~ 1.5 and determine by final ph after material reaction in described step (d).
Described step (d) adds in pipeline reactor after first normal pressure acidleach filtrate (B) being heated to 90 DEG C ~ 95 DEG C again.
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 ore pulp produces makes temperature of charge raise to impel the metal (nickel, cobalt, iron, magnesium, chromium, aluminium etc.) in high silicon magnesium ore deposit and sulfuric acid rapid reaction to generate metal sulfate, and a large amount of reaction heat makes temperature of charge be increased to 160 DEG C ~ 280 DEG C further to ensure to react and carry out fully and completely simultaneously.Silicon-dioxide and the unreacted iron of minute quantity and non-ferrous metal are formed and leach residue.The add-on of acid is 0.8 ~ 1.2 times that stoichiometry dissolves iron in ore and the required acid amount of non-ferrous metal.Reaction times is 1 minute to 12 minutes.
In pipeline reactor, the Fe in normal pressure acidleach filtrate
3+be hydrolyzed to hematite precipitation and discharge acid and leach low silicon magnesium height iron ore again.Wherein normal pressure leaching liquid and low silicon magnesium height iron ore slurry add-on according to make reaction mass final ph be 0.5 ~ 1.5 ratio control.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, and be enough 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 195 DEG C ~ 230 DEG C, preferably 210 DEG C ~ 230 DEG C.Extraction time is 0.5 hour ~ 1.0 hours.Pressure leaching material is lowered the temperature and carries out solid-liquid separation to obtaining pressure leaching slag (C) and pressureleaching solution (D), 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.
Compared with prior art, the invention has the advantages that:
1, achieve a kind of technique can process whole laterite simultaneously, overcome the deficiency that traditional employing thermal process and wet processing process respectively to laterite.Particularly in technological process, very naturally easily the main component ironworking of laterite is become Iron concentrate, part silicon is recovered as higher-grade silica product, make waste residue amount be reduced to about 5 percent of raw ore amount;
2, compared with high pressure Ore Leaching (HPAL) technique, pressure leaching of the present invention carries out under 1.5MPa ~ 3.0MPa, than mild condition many of high pressure acidleach 4.5MPa ~ 5.0MPa, the cost of investment of corresponding pressure exerting device and much lower than the autoclave of high pressure acidleach of working cost, and operation and maintenance is also simpler;
3, compared with normal pressure acidleach, the normal pressure leaching time of the present invention is 1 minute to 12 minutes, and normal pressure leaching time is generally 240 minutes to 2400 minutes, corresponding normal pressure pickling equipment investment of the present invention is apparent much smaller than existing normal pressure pickling equipment investment;
4, sulfuric acid consumption of the present invention not only consumes far below the acid of normal pressure acidleach, and consumes lower than the acid of high pressure acidleach.Under normal circumstances, use similar laterite and saprolite/limonite ratio, 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 250 ~ 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.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; And in method of the present invention, although need to consume more sulfuric acid in the normal pressure leaching stage, then do not need separately to add sulfuric acid in the pressure leaching stage, but rely on Fe
3+the proton (acid) being hydrolyzed to hematite precipitation release leaches limonite, 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;
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%; 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 high silicon magnesium ore deposit 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, is easy to produce 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 substantially can be avoided;
7, existing high pressure acidleach comprises the 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 is that to leach the quantity of slag large, and is the mixing slag of silicon and iron, can not cost-effectively develop.And the main component iron of laterite, magnesium and part silicon very naturally can be able to cost-effective recycling easily by method of the present invention in technological process.Under normal circumstances, limonite accounts for about 70% of laterite total amount, and saprolite accounts for 30%; In limonite, silicone content is about 0.5 ~ 5%, and in saprolite, silicone content is about 15 ~ 25%, and that is in laterite, most silicon tax is stored in a small amount of saprolite ore deposit.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 normal pressure leaching quantity of slag only has high silicon magnesium ore deposit to measure after solid-liquid separation 30 ~ 50%, account for 8 ~ 15% of laterite total amount, in slag, dioxide-containing silica reaches 80 ~ 85% even higher; 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 even higher up to 58 ~ 65%, and namely simple process can be used as Iron concentrate and sell.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 low-grade laterite nickel ore be mixed into by limonite and transition ore deposit.Method of the present invention is particularly suitable for processing low-grade laterite nickel ore.
Accompanying drawing explanation
Fig. 1 is schema of the present invention.
Embodiment
By the following examples present method is illustrated.Use in these embodiments 1
#ore is from laterite mineral deposit, New Caledonia, and washing classification obtains 2
#with 3
#ore; 4
#ore is from Indonesia's laterite mineral deposit, and washing classification obtains 5
#with 6
#ore.The main component of ore is in table 1.Ore is broken and grind before for experiment, and thicker is+80 orders, and comparatively fine fraction is-80 orders.
Under normal circumstances, people's subjectivity laterite mineral deposit from upper (upper strata) under (lower floor) be divided into three layers, i.e. limonite ore bed, transition ore deposit ore bed and saprolite (vegetable mould) ore bed.Limonite particle is trickle, nickeliferous lower, and silicon, Mg content are also low, but iron content is high; The nickeliferous height in saprolite ore deposit, silicon, Mg content are also high, but iron content is low, and transition ore deposit is between therebetween.Therefore " low-grade laterite " of the present invention refers to the laterite not having saprolite ore deposit, namely containing one or both laterite of limonite or transition ore deposit.
Embodiment 1
Get 500Kg(butt) be ground to 80 objects 2
#high silicon magnesium ore deposit adds 500Kg water and makes high silicon magnesium ore pulp, prepares the 500Kg vitriol oil (98%).Add water high silicon magnesium ore deposit slurrying, high silicon magnesium ore pulp is heated to 60 DEG C ~ 100 DEG C, 98% vitriol oil is heated to 150 DEG C ~ 200 DEG C, strictly control with mortar pump and the vitriol oil pump opening for feed that high silicon magnesium ore pulp and the vitriol oil synchronously to add duplex pusher reactor by flow, ore pulp and the vitriol oil are pushed out duplex pusher reactor be forced into the rapid reaction of duplex pusher reactor after short mix after.10 minutes total overall reaction used times.
Through cooling, leaching tank of being fallen back by the reaction mass simple crushing of loose cellular solid-state lotion, adds 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 (A1) 205Kg(do), normal pressure acidleach filtrate (B1) 1450L and washings (E1) 1150L.The composition of normal pressure acidleach filter residue (A1), normal pressure acidleach filtrate (B1) and washings (E1) is in Table 1-1, table 1-2 and table 1-3.
Get 30Kg(to do) 3
#low silicon magnesium ore deposit, add washings (E1) 60L and be mixed with low silicon magnesium high ferro ore pulp, move into after being heated to 95 DEG C in the circulation tank of capstan reactor, then add normal pressure acidleach filtrate (B1) 30L of 95 DEG C in the circulation tank of capstan reactor.Open force (forcing) pump after sealing circulation tank, pressure, not higher than 3.0Mpa, opens the hot oil heater of capstan reactor 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.After material reaction, final ph is about 1.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.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.Pressureleaching solution (D1) magnesium oxide removes non-nickel, cobalt impurity, precipitation, filtration, recycling precipitate nickel, cobalt, the magnesium sulfate heptahydrate that filtrate evaporative crystallization arrives; Gained pressure leaching slag (C1) adds stirring in soda ash solution, then filters, and dries namely obtain Iron concentrate to gained filter cake; Normal pressure acidleach filter residue (A1) obtains higher-grade silica product and building sand through screening process.
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: 98.5%; Normal pressure acidleach cobalt leaching yield: 96.5%;
Pressure leaching nickel leaching yield: 95.6%; Pressure leaching cobalt leaching yield: 92.4%;
Amount to nickel leaching yield 96.8%; Cobalt leaching yield 93.5%;
Iron recovery >96%;
Sulfuric acid consumption: 200Kg sulfuric acid/t ore deposit;
Amount to slag rate: 41g white residue/1000g laterite.
Embodiment 2
Get 500Kg(butt) be ground to 80 objects 2
#high silicon magnesium ore deposit adds 500Kg water and makes high silicon magnesium ore pulp, prepares the 500Kg vitriol oil (98%).Add water high silicon magnesium ore deposit slurrying, high silicon magnesium ore pulp is heated to 60 DEG C ~ 100 DEG C, 98% vitriol oil is heated to 150 DEG C ~ 200 DEG C, strictly control with mortar pump and the vitriol oil pump opening for feed that high silicon magnesium ore pulp and the vitriol oil synchronously to add duplex pusher reactor by flow, ore pulp and the vitriol oil are pushed out duplex pusher reactor be forced into the rapid reaction of duplex pusher reactor after short mix after.10 minutes total overall reaction used times.
Through cooling, leaching tank of being fallen back by the reaction mass simple crushing of loose cellular solid-state lotion, adds 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) 230Kg(do), normal pressure acidleach filtrate (B2) 1400L and washings (E2) 1180L.The composition of normal pressure acidleach filter residue (A2), normal pressure acidleach filtrate (B2) and washings (E2) is in Table 2-1, table 2-2 and table 2-3.
Get 40Kg(to do) 6
#low silicon magnesium ore deposit, add washings (E2) 80L and be mixed with low silicon magnesium high ferro ore pulp, move into after being heated to 95 DEG C in the circulation tank of capstan reactor, then add normal pressure acidleach filtrate (B2) 30L of 95 DEG C in the circulation tank of capstan reactor.Open force (forcing) pump after sealing circulation tank, pressure, not higher than 3.0Mpa, opens the hot oil heater of capstan reactor 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.After material reaction, final ph is about 1.5.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.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.Pressureleaching solution (D2) magnesium oxide removes non-nickel, cobalt impurity, precipitation, filtration, recycling precipitate nickel, cobalt, the magnesium sulfate heptahydrate that filtrate evaporative crystallization arrives; Gained pressure leaching slag (C2) adds stirring in soda ash solution, then filters, and dries namely obtain Iron concentrate to gained filter cake; Normal pressure acidleach filter residue (A2) obtains higher-grade silica product and building sand through screening process.
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: 97.6%; Normal pressure acidleach cobalt leaching yield: 95.4%;
Pressure leaching nickel leaching yield: 94.7%; Pressure leaching cobalt leaching yield: 93.6%;
Amount to nickel leaching yield 95.9%; Cobalt leaching yield 93.4%;
Iron recovery >96%;
Sulfuric acid consumption: 200Kg sulfuric acid/t ore deposit;
Amount to slag rate: 92.0g 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 3
@new noise made in coughing or vomiting low silicon magnesium ore deposit has changed 6 into
#indonesia's low silicon magnesium ore deposit.
Get 30Kg(to do) 6
#low silicon magnesium ore deposit, add washings (E1) 60L and be mixed with low silicon magnesium ore pulp, move into after being heated to 95 DEG C in the circulation tank of capstan reactor, then add normal pressure acidleach filtrate (B1) 30L of 95 DEG C in the circulation tank of capstan reactor.Open force (forcing) pump after sealing circulation tank, pressure, not higher than 3.0Mpa, opens the hot oil heater of capstan reactor 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.After material reaction, final ph is 1.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.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.Pressureleaching solution (D3) magnesium oxide removes non-nickel, cobalt impurity, precipitation, filtration, recycling precipitate nickel, cobalt, the magnesium sulfate heptahydrate that filtrate evaporative crystallization arrives; Gained pressure leaching slag (C3) adds stirring in soda ash solution, then filters, and dries namely obtain Iron concentrate to gained filter cake.
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: 95.1%; Pressure leaching cobalt leaching yield: 95.7%;
Amount to nickel leaching yield 96.3%; Cobalt leaching yield 96.2%;
Iron recovery >96%;
Sulfuric acid consumption: 200Kg sulfuric acid/t ore deposit;
Amount to slag rate: 82.0g 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 6
@indonesia's low silicon magnesium ore deposit has changed 3 into
#new noise made in coughing or vomiting low silicon magnesium ore deposit.
Get 40Kg(to do) 3
#low silicon magnesium ore deposit, add washings (E2) 80L and be mixed with low silicon magnesium ore deposit ore pulp, move into after being heated to 95 DEG C in the circulation tank of capstan reactor, then add normal pressure acidleach filtrate (B2) 30L of 95 DEG C in the circulation tank of capstan reactor.Open force (forcing) pump after sealing circulation tank, pressure, not higher than 3.0Mpa, opens the hot oil heater of capstan reactor 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.After material reaction, final ph is 0.7.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.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.Pressureleaching solution (D4) magnesium oxide removes non-nickel, cobalt impurity, precipitation, filtration, recycling precipitate nickel, cobalt, the magnesium sulfate heptahydrate that filtrate evaporative crystallization arrives; Gained pressure leaching slag (C4) adds stirring in soda ash solution, then filters, and dries namely obtain Iron concentrate to gained filter cake.
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: 94.9%; Pressure leaching cobalt leaching yield: 92.7%;
Amount to nickel leaching yield 95.4%; Cobalt leaching yield 93.1%;
Iron recovery >96%;
Sulfuric acid consumption: 200Kg sulfuric acid/t ore deposit;
Amount to slag rate: 92.0g 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 3
@new noise made in coughing or vomiting low silicon magnesium ore deposit has changed 4 into
#indonesia's laterite.
Get 30Kg(to do) 4
#indonesia's laterite, 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 add normal pressure acidleach filtrate (B1) 30L of 95 DEG C in the circulation tank of capstan reactor.Open force (forcing) pump after sealing circulation tank, open the hot oil heater of capstan reactor simultaneously, control temperature heats, and continues thermostatically heating and within 60 minutes, stop afterwards heating and cooling when temperature is increased to 225 DEG C.After material reaction, final ph is about 1.2.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 (F5) 47L.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.Pressureleaching solution (D5) magnesium oxide removes non-nickel, cobalt impurity, precipitation, filtration, recycling precipitate nickel, cobalt, the magnesium sulfate heptahydrate that filtrate evaporative crystallization arrives; Gained pressure leaching slag (C5) adds stirring in soda ash solution, then filters, and dries namely obtain Iron concentrate to gained filter cake; Normal pressure acidleach filter residue (A1) obtains higher-grade silica product and building sand through screening process.
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: 94.9%; Pressure leaching cobalt leaching yield: 92.8%;
Amount to nickel leaching yield 95.5%; Cobalt leaching yield 93.3%;
Iron recovery >96%;
Sulfuric acid consumption: 200Kg sulfuric acid/t ore deposit;
Amount to slag rate: 82.0g white residue/1000g laterite.
In above embodiment, embodiment 1 and the embodiment 2 high silicon magnesium ore deposit in same mineral deposit and the combination of low silicon magnesium ore deposit; Embodiment 3 and the embodiment 4 high silicon magnesium ore deposit in different mineral deposit and the combination of low silicon magnesium ore deposit; As a comparison, embodiment 5 high silicon magnesium ore deposit and composite ore combination.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 53.87%, 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 62%, the rhombohedral iron ore iron level of recovery is all about 63%, and iron recovery is more than 96%.Amount to slag rate about 90.0g white residue/1000g laterite, about slag rate is down to 45g white residue/1000g laterite after reclaiming silicon-dioxide.
Claims (10)
1. from low-grade laterite nickel ore, reclaim a novel method for nickel, cobalt, iron, silicon and magnesium, comprise the following steps: (a) obtains the thicker high silicon magnesium ore deposit of particle diameter and the thinner low silicon magnesium height iron ore of particle diameter to low-grade laterite nickel ore washing classification; B high silicon magnesium ore deposit adds water slurrying by (), high silicon magnesium ore pulp is heated to 60 DEG C ~ 100 DEG C, 98% vitriol oil is heated to 150 DEG C ~ 200 DEG C, the high silicon magnesium ore pulp of heating and 98% vitriol oil synchronously add duplex pusher reactor makes it reaction; To adding water after the loose cellular object simple crushing generated and stirring pulping c () reacted material shifts out duplex pusher reactor after, then institute's pulping is carried out press filtration and obtain filter residue, normal pressure acidleach filtrate (B), washing filter residue obtains normal pressure acidleach filter residue (A) and washings (E); D () adds washings (E) slurrying to low silicon magnesium height iron ore, obtained low silicon magnesium high ferro ore pulp and normal pressure acidleach filtrate (B) are added in pipeline reactor, start pressurization, heating after sealing, temperature 195 DEG C ~ 230 DEG C, pressure is not higher than pressure leaching under 3.0Mpa condition; E () reduces pressure, temperature, taken out by reactant in pipeline reactor and carry out solid-liquid separation, obtain pressure leaching slag (C) and pressureleaching solution (D); F () pressureleaching solution (D) magnesium oxide removes non-nickel, cobalt impurity, precipitation, filtration, reclaim nickel, cobalt; G magnesium sulfate heptahydrate that the filtrate evaporative crystallization of () f arrives; H () gained pressure leaching slag (C) adds stirring in soda ash solution, then filters, dry namely obtain Iron concentrate to gained filter cake; (i) normal pressure acidleach filter residue (A) obtains higher-grade silica product and building sand through screening process.
2. the novel method reclaiming nickel, cobalt, iron, silicon and magnesium from low-grade laterite nickel ore according to claim 1, is characterized in that, after step (a) ore grinding, high silicon magnesium ore deposit is+80 orders, and low silicon magnesium height iron ore is-80 orders.
3. the novel method reclaiming nickel, cobalt, iron, silicon and magnesium from low-grade laterite nickel ore according to claim 1, it is characterized in that, step (b) high silicon magnesium ore deposit add water slurrying time ore deposit, quality than for 1:0.9 ~ 1:1.1, slurry is 1:0.45 ~ 1:0.5 with the mass ratio of 98% vitriol oil.
4. the novel method reclaiming nickel, cobalt, iron, silicon and magnesium from low-grade laterite nickel ore according to claim 1, is characterized in that, the reacted material of step (c) and the mass ratio added water are 1:0.9 ~ 1:1.1.
5. the novel method reclaiming nickel, cobalt, iron, silicon and magnesium from low-grade laterite nickel ore according to claim 1, it is characterized in that, material reaction temperature in step (b) duplex pusher reactor is 160 DEG C ~ 280 DEG C, and the reaction times is 1 minute to 12 minutes.
6. the novel method reclaiming nickel, cobalt, iron, silicon and magnesium from low-grade laterite nickel ore according to claim 5, is characterized in that, step (b) reaction times is 5 minutes to 10 minutes.
7. the novel method reclaiming nickel, cobalt, iron, silicon and magnesium from low-grade laterite nickel ore according to claim 1, is characterized in that, wherein in step (c), the dioxide-containing silica of normal pressure acidleach filter residue (A) is 65% ~ 90%.
8. the novel method reclaiming nickel, cobalt, iron, silicon and magnesium from low-grade laterite nickel ore according to claim 1, is characterized in that, the iron level wherein obtaining pressure leaching slag (C) in step (e) is 58% ~ 65%.
9. the novel method reclaiming nickel, cobalt, iron, silicon and magnesium from low-grade laterite nickel ore according to claim 1, it is characterized in that, the additional proportion of normal pressure acidleach filtrate (B) and low silicon magnesium high ferro ore pulp reaches 0.5 ~ 1.5 and determine by final ph after material reaction in step (d).
10. the novel method reclaiming nickel, cobalt, iron, silicon and magnesium from low-grade laterite nickel ore according to claim 1, it is characterized in that, step (d) adds in pipeline reactor after first normal pressure acidleach filtrate (B) being heated to 90 DEG C ~ 95 DEG C again.
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