CN102286661A - Method for direct electrolysis of laterite nickel ore by sulfuric acid leaching - Google Patents
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Abstract
The invention provides a method for direct electrolysis of laterite nickel ore by sulfuric acid leaching, and relates to a method for sulfuric acid normal-pressure leaching of low-grade laterite nickel ore, belonging to the technical field of hydrometallurgy. The method comprises the steps: separately grinding and pulping iron ore and magnesium ore in the laterite nickel ore, carrying out sulfuric leaching of the iron ore at high acidity and high acid-to-ore ratio, adding the magnesium ore pulp to adjust the pH value for settling ferroalumen, adding a basic neutralizing agent to the mother liquor for removing aluminum and silicon, adsorbing nickel ion from the filtered leachate with ion exchange resin, after the adsorbed nickel ion is saturated, washing with an acid to desorb the nickel ion, purifying the generated enriched nickel sulfate solution to remove impurities, then electrolyzing to produce an electrolytic nickel product, adding calcium hydroxide to the ion-resin-exchanged solution containing magnesium sulfate for precipitating, and carbonizing and separating calcium and magnesium to obtain magnesium carbonate. By using the method provided by the invention, the defects that the process is long and magnesium-containing wastewater is large in amount and is difficult to treat in the prior art are solved, so that magnesium is processed into the product, wastewater can be directly discharged or recycled, and at the same time, partial recovered magnesium can be returned to the process to be recycled as the neutralizing agent.
Description
Technical field
The present invention relates to a kind of sulfuric acid normal pressure and leach low-grade red soil nickel ore, through heavy iron, take off assorted, filter the adsorption-desorption that the back spent ion exchange resin carries out nickel, the method for production electrolytic nickel belongs to technical field of wet metallurgy after the refining.
Background technology
Red soil nickel ore accounts for 70% of global nickel resources total amount, but recovery percent is far away from nickel sulfide ore.Different by its main component, mineral composition with treatment process, mainly be divided into two big classes.One class is the low irony nickel minerals of the high magnesium of iron, and a class is the low high magnesia nickel minerals of magnesium of iron.Its smelting technology pyrogenic process, wet method, fiery wet method mainly contain high pressure acidleach, normal pressure acidleach (containing dump leaching and agitation leach), reduction roasting-ammonia leaching, rotary kiln drying prereduction-ore-smelting furnace retailoring etc. in conjunction with all having.
Pure wet processing mainly contains ammonia and soaks (alkali soaks), acidleach and biological leaching etc., and the branch that acidleach has sulfuric acid, nitric acid, hydrochloric acid and mixes acidleach.Limonite type laterite be fit to is handled in the high pressure acidleach, and (under 4.5～4.7MPa) conditions, with 97% nickel, 95% cobalt leaches and enters solution in sulfuric acid medium, and molten iron is separated and generated rhombohedral iron ore and enter in the slag at high temperature (240～260 ℃), high pressure.The precipitable production nickel of leach liquor cobalt sulfide or oxyhydroxide, further metallic nickel is produced in refining, also directly extracting and separating enriching nickel, cobalt.Representative factory comprises Murrin Murrin, Cawse and Bulong.Normal pressure leaches (containing dump leaching and agitation leach) relatively more suitable processing red soil nickel ore that iron content is low, magnesium is high, and 80～85 ℃ of following agitation leachs, liquid-solid separation postprecipitation reclaims the nickel cobalt.In general this technology founded the factory in the coastland to solve and contained magnesium discharge of wastewater problem in a large number, limitation clearly, but investment is very low, is fit to small-scale production.
Domesticly done big quantity research at the sulfuric acid extract technology, main patent has:
BHP Billiton SSM Dev Pty Ltd.'s patent, " method of normal pressure acid leaching of laterite " (CN101778958A), preparing solids content respectively is 20%～40% limonite slurry and saprolite ore pulp, with sour ore deposit weight ratio (sulfuric acid and limonite) is to carry out elementary lixiviate under 1:30 to 1:65, normal atmosphere and 105 ℃, move to again in other one or more reactors, add the saprolite ore pulp and under normal atmosphere and 105 ℃, carry out secondary lixiviate.
Guangxi Metallurgy Inst.'s patent, " method of Separation and Recovery nickel cobalt, magnesium, iron and silicon from red soil nickel ore " (CN101525690A), adopt the nickel cobalt magnesium iron in the high temperature peracid leaching red soil nickel ore, after press filtration, obtain leach liquor, in leach liquor, add serpentine, two sections deironing of magnesite breeze again, obtain qualified Ni-Mg solution, add magnesite breeze precipitation nickelous carbonate again, heavy nickel mother liquor condensing crystal reclaim(ed) sulfuric acid magnesium.
Jinchuan Group Co.,Ltd's patent, " a kind of laterite nickel ore leaching method " (CN101139656A) are carried out one section pressurization to laterite nickel mixing ore deposit and are leached, and add the detritus soil ore pulp again, carry out two sections pressurization oxygenations and leach.
Jiangxi Rare and rare earth tungsten industry Group Co.,Ltd's patent, " a kind of method of extracting nickel and/or cobalt " (CN101270417A) adopt normal pressure to heat to limonite model ore and stir leaching, and serpentine type ore then adopts the leaching of dump leaching method.
Carry out processing behind solid-liquid separation, the desiliconization aluminium for the red soil nickel ore pickling liquor, modes such as precipitate nickel sulphides, nickel hydroxide are arranged, main patent has:
Central South University's patent, " a kind of method from red soil nickel ore leach liquor separation and concentration nickel cobalt " (CN101298638A) after sulfuric acid or hydrochloric acid leaching solid-liquid separation, add sodium sulphite, hydrogen sulfide or ammonium sulfide, the reaction precipitation nickelous sulfide." a kind of method that adopts sulfide precipitation concentrating cobalt and nickel from the red soil nickel ore leach liquor " (CN101302584A) then adopts hydrogeneous and not hydrogenous vulcanizing agent to mix or add respectively and carries out nickel sulphide precipitation in the leach liquor.
The scientific and technological mining and metallurgy of Guangxi silver hundred million company limited patent, " a kind of two-section type sink nickel method " (CN102061387A), in magniferous nickel sulfate solution, add sodium hydroxide solution, adjust pH value and be 7.5～8.5,20～80 ℃ of temperature of reaction, 0.5～3 hour reaction times, carry out one section and precipitate nickel hydroxide; In heavy nickel mother liquor, add sodium hydroxide solution again after the solid-liquid separation, adjust pH value and be 9～10,20～80 ℃ of temperature of reaction, 0.5～3 hour reaction times, carry out two sections and precipitate nickel hydroxides.
For the enrichment of nickel, cobalt in the sulphuric acid soln of nickeliferous, cobalt, magnesium, mainly contain extraction agent extraction, back extraction, and modes such as ion exchange resin absorption, desorb, domestic main patent has:
Xien Chemical Equipment Co., Ltd., Shanghai's patent, " method of enrichment and purifying nickel, cobalt or cupric ion " (CN101338367A), nickel, cobalt or copper solutions are adopted aeration or add the oxygenant mode, make the divalent iron ion be oxidized to 3 valencys, add lime carbonate or magnesium oxide and regulate the pH value, re-use the imido oxalic acid type resin nickel in the solution, cobalt or copper are adsorbed, use sulfuric acid, hydrochloric acid or nitric acid to carry out the pickling desorb at last, reach the purpose of enriching nickel, cobalt or copper.
Generally speaking, sulfuric acid leaches red soil nickel ore technology and mainly exists not high, the sour consumption of nickel leaching yield, the rate of recovery big, contain particularly that the magnesium wastewater flow rate is big, the shortcoming of difficult treatment, in addition, if adopt the mode of precipitate nickel sulphides, can produce hypertoxic hydrogen sulfide, there is bigger potential safety hazard, and the oxygenation acidleach nickelous sulfide that need pressurize, carry out the deep purifying of deferrization, aluminium silicon again, just can carry out the production of electrolytic nickel.
Summary of the invention
In view of this, the object of the present invention is to provide a kind of red soil nickel ore sulfuric acid to leach direct electrolytic method, its acid consumption is little, technical process is short, magnesium in the system can obtain open circuit and become useful products, factory effluent can directly efflux or reuse, but simultaneously partially recycled magnesium Returning process is as neutralizing agent.
The present invention achieves the above object by the following technical programs: to the irony ore deposit and the magnesia ore deposit difference ore grinding that contains magnesium 10～30% of the iron content in the red soil nickel ore 15～30%, slurrying, sulfuric acid leaches the irony ore deposit under the sour ore deposit mass ratio of the acidity of 200～300g/L and 0.8～1.2:1, add magnesia ore pulp and adjust pH value to 3.0 precipitation siderotil, add alkaline neutraliser adjustment pH value to 6.0 in the mother liquor again and remove aluminium silicon, leach liquor spent ion exchange resin absorbed Ni ion after the filtration, adsorb saturated back acid elution desorb nickel ion, the enrichment nickel sulfate solution of output takes off assorted through purification, electrolysis output electrolytic nickel product, the sulfur acid magnesium solution behind ion exchange resin adds the calcium hydroxide neutralization precipitation, get magnesiumcarbonate behind the carbonization separating magnesium calcium.
Concrete steps of the present invention are:
A, elect the red soil nickel ore branch as irony ore deposit and magnesia ore deposit, ore grinding is to granularity 60～200 orders respectively, and is prepared into the ore pulp of concentration 20～55wt%;
B, the irony ore pulp is added in the reactor, add sulfuric acid agitation leach under whipped state;
After C, irony ore deposit are leached and finished, in the leaching ore pulp, add magnesia ore pulp and leach magnesium, iron is precipitated as yellow modumite;
After D, heavy iron are finished, add neutralizing agent magnesium hydroxide, sodium hydroxide or calcium hydroxide and neutralize except that aluminium silicon;
Leach liquor after E, the filtration with imido oxalic acid type ion exchange resin absorbed Ni ion, adsorbs saturated back sulfuric acid scrubbing desorb nickel ion, the enrichment nickel sulfate solution of the nickeliferous 45～50g/L of output;
F, nickel sulfate solution take off assorted, electrolysis output electrolytic nickel product through purification;
Liquid sulfur acid magnesium solution behind G, the ion exchange resin absorbed Ni ion, add calcium hydroxide and obtain magnesium hydroxide, part is returned this technical process and is used as neutralizing agent, and redundance obtains magnesiumcarbonate again after carbonization, pyrolysis, calcine magnesiumcarbonate again and obtain magnesium oxide product.
The neutralizing agent that adds among the above-mentioned steps D of the present invention is a resulting magnesium hydroxide among the step G after this technology.
The irony ore deposit that red soil nickel ore of the present invention sub-elects is nickeliferous 0.8～1.8%, iron 15～30%, magnesium＜15%; Magnesia ore deposit is nickeliferous 0.8～1.8%, iron＜15%, magnesium 10～30%.
Outstanding advantage of the present invention is:
The present invention than under the condition, does not need airtight, pressurization, oxygenation in high acidity, peracid ore deposit, can fully leach into the nickel in the irony ore deposit of red soil nickel ore in the liquid phase under normal pressure, and iron fully is oxidized to three valence states.
The present invention adds magnesia ore deposit after finish in leaching irony ore deposit, improve the pH value, make ferric iron reach precipitation ferrovanadium condition, in precipitation process, discharge the acid that it consumes, utilize the acid of residual acid and release to carry out the leaching of nickel in the magnesia ore deposit, reduce the whole acid consumption that nickel leaches, further, reduced reactor quantity.Because leach easily than irony ore deposit in magnesia ore deposit, can carry out under lower acidity, with magnesia ore deposit in-situ precipitate siderotil, is precipitated as yellow modumite, has also improved the filterableness of leached mud, reduce and filter energy consumption.
The present invention adds alkali such as the magnesium hydroxide that reclaims in the follow-up flow process or sodium hydroxide/calcium hydroxide, further precipitation of aluminium, silicon after iron precipitation is finished, the filterableness of acid leaching ore pulp is strengthened, further, make the magnesium in the wet processing can reuse, saved production cost.
The present invention adopts ion exchange resin adsorption-desorption nickel ion, obtains the nickel sulfate solution of enrichment, takes off the direct electrolysis in assorted back through purification.Cancel nickel precipitation and dissolved operation again, saved production cost.
Description of drawings
Figure of description is a principle process flow sheet of the present invention.
Specific embodiment
Below by specific embodiment technical scheme of the present invention is described in further detail, providing of embodiment limits the present invention anything but.
The present invention is that a kind of red soil nickel ore sulfuric acid leaches direct electrolytic technology, and performing step is as follows:
Embodiment 1:Get laterite ferronickel matter ore deposit (nickeliferous 0.8～1.8%, iron 15～30%, magnesium＜15%) 200g ore grinding to-100 orders, add water and be prepared into and contain solid 30% irony ore pulp.
Get the magnesia ore deposit of laterite nickel (nickeliferous 0.8～1.8%, iron＜15%, magnesium 10～30%) 200g ore grinding to-100 orders, add water and be prepared into and contain solid 30% magnesia ore pulp.
Slowly add sulfuric acid 120ml in the irony ore pulp, normal pressure stirs, and carries out irony ore deposit sulfuric acid and leaches extraction time 4 hours.
In finishing the acid leaching ore pulp of leaching, slowly add the magnesia ore pulp for preparing, add 20g sodium sulfate, normal pressure stirs, and monitoring pH value up to pH=3.0, stops to add magnesia ore pulp, continues to stir 3 hours, finishes the precipitation ferrovanadium.Slowly add aqua calcis, monitoring pH value up to pH=6.0, is stablized and is finished aluminium silicon behind the no change and precipitate.
Filter, clear liquid is single nickel salt, magnesium solution, enters ion exchange resin column absorbed Ni ion, behind nickel ion concentration＜0.2g/L, is the sulfuric acid scrubbing ion exchange resin of 300g/L with acidity in the liquid of absorption back, obtains the nickel sulfate solution that nickel ion concentration is 48g/L.
Nickel sulfate solution takes off assorted through purification, directly electrolysis obtains electrolytic nickel.
Mother liquor is an Adlerika after the ion-exchange, adds aqua calcis and is neutralized to pH〉10, obtain magnesium hydroxide, the part Returning process, all the other magnesium, calcium after carbonization, pyrolysis separate, and obtain magnesiumcarbonate.
Embodiment 2:Get laterite ferronickel matter ore deposit (nickeliferous 0.8～1.8%, iron 15～30%, magnesium＜15%) 200g ore grinding to-160 orders, add water and be prepared into and contain solid 35% irony ore pulp.
Get the magnesia ore deposit of laterite nickel (nickeliferous 0.8～1.8%, iron＜15%, magnesium 10～30%) 200g ore grinding to-100 orders, add water and be prepared into and contain solid 30% magnesia ore pulp.
Slowly add sulfuric acid 110ml in the irony ore pulp, normal pressure stirs, and carries out irony ore deposit sulfuric acid and leaches extraction time 4 hours.
In finishing the acid leaching ore pulp of leaching, slowly add the magnesia ore pulp for preparing, add 20g sodium sulfate, normal pressure stirs, and monitoring pH value up to pH=3.0, stops to add magnesia ore pulp, continues to stir 3 hours, finishes the precipitation ferrovanadium.Slowly add aqua calcis, monitoring pH value up to pH=6.0, is stablized and is finished aluminium silicon behind the no change and precipitate.
Filter, clear liquid is single nickel salt, magnesium solution, enters ion exchange resin column absorbed Ni ion, behind nickel ion concentration＜0.2g/L, is the sulfuric acid scrubbing ion exchange resin of 300g/L with acidity in the liquid of absorption back, obtains the nickel sulfate solution that nickel ion concentration is 50g/L.
Nickel sulfate solution takes off assorted through purification, directly electrolysis obtains electrolytic nickel.
Mother liquor is an Adlerika after the ion-exchange, adds aqua calcis and is neutralized to pH〉10, obtain magnesium hydroxide, the part Returning process, all the other magnesium, calcium after carbonization, pyrolysis separate, and obtain magnesiumcarbonate.
Embodiment 3:Get laterite ferronickel matter ore deposit (nickeliferous 0.8～1.8%, iron 15～30%, magnesium＜15%) 200g ore grinding to-200 orders, add water and be prepared into and contain solid 40% irony ore pulp.
Get the magnesia ore deposit of laterite nickel (nickeliferous 0.8～1.8%, iron＜15%, magnesium 10～30%) 200g ore grinding to-100 orders, add water and be prepared into and contain solid 30% magnesia ore pulp.
Slowly add sulfuric acid 95ml in the irony ore pulp, normal pressure stirs, and carries out irony ore deposit sulfuric acid and leaches extraction time 4 hours.
In finishing the acid leaching ore pulp of leaching, slowly add the magnesia ore pulp for preparing, add 20g sodium sulfate, normal pressure stirs, and monitoring pH value up to pH=3.0, stops to add magnesia ore pulp, continues to stir 3 hours, finishes the precipitation ferrovanadium.Slowly add aqua calcis, monitoring pH value up to pH=6.0, is stablized and is finished aluminium silicon behind the no change and precipitate.
Filter, clear liquid is single nickel salt, magnesium solution, enters ion exchange resin column absorbed Ni ion, behind nickel ion concentration＜0.2g/L, is the sulfuric acid scrubbing ion exchange resin of 300g/L with acidity in the liquid of absorption back, obtains the nickel sulfate solution that nickel ion concentration is 46g/L.
Nickel sulfate solution takes off assorted through purification, directly electrolysis obtains electrolytic nickel.
Mother liquor is an Adlerika after the ion-exchange, adds aqua calcis and is neutralized to pH〉10, obtain magnesium hydroxide, the part Returning process, all the other magnesium, calcium after carbonization, pyrolysis separate, and obtain magnesiumcarbonate.
Claims (4)
1. a red soil nickel ore sulfuric acid leaches direct electrolytic method, it is characterized in that: to the irony ore deposit and the magnesia ore deposit difference ore grinding that contains magnesium 10～30% of the iron content in the red soil nickel ore 15～30%, slurrying, sulfuric acid leaches the irony ore deposit under the sour ore deposit mass ratio of the acidity of 200～300g/L and 0.8～1.2 ︰ 1, add magnesia ore pulp and adjust pH value to 3.0 precipitation siderotil, add alkaline neutraliser adjustment pH value to 6.0 in the mother liquor again and remove aluminium silicon, leach liquor spent ion exchange resin absorbed Ni ion after the filtration, adsorb saturated back acid elution desorb nickel ion, the enrichment nickel sulfate solution of output takes off assorted through purification, electrolysis output electrolytic nickel product, the sulfur acid magnesium solution behind ion exchange resin adds the calcium hydroxide neutralization precipitation, get magnesiumcarbonate behind the carbonization separating magnesium calcium.
2. leach direct electrolytic method by the described red soil nickel ore sulfuric acid of claim 1, it is characterized in that concrete steps are:
A, elect the red soil nickel ore branch as irony ore deposit and magnesia ore deposit, ore grinding is to granularity 60～200 orders respectively, and is prepared into the ore pulp of concentration 20～55wt%;
B, the irony ore pulp is added in the reactor, add sulfuric acid agitation leach under whipped state;
After C, irony ore deposit are leached and finished, in the leaching ore pulp, add magnesia ore pulp and leach magnesium, iron is precipitated as yellow modumite;
After D, heavy iron are finished, add neutralizing agent magnesium hydroxide, sodium hydroxide or calcium hydroxide and neutralize except that aluminium silicon;
Leach liquor after E, the filtration with imido oxalic acid type ion exchange resin absorbed Ni ion, adsorbs saturated back sulfuric acid scrubbing desorb nickel ion, the enrichment nickel sulfate solution of the nickeliferous 45～50g/L of output;
F, nickel sulfate solution take off assorted, electrolysis output electrolytic nickel product through purification;
Liquid sulfur acid magnesium solution behind G, the ion exchange resin absorbed Ni ion, add calcium hydroxide and obtain magnesium hydroxide, part is returned this technical process and is used as neutralizing agent, and redundance obtains magnesiumcarbonate again after carbonization, pyrolysis, calcine magnesiumcarbonate again and obtain magnesium oxide product.
3. leach direct electrolytic method by the described red soil nickel ore sulfuric acid of claim 2, it is characterized in that: the neutralizing agent that adds among the step D is a resulting magnesium hydroxide among the step G after this technology.
4. leach direct electrolytic method by claim 2 or 3 described red soil nickel ore sulfuric acid, it is characterized in that: the irony ore deposit that red soil nickel ore sub-elects is nickeliferous 0.8～1.8%, iron 15～30%, magnesium＜15%; Magnesia ore deposit is nickeliferous 0.8～1.8%, iron＜15%, magnesium 10～30%.
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| CN104120259A (en) * | 2014-07-30 | 2014-10-29 | 广西师范大学 | Nickel oxide ore acid leaching solution two-step iron removal method |
| CN104254498A (en) * | 2012-03-20 | 2014-12-31 | 曼特尓斯矿业私人有限公司 | Treatment of acid mine drainage |
| CN106191442A (en) * | 2016-08-23 | 2016-12-07 | 金川集团股份有限公司 | A kind of method of nickel solution deeply purifying and removing silicon |
| CN106229482A (en) * | 2016-08-23 | 2016-12-14 | 兰州金川新材料科技股份有限公司 | A kind of method preparing ternary precursor for raw material with nickel cobalt mixed solution |
| CN106219581A (en) * | 2016-07-22 | 2016-12-14 | 中国科学院青海盐湖研究所 | A kind of method utilizing selection absorption method to prepare magnesium nitrate |
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| CN108517407A (en) * | 2018-05-22 | 2018-09-11 | 广西银亿新材料有限公司 | A kind of method for removing iron of red soil nickel ore leaching liquid |
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| CN104120259B (en) * | 2014-07-30 | 2016-03-02 | 广西师范大学 | A kind of nickel oxide ore pickling liquor two step method for removing iron |
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