CN104611558B - A kind of method reclaiming nickel, cobalt, ferrum and silicon by combined leaching process from lateritic nickel ore - Google Patents
A kind of method reclaiming nickel, cobalt, ferrum and silicon by combined leaching process from lateritic nickel ore Download PDFInfo
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Abstract
The invention discloses a kind of method reclaiming nickel, cobalt, ferrum and silicon by combined leaching process from lateritic nickel ore, add the saprolife ore pulp after heating and concentrated sulphuric acid in Double helix pusher reactor, reaction mass is carried out with water-soluble rear solid-liquid separation and residue washing obtains normal pressure leaching slag, normal pressure leaching liquid and cleaning mixture；Make limonite slurry with cleaning mixture and limonite, limonite slurry and normal pressure leaching liquid are heated addition capstan reactor pressure leaching, the Fe in normal pressure leaching liquid respectively3+Hydrolysis discharges acid and leaches limonite again；Reduce temperature and carry out solid-liquid separation, obtain pressure leaching slag and pressureleaching solution；Pressureleaching solution is gone unless passed through have method to reclaim nickel and/or cobalt after nickel cobalt impurity；With soda ash solution, post-drying is washed to pressure leaching slag and obtains Iron concentrate；To normal pressure leaching slag, screened process obtains silicon dioxide and building sand.It is little that extraction time of the present invention is short, nickel leaches high, sour consumption, ferrum and part silicon energy efficient recovery.
Description
Technical field
The present invention relates to the hydrometallurgical processes technical field of lateritic nickel ore is and in particular to a kind of pass through combined leaching process
Nickel, the method for cobalt, ferrum and silicon is reclaimed from lateritic nickel ore.
Background technology
Laterite is to be gone bad through long-term weathering leaching on a large scale in the torrid zone or subtropical zone by nickeliferous peridotite to form
Nickel ore, due to there is the difference of geographical position, weather conditions and rate of decay, laterite type all over the world is not
Identical.Efflorescence typically produces bedded deposit, wherein near surface exist completely or the most thoroughly air slaking produce
Thing, fades to the sedentary product of lesser extent with depth increase, and finally terminates as non-air slaking in certain deeper depth
Rock.Most of nickel that height weathered layer is generally contained is trickle to be distributed in goethitum granule in small, broken bits.This layer is usual
Referred to as limonite, it typically contains silicon and the magnesium of a high proportion of ferrum and low ratio.Nickel contained by the lighter layer of air slaking is typically more
Be contained in various magnesium silicate minerals, such as serpentine.Not exclusively may there are a lot of other silicic acid containing nickel in weathered zone
Salt mineral.The height of part air slaking contains magnesium ribbon and is commonly referred to saprolife or garnierite.It typically contains ferrum and the Gao Bi of low ratio
The silicon of example and magnesium.Also have another kind to be generally in the nontronite that mainly contains between limonite and saprolife in some mineral deposits to glue
The band of soil, referred to as transition ore deposit." low-grade laterite " refers to the laterite not having saprolife ore deposit, that is, by limonite and transition
The laterite of ore deposit composition.Under normal circumstances, limonite is the key component of lateritic nickel ore, accounts for the 65%- of laterite total amount
75%；Saprolife accounts for 15%-25%；Transition ore deposit accounts for 10%.Reclaim nickel from lateritic nickel ore, the where the shoe pinches of cobalt are, changed
Learn to process and separate metal value（As nickel and cobalt）The useful component of the abundant enriching nickel of physics mode generally can not be passed through before,
Cannot be enriched with the technology of ore dressing, this make lateritic nickel ore processing cost very high.And due to limonite and sapropel
Different mineral and chemical composition in native ore deposit, these Ores are normally unsuitable for being processed using same treatment technology.Decades
To always search for reducing the method for the cost processing lateritic nickel ore.
The handling process of lateritic nickel ore is commonly divided into thermal process and wet processing two big class at present.Fire metallurgy process
It is suitable for processing saprolife ore deposit.This technique is typically only capable to produce ferronickel it is impossible to Call Provision, and its application is restricted.Hydrometallurgy work
Skill is suitable for processing limonite.Hydrometallurgical technology include high pressure acidleach and reduction roasting _ ammonia leaching and occur in recent years as usual
Pressure acidleach, dump leaching process etc..Heap Leaching leaching rate is relatively low, is only applicable to process the laterite of high content of magnesium；Reduction roasting-ammonia
Soaking technology is higher due to energy consumption, technological process length and less be used；Normal pressure acidleach technical operation is simple, does not require the use of costliness
Autoclave, but mineral to be made be completely dissolved then required acid consumption larger, and in leachate contain each metal ion species, make subsequently to soak
Changing separation circuit becomes complicated.High pressure acidleach（HPAL) technique uses sulphuric acid in high temperature（250℃）And high pressure（50MPa）Lower leaching
Go out lateritic nickel ore.Under high temperature, condition of high voltage, the metalliferous mineral in Ore is almost completely dissolved.The ferrum of dissolving is being adopted
It is hydrolyzed to rapidly bloodstone under high temperature（Fe203) precipitation, nickel, cobalt etc. stay in the solution, after cooling the leaching of iron content and silicon
Residue passes through in a series of washing concentrating, i.e. so-called counter-current decantation washing（CCD) in loop concentrate and from nickeliferous, cobalt solution
Middle separation.Therefore reach the main purpose of extract technology -- nickel is separated with ferrum.
High pressure Ore Leaching（HPAL) advantage of technique is：Nickel, cobalt leaching rate are high；Response speed is fast, the response time is short；Ferrum exists
Do not consume sulphuric acid during acidleach in theory and hydrolyzate is bloodstone（Fe203) precipitation.But high pressure Ore Leaching（HPAL) work
The shortcoming of skill is also very prominent：It is the equipment that it needs complicated high temperature, the autoclave of high pressure and correlation first, it is installed and dimension
Shield is all costly；Two is high pressure acidleach（HPAL）The sulphuric acid of technique consumption becomes than the nonferrous metal stoichiometrically dissolving in Ore
Sulphuric acid needed for point is more.Because most sulfate ion connections being provided by sulphuric acid form hydrogen sulfate under the conditions of high pressure acidleach
Radical ion（HSO4 -）.That is sulphuric acid only dissociates under the conditions of high pressure acidleach and discharges a proton（H+).Cold in leachate
But and neutralization when, hydrogen sulfate ion resolves into sulfate radical（SO4 2-）With another proton.A therefore rear proton (acid）No
It is sufficiently used for leaching, and lead to excessive sulphuric acid to be to have to be neutralized and consume nertralizer in subsequent treatment；Three is HPAL
Technique is only limited to process the raw material being mainly limonite class, because the presence of saprolife can lead to a large amount of increasings of sulfuric acid consumption
Plus.This is because the content of magnesium of magnesium in saprolife is higher caused；Four is that HPAL technique is easy in running mesohigh kettle
Fouling, need to periodically stop production cleaning, and the utilization of capacity is low；Five is to leach that the quantity of slag is big, and is the mixing slag of silicon and ferrum it is impossible to economical and effective
Exploitation.
United States Patent (USP) No. 4,097,575 describe the improvement to HPAL technique, brown including occurring in described autoclave
The high pressure of iron mine leaches, and it is higher that the emission that high pressure leaches is used in less than about 820 DEG C roastings and sulphuric acid reactivities
With excessive acid in saprolife ore deposit roasting sand, the nickel containing in saprolife ore deposit in this N-process dissolves in a large number.This work
The advantage of skill is the sulphuric acid that it better profits from adding in limonite pressure leaching process, decreases for processing autoclave discharge
The limestone of liquid or the consumption of other expensive neutralization reagents, and obtain to the limonite component in lateritic nickel ore body
The ability being processed with saprolite component.But this technique remains a need for being used for the leaching of limonite using expensive autoclave,
And need to carry out calcination process to saprolife ore deposit, this handling process is all costly in fund input and running cost.
United States Patent (USP) No. 6,379,636 B2 describe to United States Patent (USP) No. 4, the entering of the technique described in 097,575
One step is improved, and eliminates saprolife calcination stepses, and saprolife raw ore is used for neutralizing the acid that autoclave discharges excess in solution.
Furthermore, it is possible to add the more acid can leaching content with increase saprolife in relief liquor.But this technique still needs and makes
With expensive autoclave.
In order to avoid using expensive autoclave, the laterite nickel resources of exploitation saprolife and limonite simultaneously, Ren Menti
Some improved normal pressure acidleach technology are gone out.If the patent of invention of Publication No. CN101273146A is it is proposed that extract brown simultaneously
Two step normal pressure leach extraction methods of saprolife ore deposit are extracted, the method has and do not use after iron mine and saprolife ore deposit or first extraction limonite
The advantage of autoclave, but propose when being processed infusion solution to remove Fe and/or A1 in the flow process described in this application,
Need to add the residual acid in nertralizer and in leachate, so that most of ferrum is deposited as ferric hydroxide, this can cause nickel cobalt
Difficult Deng the loss of valuable element and slurry filtration.And for example the patent of invention of Publication No. CN101541985A is it is proposed that one kind
The method of the mixture of normal pressure leaching limonite and saprolife ore deposit, but its ferrum precipitated product is autunezite, contains in autunezite
There is sulfate radical, therefore can increase the acid consumption of leaching process；And autunezite is a kind of compound of thermodynamic instability, pile up and
Sulphuric acid can be discharged, thus causing environmental pollution when depositing.For another example Publication No. CN101006190A patent of invention it is proposed that
A kind of concentrated acid processes the method that the mixture of limonite and saprolife ore deposit and then water logging go out nickel cobalt, the deposition of iron that the method produces
Thing is the ferric oxide or hydroxide in addition to autunezite, but the extraction time of this application needs 12-48h, leaches
Time is longer, leads to process cycle longer, and production cost rises.
For another example the patent of invention of Publication No. CN102206749A is it is proposed that one kind first uses sulfuric acid leaching limonite, then uses
One time leachate extracts saprolife ore deposit, part afterwards（Or all）The circulation that secondary leachate returns again to once leach limonite is normal
Pressure leaching method, the method possesses and can process limonite and saprolife ore deposit and the higher advantage of nickel cobalt leaching rate simultaneously, but technique
Flow process is complex, sulfuric acid consumption is higher（Meansigma methodss are about 0.7g acid/1.0g ore deposit）Shortcoming, and saprolife ore deposit amount used is
More than 1.5 times of limonite amount, and laterite mine belt constitute contradict.For another example the invention of Publication No. CN101001964A is special
Profit it is proposed that a kind of first with enough sulphuric acid in normal pressure（100℃-105℃）Lower leaching limonite, then the normal pressure leaching with limonite
Go out ore pulp with saprolife ore pulp in middle pressure（About 0.5MPa, 150 DEG C）Lower leaching extracts nickel, the method for cobalt.The method excellent
Putting is：Limonite and saprolife ore deposit can be processed simultaneously；Avoid using under the conditions of middle pressure using expensive autoclave
Relatively simple pressurized equipment achieves the higher nickel leaching rate of saprolife ore deposit.But the method suffers from the drawback that and not enough：First
The time of first normal pressure leaching limonite is longer, usually more than 4 hours, and therefore required normal pressure leaching equipment is huge；Two is that acid disappears
Consume higher, total acid/Ore=0.6/1, although this acid consumption index is far below normal pressure acidleach and is far above high pressure acidleach；Three is institute
It it is 1 times of limonite amount with saprolife ore deposit amount, this same and laterite mine belt composition contradicts it is well known that laterite nickel
In mineral deposit, limonite amount: saprolife ore deposit amount >=2: 1.
In a word, in the patent of invention of above-mentioned laterite nickel ore hydrometallurgical, high pressure acidleach（HPAL）Technique and improved height
Pressure acid leaching process shortcoming be：Need the equipment of complicated high temperature, the autoclave of high pressure and correlation, its I＆M is all very
Expensive；The sulphuric acid of HPAL technique consumption is more more than the sulphuric acid needed for the non-ferrous metal components stoichiometrically dissolving in Ore；
HPAL technique is only limited to process the raw material being mainly limonite class；HPAL technique, in the easy fouling of running mesohigh kettle, needs
Periodically stop production cleaning, and the utilization of capacity is low.The shortcoming of normal pressure acid leaching process and improved normal pressure acid leaching process is：Sulfuric acid consumption is high；Nickel,
Cobalt leaching rate is low；Response time is long, and equipment needed thereby is huge.High pressure acidleach includes improved high pressure acid leaching process and normal pressure acidleach work
The common drawback that skill includes improved normal pressure acid leaching process is to leach that the quantity of slag is big, and is the mixing slag of silicon and ferrum so that laterite
The main component ferrum of ore deposit can not cost-effective develop.Although being referred to leached mud in the patent of invention of CN102206749A
Recycling, but due to the silicon dioxide in slag and ferrum oxide, goethitum etc. be reaction generate fine particles, their phases
Mutually " grow " together, be difficult to be separated them with methods such as simple magnetic separation, the economy that therefore above-mentioned leached mud develops
Benefit is very poor, can only work as useless solid process, must work as danger waste residue even for the relatively low leached mud of nickel leaching rate and be processed.
Content of the invention
The invention aims to technical problem present in solution prior art, provide one kind by combining leaching work
Skill carries out sulphuric acid normal pressure leaching and with normal pressure leaching liquid, limonite component is carried out adding to the saprolife ore deposit composition in lateritic nickel ore
What pressure leached reclaims nickel, the method for cobalt, ferrum and silicon.
In order to achieve the above object, the present invention employs the following technical solutions：A kind of combined leaching process that passes through is from laterite nickel
Reclaim nickel, the method for cobalt, ferrum and silicon in ore deposit, comprise the following steps：（a）Add water in saprolife ore deposit prepared saprolife ore pulp, will
Saprolife ore pulp be heated to 60 DEG C -100 DEG C, concentrated sulphuric acid be heated to 150 DEG C -200 DEG C, in Double helix pusher reactor add plus
Saprolife ore pulp after heat and concentrated sulphuric acid, react to dissolve solubility nonferrous metal and soluble iron in saprolife ore deposit；(b)
Water-soluble rear solid-liquid separation is carried out to reaction mass and residue washing obtains normal pressure leaching slag（A）, normal pressure leaching liquid (B) and cleaning mixture
（E）；C () uses cleaning mixture（E）Make limonite slurry with limonite, limonite slurry and normal pressure leaching liquid (B) are separately heated to 95
Add after DEG C -100 DEG C in capstan reactor, pressure be 1.5MPa-4.0Mpa, temperature be 150 DEG C -240 DEG C of condition
Lower pressure leaching 0.5-1.5 hour, the Fe in normal pressure leaching liquid (B)3+Be hydrolyzed to hematite precipitation and discharge acid leach again brown
Iron mine；D () is reduced after temperature is less than 80 DEG C and is carried out solid-liquid separation, obtain pressure leaching slag (C) and pressureleaching solution (D)；(e)
Pressureleaching solution (D) is gone unless passed through have method to reclaim nickel and/or cobalt after nickel cobalt impurity；F () is to pressure leaching slag (C)
Wash post-drying with soda ash solution and obtain Iron concentrate；G () is to normal pressure leaching slag（A）Screened process obtains silicon dioxide and builds
Build sand.
Further, described step（a）The granularity of middle saprolife ore deposit is -80 mesh, and the granularity of limonite is -80 mesh.
Further, described step（a）Middle saprolife ore deposit is 1 with the mass ratio of water:1.2-1:1.
Further, described step（A) in, the mass ratio of saprolife ore pulp and concentrated sulphuric acid is 2:1-2.2:1, the response time
For 1-12 minute.
Further, described step（b）In water-soluble when reaction mass and water mass ratio be 1:1.2-1:1.
Further, described step（C) cleaning mixture in（E）Making proportioning during limonite slurry with limonite is 2L：1Kg.
Further, described step（C) normal pressure leaching liquid (B) is added to make reaction mass final pH in limonite slurry
It is worth for 0.5-1.5.
Further, described step（F) in, the mass fraction of soda ash solution is 10%, and drying temperature is 120 DEG C -150 DEG C.
Further, described step（B) in, normal pressure leaching slag (A) is white residue, and its dioxide-containing silica is 65%-90%.
Further, described step（D) obtaining pressure leaching slag (C) in is bloodstone slag, and wherein iron content is 58%-
65%.
Wherein, the first step is during saprolife acidleach, and the concentrated sulphuric acid of saprolife ore pulp and q.s is quickly fully mixed
Close, the heat of dilution that the water in concentrated sulphuric acid and ore pulp produces makes temperature of charge raise the metal promoting in saprolife ore deposit（Nickel, cobalt, ferrum,
Magnesium, chromium, aluminum etc.）Generate metal sulfate with sulphuric acid fast reaction, substantial amounts of reaction heat makes temperature of charge improve further simultaneously
Ensure that reaction is carried out fully and completely to 95 DEG C -120 DEG C.Silicon dioxide and the unreacted ferrum of very small amount and nonferrous metal form leaching
Go out residue.Second step is the water-soluble and separation of solid and liquid process of normal pressure acidleach material, and the normal pressure leaching material of the first step places one section
Time, temperature-fall period forms loose cellular solid-state mastic, add and can guarantee that the whole water dissolving of metal sulfate simultaneously
Stirring, makes metal sulfate all dissolve entrance solution, obtains normal pressure leaching slag after carrying out solid-liquid separation and residue washing（A）、
Normal pressure leaching liquid (B) and cleaning mixture（E）.3rd step goes out the process of limonite for normal pressure leaching immersion, by normal pressure leaching liquid and brown
Iron mine slurry adds pressure leaching in autoclave, the Fe in filtrate3+It is hydrolyzed to hematite precipitation and discharge acid and leach limonite again,
During reaction pressure be 1.5MPa-4.0Mpa, reaction temperature be 150 DEG C -240 DEG C, not only can guarantee that the hydrolyzate of iron ion is
Bloodstone also has fast hydrolysis rate and higher nickel cobalt leaching rate and leaching velocity.4th step is to drop pressure leaching material
Temperature simultaneously obtains pressure leaching slag (C) and pressureleaching solution (D), wherein pressure leaching slag (C) main component after carrying out solid-liquid separation
For bloodstone, iron content is very high, and pressureleaching solution (D) nickel concentration is higher and ferrum/nickel ratio is relatively low.
Hinge structure of the present invention has the advantages that：
1st, achieve and a kind of sulphuric acid normal pressure leaching is carried out to the saprolife ore deposit composition in lateritic nickel ore by combined leaching process
Go out and with normal pressure leaching liquid, limonite component is carried out pressure leaching reclaims nickel, the method for cobalt, ferrum and silicon, overcomes traditional
It is respectively adopted the deficiency that thermal process and wet processing are processed, the shortcoming eliminating existing high pressure Ore Leaching technique, obtain simultaneously
The nickel higher than known normal pressure leaching technique and the cobalt response rate and faster reclaim speed, the acid lower than existing high pressure acidleach
Consume, naturally easily the main component ironworking of lateritic nickel ore is become Iron concentrate particularly in technical process, by part
Silicon is recovered as high-grade silica product, makes waste residue amount be reduced to 5 the percent about of raw ore amount.With high pressure Ore Leaching
（HPAL) technique is compared, and the pressure leaching of the present invention is carried out, than high pressure acidleach 4.5MPa-5.0MPa under 1.5MPa-4.0Mpa
Mild condition many, compared with normal pressure acidleach, normal pressure leaching time of the present invention is 1-12 minute, and during existing normal pressure acidleach
Between be usually 240 minutes to 2400 minutes, the investment of the normal pressure pickling equipment of the corresponding present invention sets much smaller than existing normal pressure acidleach
Standby investment.
2nd, the sulfuric acid consumption of the present invention is not only far below the acid consumption of existing normal pressure acidleach, and less than existing high pressure acidleach
Acid consumption, the acid consumption of existing normal pressure acidleach is 2.57-3.33 times of present invention acid consumption, and the acid consumption of existing high pressure acidleach is the present invention
1.39-1.71 times of acid consumption.Under the conditions of high pressure acidleach, most sulfate ion connections being provided by sulphuric acid form bisulfate ion
Ion（HSO4 -）That is to say, that sulphuric acid only dissociates under the conditions of high pressure acidleach discharges a proton（H+), cool down in leachate
And during neutralization, hydrogen sulfate ion resolves into sulfate radical（SO4 2-）With another proton, a therefore rear proton (acid）Do not fill
Point it is used for leaching, and lead to excessive sulphuric acid to be to have to be neutralized and consume nertralizer in subsequent treatment.And the present invention
Although needing to consume more sulphuric acid and ferrum reaction generation iron sulfate in the saprolife ore deposit normal pressure leaching stage in method, but brown
The iron mine pressure leaching stage is then not required to separately add sulphuric acid, but relies on Fe3+It is hydrolyzed to the proton of hematite precipitation release（Acid）To soak
Go out limonite, avoiding problems because of hydrogen sulfate ion（HSO4 -）And lead to the low defect of acid-utilising rate, and can significantly drop
The consumption of low follow-up nertralizer.In addition, existing high pressure acid leaching process is ore pulp and concentrated sulphuric acid to be directly added into autoclave leach, high
Press regional area sulfuric acid concentration in kettle very high it is easy to generate the fouling such as ferric subsulfate and Alumen, and the pressurization of present invention leaching
Going out the stage does not have the addition of concentrated sulphuric acid, can avoid the generation of foulant.
3rd, existing high pressure acid leaching process and normal pressure acid leaching process leach the quantity of slag greatly, and its leached mud is the mixing of silicon and ferrum
Slag it is impossible to cost-effective exploitation, specifically, due to the silicon dioxide in leached mud and ferrum oxide, goethitum etc. all
The fine particles generating for reaction, their mutual " growths " together, are difficult to be separated them with methods such as simple magnetic separation, because
The economic benefit that this is developed using the leached mud that existing high pressure acid leaching process and normal pressure acid leaching process obtain is very poor, can only
When useless solid process, danger waste residue must be worked as even for the relatively low leached mud of nickel leaching rate and be processed.And method of the present invention energy
Naturally easily the main component ferrum in ore deposit and part silicon are able to cost-effective recycling in technical process.According to
The method of the present invention, in the normal pressure leaching stage, in saprolife ore deposit ferrum and nonferrous metal and sulfuric acid reaction generate sulfate enter molten
Liquid, silicon formed silicon dioxide become leaching residue, after solid-liquid separation the normal pressure leaching quantity of slag only have saprolife ore deposit amount 30-50%,
Account for the 8-15% of lateritic nickel ore total amount, in normal pressure leaching slag, dioxide-containing silica reaches 80-85%；In pressure leaching stage, normal pressure
Fe in leachate3+All generating bloodstone with the ferrum in limonite becomes leaching residue with a small amount of silicon, adds after solid-liquid separation
In pressure leached mud, iron content is up to 58-65%, and simple process can be used as Iron concentrate and sells.
4th, the nickel leaching rate of the present invention is not only far above the nickel leaching rate of existing normal pressure acidleach, and also above existing high pressure
The nickel leaching rate of acidleach.The nickel leaching rate of existing normal pressure acidleach is 70-85%, and the nickel leaching rate of existing high pressure acidleach is 90-93%,
And the nickel leaching rate of the present invention is more than 95%.
Brief description
Fig. 1 is the schematic flow sheet of the present invention.
Specific embodiment
1 used in following embodiment#、2#With 3#Ore be derived from New Caledonia laterite mineral deposit, 4#With 5#Ore
From Indonesia's laterite mineral deposit, the main component of Ore is shown in Table 1.Saprolife ore deposit and limonite are broken before for experiment
Broken and be ground to granularity be -80 mesh.
The main component table of table 1 Ore
With reference to specific embodiment, the invention will be further described.
Embodiment 1
Take 500Kg 2#Saprolife ore deposit（Dry）500Kg water is added to make saprolife ore pulp, preparing 500Kg mass fraction is
98% concentrated sulphuric acid, by saprolife ore pulp be heated to 60 DEG C, concentrated sulphuric acid be heated to after 200 DEG C use mortar pump and concentrated sulphuric acid pump will plus
Saprolife ore pulp after heat and the charging aperture of concentrated sulphuric acid synchronization addition Double helix pusher reactor, saprolife ore pulp and concentrated sulphuric acid exist
Quick mix after be forced in Double helix pusher reactor fast reaction to dissolve solubility nonferrous metal and soluble iron,
Reaction mass was released Double helix pusher reactor after 1 minute by reaction.It is cooled to less than 60 DEG C, by loose cellular solid-state cream
The reaction mass simple crushing of body is fallen back in leaching tank, adds 1500Kg water, and stirring carries out water-soluble, by water-soluble gained for 30 minutes
Slurry pumps in filter press and carries out solid-liquid separation and residue washing, obtains normal pressure leaching slag（A1）185Kg（Dry）, normal pressure leaching
Go out liquid (B1) 1480L and cleaning mixture (E1) 1200L.Normal pressure leaching slag（A1）, normal pressure leaching liquid (B1) becomes with cleaning mixture (E1's)
Divide and be shown in Table 1-1, table 1-2 and table 1-3.
Take 30Kg1#Limonite（Dry）, add cleaning mixture (E1) 60L to be configured to limonite slurry, limonite slurry be heated to 95
Add after DEG C in the circulating tank of capstan reactor, then be heated to 95 DEG C in the circulating tank of capstan reactor
It is 0.5 that normal pressure leaching liquid (B1) makes reaction mass final ph, opens force (forcing) pump after sealing circulating tank, opens compression tube simultaneously
The hot oil heater of road reactor, control temperature heating, pressure be 1.5MPa, temperature be 240 DEG C under conditions of pressurize
Leach 50 minutes, the Fe in normal pressure leaching liquid (B1)3+It is hydrolyzed to hematite precipitation and discharge acid and leach limonite again；It is cooled to
After 85 DEG C, from the circulating tank of capstan reactor, removal reaction paste carries out solid-liquid separation and washs filtering residue, obtains pressurization leaching
Slag tap（C1）28Kg（Dry）, pressureleaching solution (D1) 76L and cleaning mixture (F1) 46L, pressureleaching solution (D1) is gone unless nickel cobalt
Pass through have method to reclaim nickel and/or cobalt after impurity.Pressure leaching slag（C1）, pressureleaching solution (D1) becomes with cleaning mixture (F1's)
Divide and be shown in Table 1-4, table 1-5 and table 1-6.
Take 300g pressure leaching slag（C1）Add in the beaker filling the soda ash solution that 1000ml mass fraction is 10%, plus
Heat to 60 DEG C and stir 30 minutes, simultaneously dry after washing filter cake under the conditions of temperature is 120 DEG C, obtains bloodstone by solid-liquid separation
（G1）295g.Bloodstone（G1）Composition is shown in Table 1-7.
Take 300g normal pressure leaching slag（A1）Carry out hydrocyclone separation technology, obtain -100 mesh silicon dioxide powders（H1）145g and+
100 mesh fine sand (I1) 150g.Silicon dioxide powder（H1）It is shown in Table 1-8 and table 1-9 with fine sand (I1) composition.
Calculate nickel, cobalt leaching rate, slag rate and acid consumption data as follows：
Normal pressure acidleach nickel leaching rate：98.8%；Normal pressure acidleach cobalt leaching rate：97.6%.
Pressure leaching nickel leaching rate：95.6%；Pressure leaching cobalt leaching rate：94.1%.
Amount to nickel leaching rate 96.9%；Cobalt leaching rate 94.8%.
Iron recovery>96%.
Sulfuric acid consumption：250Kg sulphuric acid/t ore deposit.
Amount to slag rate：46g white residue/1000g lateritic nickel ore.
Embodiment 2
Take 500Kg 5#Saprolife ore deposit（Dry）600Kg water is added to make saprolife ore pulp, preparing 500Kg mass fraction is
98% concentrated sulphuric acid, by saprolife ore pulp be heated to 100 DEG C, concentrated sulphuric acid be heated to after 150 DEG C use mortar pump and concentrated sulphuric acid pump will plus
Saprolife ore pulp after heat and the charging aperture of concentrated sulphuric acid synchronization addition Double helix pusher reactor, saprolife ore pulp and concentrated sulphuric acid exist
Quick mix after be forced in Double helix pusher reactor fast reaction to dissolve solubility nonferrous metal and soluble iron,
Reaction mass was released Double helix pusher reactor after 12 minutes by reaction.It is cooled to less than 60 DEG C, by loose cellular solid-state
The reaction mass simple crushing of mastic is fallen back in leaching tank, adds 1920Kg water, and stirring carries out water-soluble, by water-soluble institute for 30 minutes
Obtain slurry and pump in filter press and carry out solid-liquid separation and residue washing, obtain normal pressure leaching slag（A2）230Kg（Dry）, normal pressure
Leachate (B2) 1500L and cleaning mixture (E2) 1350L.Normal pressure leaching slag（A2）, normal pressure leaching liquid (B2) and cleaning mixture (E2)
Composition is shown in Table 2-1, table 2-2 and table 2-3.
Take 40Kg4#Limonite（Dry）, add cleaning mixture (E2) 80L to be configured to limonite slurry, limonite slurry be heated to
Add after 100 DEG C in the circulating tank of capstan reactor, then be heated to 100 in the circulating tank of capstan reactor
DEG C normal pressure leaching liquid (B2) make reaction mass final ph be 1.5, sealing circulating tank after open force (forcing) pump, simultaneously open plus
The hot oil heater of pressure pipeline reactor, control temperature heating, pressure be 4.0MPa, temperature be 150 DEG C under conditions of
Pressure leaching 30 minutes, the Fe in normal pressure leaching liquid (B2)3+It is hydrolyzed to hematite precipitation and discharge acid and leach limonite again；Fall
Temperature removal reaction paste from the circulating tank of capstan reactor to after 85 DEG C carries out solid-liquid separation and washs filtering residue, is added
Pressure leached mud（C2）34Kg（Dry）, pressureleaching solution (D2) 94L and cleaning mixture (F2) 55L, pressureleaching solution (D2) is gone unless
Pass through have method to reclaim nickel and/or cobalt after nickel cobalt impurity.Pressure leaching slag（C2）, pressureleaching solution (D2) and cleaning mixture (F2)
Composition be shown in Table 2-4, table 2-5 and table 2-6.
Take 300g pressure leaching slag（C2）Add in the beaker filling the soda ash solution that 1000ml mass fraction is 10%, plus
Heat to 60 DEG C and stir 30 minutes, simultaneously dry after washing filter cake under the conditions of temperature is 120 DEG C, obtains bloodstone by solid-liquid separation
（G2）295g.Bloodstone（G2）Composition is shown in Table 2-7.
Take 300g normal pressure leaching slag（A2）Carry out hydrocyclone separation technology, obtain -100 mesh silicon dioxide powders（H1）143g and+
100 mesh fine sand (I1) 151g.Silicon dioxide powder（H2）It is shown in Table 2-8 and table 2-9 with fine sand (I2) composition.
Calculate nickel, cobalt leaching rate, slag rate and acid consumption data as follows：
Normal pressure acidleach nickel leaching rate：98.1%；Normal pressure acidleach cobalt leaching rate：93.5%.
Pressure leaching nickel leaching rate：94.6%；Pressure leaching cobalt leaching rate：92.1%.
Amount to nickel leaching rate 95.5%；Cobalt leaching rate 93.1%.
Iron recovery>96%.
Sulfuric acid consumption：180Kg sulphuric acid/t ore deposit.
Amount to slag rate：46.3g white residue/1000g lateritic nickel ore.
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 changes into
4#Indonesia's limonite.
Take 30Kg4#Limonite（Dry）, add cleaning mixture (E1) 60L to be configured to limonite slurry, limonite slurry be heated to 95
Add after DEG C in the circulating tank of capstan reactor, then be heated to 95 DEG C in the circulating tank of capstan reactor
It is 1.0 that normal pressure leaching liquid (B1) makes reaction mass final ph, opens force (forcing) pump after sealing circulating tank, opens compression tube simultaneously
The hot oil heater of road reactor, control temperature heating, pressure be 2.0MPa, temperature be 223 DEG C under conditions of pressurize
Leach 60 minutes, the Fe in normal pressure leaching liquid (B1)3+It is hydrolyzed to hematite precipitation and discharge acid and leach limonite again；It is cooled to
After 85 DEG C, from the circulating tank of capstan reactor, removal reaction paste carries out solid-liquid separation and washs filtering residue, obtains pressurization leaching
Slag tap（C3）29Kg（Dry）, pressureleaching solution (D3) 76L and cleaning mixture (F3) 44L, pressureleaching solution (D3) is gone unless nickel cobalt
Pass through have method to reclaim nickel and/or cobalt after impurity.Pressure leaching slag（C3）, pressureleaching solution (D3) becomes with cleaning mixture (F3's)
Divide and be shown in Table 3-1, table 3-2 and table 3-3.
Take 300g pressure leaching slag（C3）Add in the beaker filling the soda ash solution that 1000ml mass fraction is 10%, plus
Heat to 60 DEG C and stir 30 minutes, simultaneously dry after washing filter cake under the conditions of temperature is 130 DEG C, obtains bloodstone by solid-liquid separation
（G3）295g.Bloodstone（G3）Composition is shown in Table 3-4.
Take 300g normal pressure leaching slag（A1）Carry out hydrocyclone separation technology, obtain -100 mesh silicon dioxide powders（H1）145g and+
100 mesh fine sand (I1) 150g.
Calculate nickel, cobalt leaching rate, slag rate and acid consumption data as follows：
Pressure leaching nickel leaching rate：95.4%；Pressure leaching cobalt leaching rate：93.2%.
Amount to nickel leaching rate 96.6%；Cobalt leaching rate 93.3%.
Iron recovery>96%.
Sulfuric acid consumption：250Kg sulphuric acid/t ore deposit.
Amount to slag rate：92.5g white residue/1000g lateritic nickel ore.
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 changes into
1#New noise made in coughing or vomiting limonite.
Take 40Kg1#Limonite（Dry）, add cleaning mixture (E1) 80L to be configured to limonite slurry, limonite slurry be heated to
Add after 100 DEG C in the circulating tank of capstan reactor, then be heated to 100 in the circulating tank of capstan reactor
DEG C normal pressure leaching liquid (B1) make reaction mass final ph be 1.5, sealing circulating tank after open force (forcing) pump, simultaneously open plus
The hot oil heater of pressure pipeline reactor, control temperature heating, pressure be 3MPa, temperature be 185 DEG C under conditions of plus
Pressure leaches 45 minutes, the Fe in normal pressure leaching liquid (B1)3+It is hydrolyzed to hematite precipitation and discharge acid and leach limonite again；Cooling
To after 85 DEG C, from the circulating tank of capstan reactor, removal reaction paste carries out solid-liquid separation and washs filtering residue, is pressurizeed
Leached mud（C4）38Kg（Dry）, pressureleaching solution (D4) 94L and cleaning mixture (F4) 55L, pressureleaching solution (D4) is gone unless nickel
Pass through have sulfide precipitation method to reclaim nickel and/or cobalt after cobalta matter.Pressure leaching slag（C4）, pressureleaching solution (D4) and washing
The composition washing liquid (F4) is shown in Table 4-1, table 4-2 and table 4-3.
Take 300g pressure leaching slag（C4）Add in the beaker filling the soda ash solution that 1000ml mass fraction is 10%, plus
Heat to 60 DEG C and stir 30 minutes, simultaneously dry after washing filter cake under the conditions of temperature is 140 DEG C, obtains bloodstone by solid-liquid separation
（G4）295g.Bloodstone（G4）Composition is shown in Table 4-4.
Take 300g normal pressure leaching slag（A2）Carry out hydrocyclone separation technology, obtain -100 mesh silicon dioxide powders（H2）143g and+
100 mesh fine sand (I2) 151g.
Calculate nickel, cobalt leaching rate, slag rate and acid consumption data as follows：
Pressure leaching nickel leaching rate：95.1%；Pressure leaching cobalt leaching rate：93.7%.
Amount to nickel leaching rate 96.9%；Cobalt leaching rate 94.4%.
Iron recovery>96%.
Sulfuric acid consumption：180Kg sulphuric acid/t ore deposit.
Amount to slag rate：92.0g white residue/1000g lateritic nickel ore.
Embodiment 5（Reference examples）
The normal pressure acid leaching stage of the present embodiment is identical with embodiment 1, in the pressure leaching stage by 1#New noise made in coughing or vomiting limonite changes into
3#New Ka Guodukuang.
Take 30Kg3#Transition ore deposit（Dry）, add cleaning mixture (E1) 60L to be configured to transition ore pulp, transition ore pulp be heated to 95
Add after DEG C in the circulating tank of capstan reactor, then be heated to 95 DEG C in the circulating tank of capstan reactor
It is 1.0 that normal pressure leaching liquid (B1) makes reaction mass final ph, opens force (forcing) pump after sealing circulating tank, opens compression tube simultaneously
The hot oil heater of road reactor, control temperature heating, pressure be 2.0MPa, temperature be 223 DEG C under conditions of pressurize
Leach 60 minutes, the Fe in normal pressure leaching liquid (B1)3+It is hydrolyzed to hematite precipitation and discharge acid and leach transition ore deposit again；It is cooled to
After 85 DEG C, from the circulating tank of capstan reactor, removal reaction paste carries out solid-liquid separation and washs filtering residue, obtains pressurization leaching
Slag tap（C5）29Kg（Dry）, pressureleaching solution (D5) 76L and cleaning mixture (F5) 47L, pressureleaching solution (D5) is gone unless nickel cobalt
Pass through have sulfide precipitation method to reclaim nickel and/or cobalt after impurity.Pressure leaching slag（C5）, pressureleaching solution (D5) and washing
The composition of liquid (F5) is shown in Table 5-1, table 5-2 and table 5-3.
Take 300g pressure leaching slag（C5）Add in the beaker filling the soda ash solution that 1000ml mass fraction is 10%, plus
Heat to 60 DEG C and stir 30 minutes, simultaneously dry after washing filter cake under the conditions of temperature is 120 DEG C, obtains bloodstone by solid-liquid separation
（G5）293g.Bloodstone（G5）Composition is shown in Table 5-4.
Calculate nickel, cobalt leaching rate, slag rate and acid consumption data as follows：
Pressure leaching nickel leaching rate：94.7%；Pressure leaching cobalt leaching rate：92.5%.
Amount to nickel leaching rate 95.4%；Cobalt leaching rate 93.6%.
Iron recovery>96%.
Sulfuric acid consumption：250Kg sulphuric acid/t ore deposit.
Amount to slag rate：92.0g white residue/1000g lateritic nickel ore.
In above example, embodiment 1 and embodiment 2 are combined with the saprolife in same mineral deposit and limonite；Embodiment 3
With embodiment 4 saprolife in different mineral deposits and limonite combination；As a comparison, embodiment 5 saprolife and transition ore deposit group
Close.In terms of analytical data, the nickel of five embodiments（Cobalt）The technical specifications such as leaching rate, sulfuric acid consumption are all preferable, but due to implementing
Example 5 uses saprolife and the combination of transition ore deposit, and the iron content of therefore pressure leaching slag is only 44.3%, and ferrum almost cannot reclaim
Using, and the iron content of the pressure leaching slag that other four embodiments obtain is all more than 58%, the bloodstone iron content of recovery is about
60%, the response rate of ferrum is more than 96%.Amount to slag rate about 90.0g white residue/1000g lateritic nickel ore, after reclaiming silicon dioxide
Slag rate is down to about 46g white residue/1000g lateritic nickel ore.
Claims (10)
1. a kind of method reclaiming nickel, cobalt, ferrum and silicon by combined leaching process from lateritic nickel ore it is characterised in that：Including
Following steps：
（a）Add water in saprolife ore deposit prepared saprolife ore pulp, saprolife ore pulp is heated to 60 DEG C -100 DEG C, concentrated sulphuric acid adds
Heat to 150 DEG C -200 DEG C, in Double helix pusher reactor add heating after saprolife ore pulp and concentrated sulphuric acid, react with
Solubility nonferrous metal and soluble iron in dissolving saprolife ore deposit；
B () carries out water-soluble rear solid-liquid separation to reaction mass and residue washing obtains normal pressure leaching slag（A）, normal pressure leaching liquid (B)
And cleaning mixture（E）；
C () uses cleaning mixture（E）Make limonite slurry with limonite, limonite slurry and normal pressure leaching liquid (B) are separately heated to 95
Add after DEG C -100 DEG C in capstan reactor, pressure be 1.5MPa-4.0Mpa, temperature be 150 DEG C -240 DEG C of condition
Lower pressure leaching 0.5-1.5 hour, the Fe in normal pressure leaching liquid (B)3+Be hydrolyzed to hematite precipitation and discharge acid leach again brown
Iron mine；
D () is reduced after temperature is less than 80 DEG C and is carried out solid-liquid separation, obtain pressure leaching slag (C) and pressureleaching solution (D)；
E () goes to pressureleaching solution (D) unless passed through have method to reclaim nickel and/or cobalt after nickel cobalt impurity；
F () is washed post-drying to pressure leaching slag (C) with soda ash solution and is obtained Iron concentrate；
G () is to normal pressure leaching slag（A）Screened process obtains silicon dioxide and building sand.
2. a kind of side reclaiming nickel, cobalt, ferrum and silicon by combined leaching process from lateritic nickel ore according to claim 1
Method it is characterised in that：Described step（a）The granularity of middle saprolife ore deposit is -80 mesh, and the granularity of limonite is -80 mesh.
3. a kind of side reclaiming nickel, cobalt, ferrum and silicon by combined leaching process from lateritic nickel ore according to claim 1
Method it is characterised in that：Described step（a）Middle saprolife ore deposit is 1 with the mass ratio of water:1.2-1:1.
4. a kind of side reclaiming nickel, cobalt, ferrum and silicon by combined leaching process from lateritic nickel ore according to claim 1
Method it is characterised in that：Described step（A) in, the mass ratio of saprolife ore pulp and concentrated sulphuric acid is 2:1-2.2:1, the response time is 1-
12 minutes.
5. a kind of side reclaiming nickel, cobalt, ferrum and silicon by combined leaching process from lateritic nickel ore according to claim 1
Method it is characterised in that：Described step（b）In water-soluble when reaction mass and water mass ratio be 1:1.2-1:1.
6. a kind of side reclaiming nickel, cobalt, ferrum and silicon by combined leaching process from lateritic nickel ore according to claim 1
Method it is characterised in that：Described step（C) cleaning mixture in（E）Making proportioning during limonite slurry with limonite is 2L：1Kg.
7. a kind of side reclaiming nickel, cobalt, ferrum and silicon by combined leaching process from lateritic nickel ore according to claim 1
Method it is characterised in that：Described step（C) normal pressure leaching liquid (B) is added to make reaction mass final ph in limonite slurry
For 0.5-1.5.
8. a kind of side reclaiming nickel, cobalt, ferrum and silicon by combined leaching process from lateritic nickel ore according to claim 1
Method it is characterised in that：Described step（F) in, the mass fraction of soda ash solution is 10%, and drying temperature is 120 DEG C -150 DEG C.
9. a kind of side reclaiming nickel, cobalt, ferrum and silicon by combined leaching process from lateritic nickel ore according to claim 1
Method it is characterised in that：Described step（B) in, normal pressure leaching slag (A) is white residue, and its dioxide-containing silica is 65%-90%.
10. according to claim 1 a kind of reclaim nickel, cobalt, ferrum and silicon from lateritic nickel ore by combined leaching process
Method it is characterised in that：Described step（D) obtaining pressure leaching slag (C) in is bloodstone slag, and wherein iron content is 58%-65%.
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| US2872306A (en) * | 1956-05-29 | 1959-02-03 | Freeport Sulphur Co | Recovery of cobalt and nickel from ores |
| US2971836A (en) * | 1957-04-29 | 1961-02-14 | James D Hall | Separation of nickel and cobalt |
| US3093559A (en) * | 1958-06-20 | 1963-06-11 | Merwin G White | Treatment of lateritic ores |
| CA922903A (en) * | 1970-07-08 | 1973-03-20 | The International Nickel Company Of Canada | Acid leaching of lateritic ore |
| US3991159A (en) * | 1975-01-09 | 1976-11-09 | Amax Inc. | High temperature neutralization of laterite leach slurry |
| ES2394915T3 (en) * | 2005-02-14 | 2013-02-06 | Bhp Billiton Ssm Development Pty Ltd | Procedure for improved acid leaching of laterite minerals |
| AU2008286193B2 (en) * | 2007-08-07 | 2011-10-27 | Bhp Billiton Ssm Development Pty Ltd | Atmospheric acid leach process for laterites |
| 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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Effective date of registration: 20190215 Address after: 730101 Jinchuan Science and Technology Park, Peace Economic Development Zone, Yuzhong County, Lanzhou City, Gansu Province Patentee after: Gansu Jinchuan Nickel-Cobalt New Material Technology Innovation Center Co., Ltd. Address before: No. 98 Jinchuan Road, Jinchang, Gansu Patentee before: Jinchuan Group Co., Ltd. |