CN102534206A - Leaching method of limonite type laterite-nickel ore - Google Patents
Leaching method of limonite type laterite-nickel ore Download PDFInfo
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Abstract
A method for leaching limonite type laterite-nickel ore, which relates to a process method for recovering nickel, cobalt and iron by processing the laterite-nickel ore by a wet method. The method is characterized by comprising the following steps: (1) grinding and pulping raw limonite laterite-nickel ore, and adding sulfuric acid for heating and pre-leaching; (2) adding Mg (NO) into the pre-soaked ore pulp3)2Heating and pressurizing to leach under stirring; (3) after leaching is finished, ore pulp is neutralized to remove iron and aluminum,separating to obtain leachate and leaching residues; (4) washing the leached slag to obtain a washing solution and iron-rich slag; and (3) neutralizing the leaching solution to precipitate nickel and cobalt to obtain nickel and cobalt hydroxide, and comprehensively recovering magnesium sulfate from the mother solution after nickel and cobalt separation through evaporation and crystallization. The method realizes the high-efficiency selective leaching of nickel and cobalt, the leaching rate can reach more than 90 percent, the leaching rate of iron is as low as less than 0.8 percent, and the iron-rich slag containing more than 55 percent of iron is obtained.
Description
Technical field
A kind of leaching method of brown iron type nickel laterite ore relates to the process method that a kind of wet processing red soil nickel ore reclaims nickel, cobalt and iron.
Background technology
Red soil nickel ore is the mineral of nickeliferous peridotites through the rotten formation of long-term weathering leaching, because the oxidation of iron takes on a red color ore after the weathering of mineral deposit, and is commonly referred to as red soil nickel ore.Can red soil nickel ore be divided into two types of brown iron type nickel laterite ore and noumeite type red soil nickel ores according to the content of iron, silicon, magnesium and nickel in the mineral deposit is different; In general; The former nickel grade is lower and the iron grade is higher, is fit to wet processing, and latter's nickel grade is higher relatively and the iron grade is relatively low; Be fit to pyrometallurgical smelting, and the former total resources is about latter's twice.Along with the continuous increase of China to nickel, cobalt and iron ore concentrate demand, how highly economical ground extracts nickel, cobalt from brown iron type nickel laterite ore, and comprehensive utilization iron wherein is significant.
At present, the brown iron type nickel laterite ore hydrometallurgy production technique of large-scale application mainly contains two kinds: reducing roasting-ammonia soaking technology and pressurized acid leaching technology.Reduction roasting-ammonia leaching technology is commonly used to handle and contains MgO greater than 10%, contains the not too complicated red soil nickel ore of Ni about 1% and Ni occurrence status.Though this process using normal pressure leaches, and has reduced equipment cost and handling cost, exists reducing atmosphere wayward, the fluctuation of nickel leaching yield is bigger, and the cobalt leaching yield is low, and ammonia is volatile, ferromagnetic to select deficiencies such as accumulation rate is low.Sulfuric acid pressurized acid leaching technology is suitable for handling and contains MgO less than 10%, particularly contains Ni less than 5% greater than 1.3% red soil nickel ore.The great advantage of this technology is that nickel, cobalt leaching yield are high, but the acid consumption becomes the maximum economic target of this technology of restriction.And the leaching of the content of magnalium and iron is relevant in acid consumption and the ore, thereby the control of iron becomes the key of this technology in the leaching process for the ore deposit of selecting.Exist with the form of magnetite because of the iron in the red soil nickel ore has part, promptly have the ferrous of a great deal of to be present in the ore deposit, can get into solution during leaching along with the dissolving of mineral and cause in the leach liquor iron level higher.Normally control the iron level in the leach liquor, but aerating oxygen not only higher requirement was proposed but also had increased Financial cost under the high-temperature and high-pressure conditions to device security through aerating oxygen or oxygen-rich air in autoclave.Nickel cobalt grade is higher, magnalium content is low and need not the leaching than strict control iron under the mild operating conditions of logical oxygen, promptly reduce Technological Economy property and the technological feasibility that acid consumption and operational condition could guarantee this acid leaching process simultaneously it is thus clear that have only.Many for this reason investigators have proposed different improvement projects to traditional sulfuric acid pressure leaching process.
Patent CN101139656 discloses a kind of laterite nickel ore leaching method, and this method adopts two sections leachings of pressurizeing, and at first brown iron type nickel laterite ore is carried out one section pressurization and leaches, and adds the vegetable mould ore deposit again, carries out two sections oxygenations, pressurization leaching.Though this method can be controlled the leaching of iron, there is the drawback of the logical oxygen of high pressure, the technical complexity that has increased technology is especially leached in two sections pressurizations.
Patent CN1676634 discloses a kind of pressure oxidation leaching-out method for nickel-cobalt oxide ore; This method does not directly adopt sulfuric acid to make leaching agent; But in autoclave, add SULPHUR POWDER slurry or sulphide concentrate slurry, generate with the oxygen reaction that feeds and leach required sulfuric acid, thereby nickel cobalt in the ore deposit is leached.Though this patent has reduced sour consumption, but still need logical oxygen under HTHP, higher to equipment requirements.
Patent CN1995414 discloses the vitriol intensified leach extraction method of nickel oxide ore; This method adds autoclave with the broken mill of raw ore back; And in autoclave, adding the reductive agent leaching of pressurizeing, temperature of reaction has obtained higher leaching yield below pressure 1.6 MPa below 200 ℃.Though this method is lower than conventional pressure leaching process equipment requirements, technological easy master, foreign matter content is higher in the leach liquor that obtains, and follow-up purification process is difficult, the recycling of this method and not mentioned iron in addition, economy is bad.
To sum up; The process modification of more than carrying out to the red soil nickel ore of different content or exist the logical oxygen of HTHP to equipment requirements is high, Financial cost is high and drawback such as Technology complicacy; Or exist the low and selectivity of recovery rate of valuable metals bad etc. not enough, all fail good comprehensive to utilize brown iron type nickel laterite ore.Therefore, exploitation is a kind of is of great practical significance than the good pressure leaching process of processing brown iron type nickel laterite ore and metal leaching selectivity under the mild conditions.
Summary of the invention
The object of the invention is exactly the problem that exists to prior art, a kind of logical oxygen of HTHP or oxygen-rich air of need not is provided, the leaching method of the brown iron type nickel laterite ore of valuable metal elemental nickel, cobalt and iron in the ability good use ore deposit.
Above-mentioned purpose realizes through following scheme.
A kind of leaching method of brown iron type nickel laterite ore is characterized in that the step of its technological process comprises:
(1) after the brown iron type nickel laterite ore raw ore is levigate, the slurrying, adds sulfuric acid and heat preextraction;
(2) ore pulp after the preimpregnation is added Mg (NO
3)
2, under agitation carry out heating and pressurizing and leach;
(3) leach to finish after, ore pulp through in deironing aluminium after, separation obtaining leach liquor and leached mud;
(4) leached mud gets washings and rich scum after washing; Leach liquor obtains the nickel cobalt hydroxide through the heavy nickel cobalt that neutralizes, and the mother liquor behind the separating nickel cobalt is through the comprehensive sal epsom that reclaims wherein of evaporative crystallization.
The leaching method of a kind of brown iron type nickel laterite ore of the present invention; It is characterized in that principal element quality percentage composition is in the described brown iron type nickel laterite ore raw ore of step (1): total iron ∑ Fe 40%～50%, wherein ferrous Fe (II) 1.0～25%, nickel 0.5%～2.0%; Cobalt Co 0.01%～0.2%; Magnesium Mg 0.3%～5%, aluminium Al 0.5%～3%, silicon SiO
23%～10%.
The leaching method of a kind of brown iron type nickel laterite ore of the present invention; The levigate process that it is characterized in that said step (1) is wet-milling; The ratio that granularity accounts for whole ore deposits amount less than the ore deposit of 74 μ m after the wet-milling is greater than 70%, after the slurrying in the ore pulp mass concentration of brown iron type nickel laterite ore be 20%～50%.
The leaching method of a kind of brown iron type nickel laterite ore of the present invention is characterized in that the sulfuric acid that adds in the said step (1) is the vitriol oil, and add-on is 200～450 kg/t butt ore deposits.
The leaching method of a kind of brown iron type nickel laterite ore of the present invention is characterized in that the temperature of the heating preextraction process of said step (1) is 60～90 ℃, time 0.5～1.5 h.
The leaching method of a kind of brown iron type nickel laterite ore of the present invention is characterized in that the gas of the heating and pressurizing leaching process generation of said step (2) absorbs with the MgO slurry, absorbs back liquid and returns step (2).
The leaching method of a kind of brown iron type nickel laterite ore of the present invention is characterized in that the Mg (NO of described step (2)
3)
2Total add-on is 2～80 kg/t butt ore deposits.
The leaching method of a kind of brown iron type nickel laterite ore of the present invention, the extraction temperature that it is characterized in that described step (2) is 200～280 ℃; Leaching pressure is 1.5～6.5Mpa; Extraction time is 0.5～5 h.
The leaching method of a kind of brown iron type nickel laterite ore of the present invention is characterized in that the leaching liquid-solid ratio 1:1～6:1 ml/g of described step (2).
The leaching method of a kind of brown iron type nickel laterite ore of the present invention is characterized in that the MgO mass concentration in the MgO slurry that gas that described absorption heating and pressurizing leaching process produces uses is 15%～30%.
The leaching method of a kind of brown iron type nickel laterite ore of the present invention, it is characterized in that described step (3) adopt the MgO slurry carry out in deironing aluminium, the mass concentration of MgO slurry is 15%～30%, transfers slurry pH to 3.8～4.0 during deironing aluminium.
The leaching method of a kind of brown iron type nickel laterite ore of the present invention is characterized in that the leached mud washing process of described step (4) adopts the washing of 5～8 stage countercurrents, washing liquid-solid ratio 2:1～4:1 ml/g.
The leaching method of a kind of brown iron type nickel laterite ore of the present invention is characterized in that it is that 15%～40%MgO starches the heavy nickel cobalt that neutralizes that described step (4) adopts MgO dry powder or mass concentration, transfers slurry pH to 7.8～8.0 when sinking the nickel cobalt.。
Method of the present invention is a raw material with the brown iron type nickel laterite ore, adopts ore pulp preextraction-efficient selective pressurization leaching-Mg (NO
3)
2Recycle wherein valuable element nickel, cobalt and iron with the novel process of heavy nickel cobalt in reprocessing cycle-leach liquor.Abundant for reserves but brown iron type nickel laterite ore that always be not fully utilized provides a kind of novel process thinking of economic low-carbon (LC).With existing brown iron type nickel laterite ore technology contrast, can find following advantage:
(1) one section leaching system that leaches and need not logical oxygen of pressurizeing makes the technology easy operation control, and reagent consumption is little, and Financial cost is lower;
(2) it is good to leach selectivity, and nickel, cobalt leaching yield are all greater than 90%, and the iron leaching yield not only helps the iron enrichment less than 0.8%, the loss of nickel cobalt when also having reduced follow-up removal of impurities.
(3) additive Mg (NO
3)
2Renewable, reduced the consuming cost of technology.
(4) the iron comprehensive utilization ratio is high, and the leached mud iron level can reach more than 55%, can be used for blast furnace ironmaking.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
A kind of leaching method of brown iron type nickel laterite ore, operation may further comprise the steps:
(1) with the broken mill of brown iron type nickel laterite ore raw ore, and is made into certain density ore pulp, adds a certain amount of vitriol oil, heat preimpregnation then;
(2) add a certain amount of Mg (NO after the preimpregnation
3)
2Regenerated liquid is if deficiency is then added a certain amount of solid Mg (NO
3)
2, be warming up to design temperature after, under high-temperature and high-pressure conditions, leach certain hour;
(3) after leaching finishes, discharge gas reactor and starch absorption with MgO, absorption liquid returns step (2); Leach ore pulp and add among the MgO and deironing aluminium, dense afterwards separation obtains leach liquor and leached mud, leached mud through dense wash washings and rich scum, washings returns the broken grinder preface of step (1);
(4) leach liquor obtains the nickel cobalt hydroxide through the heavy nickel cobalt that neutralizes, and the mother liquor behind the separating nickel cobalt is through the comprehensive MgSO that reclaims wherein of evaporative crystallization
4, evaporated liquor then returns step (3) washing procedure.
Embodiment 1
Raw ore obtains particle diameter and accounts for 75% red soil nickel ore less than 74 μ m after fragmentation, wet-milling, the ore pulp mass concentration is 30%, adds the vitriol oil of massfraction 98%, and adding the acid amount is 350 kg/t butt ore deposits, is heated to 80 ℃, preimpregnation 1 h; Preimpregnation finishes the back and adds the magnesium nitrate solid, and add-on is 60 kg/t butt ore deposits, is warmed up to 230 ℃ of leachings of pressurizeing then; Leaching pressure is 2.5 Mpa, and extraction time is 5 h, and liquid-solid ratio is 3:1 ml/g; Mixing speed is 500 rpm; Wherein the nickel leaching yield 91.2%, cobalt leaching yield 92.4%, and the iron leaching yield then is low to moderate 0.5%; Gas reactor use mass concentration is 20% Natural manganese dioxide slurry absorption; Leaching ore pulp use mass concentration is 20% Natural manganese dioxide slurry adjust pH to 4.0; After 5 grades of dense washings of dense separation and liquid-solid ratio 4:1 ml/g, get rich scum, leach liquor and washings, wherein rich scum iron content 56.6% then; The use mass concentration is 40% Natural manganese dioxide slurry accent pH of leaching solution to 8.0; Nickel cobalt to wherein carries out neutralization precipitation, gets nickel hydroxide cobalt slag and mother liquor, and mother liquor gets magnesium sulfate crystals and evaporated liquor behind evaporative crystallization; Evaporated liquor returns dense washing procedure, and washings then returns brokenly the grinder preface.
Raw ore obtains particle diameter and accounts for 78% red soil nickel ore less than 74 μ m after fragmentation, wet-milling, the ore pulp mass concentration is 42%, adds the vitriol oil of massfraction 98%, and adding the acid amount is 260 kg/t butt ore deposits, is heated to 75 ℃, preimpregnation 1.0 h; Preimpregnation finishes the back and adds regeneration magnesium nitrate solution and magnesium nitrate solid, amounts to the total add-on of magnesium nitrate solid 70 kg/t butt ore deposits, is warmed up to 220 ℃ of leachings of pressurizeing then; Leaching pressure is 2.5 Mpa, and extraction time is 2 h, and liquid-solid ratio is 2:1 ml/g; Mixing speed is 500 rpm; Wherein the nickel leaching yield 90.7%, cobalt leaching yield 91.0%, and the iron leaching yield then is low to moderate 0.4%; Gas reactor use mass concentration is 18% Natural manganese dioxide slurry absorption; Leaching ore pulp use mass concentration is 20% Natural manganese dioxide slurry adjust pH to 4.0; After 6 grades of dense washings of dense separation and liquid-solid ratio 3:1 ml/g, get rich scum, leach liquor and washings, wherein rich scum iron content 55.5% then; Transfer pH of leaching solution to 7.8 with dry powder Natural manganese dioxide, wherein nickel cobalt carried out neutralization precipitation, nickel hydroxide cobalt slag and mother liquor, mother liquor behind evaporative crystallization magnesium sulfate crystals and evaporated liquor, evaporated liquor returns dense washing procedure, washings then returns brokenly the grinder preface.
Embodiment 3
Raw ore obtains particle diameter and accounts for 85% red soil nickel ore less than 74 μ m after fragmentation, wet-milling, the ore pulp mass concentration is 20%, adds the vitriol oil of massfraction 98%, and adding the acid amount is 450 kg/t butt ore deposits, is heated to 60 ℃, preimpregnation 0.5 h; Preimpregnation finishes the back and adds regeneration magnesium nitrate solution and magnesium nitrate solid, amounts to the total add-on of magnesium nitrate solid 80 kg/t butt ore deposits, is warmed up to 200 ℃ of leachings of pressurizeing then; Leaching pressure is 1.8 Mpa, and extraction time is 3 h, and liquid-solid ratio is 6:1 ml/g; Mixing speed is 800 rpm; Wherein the nickel leaching yield 94.2%, cobalt leaching yield 95.4%, and the iron leaching yield then is low to moderate 0.8%; Gas reactor use mass concentration is 30% Natural manganese dioxide slurry absorption; Leaching ore pulp use mass concentration is 30% Natural manganese dioxide slurry adjust pH to 3.8; After 6 grades of dense washings of dense separation and liquid-solid ratio 2:1 ml/g, get rich scum, leach liquor and washings, wherein rich scum iron content 57.1% then; Transfer pH of leaching solution to 7.8 with dry powder Natural manganese dioxide, wherein nickel cobalt carried out neutralization precipitation, nickel hydroxide cobalt slag and mother liquor, mother liquor behind evaporative crystallization magnesium sulfate crystals and evaporated liquor, evaporated liquor returns dense washing procedure, washings then returns brokenly the grinder preface.
Embodiment 4
Raw ore obtains particle diameter and accounts for 80% red soil nickel ore less than 74 μ m after fragmentation, wet-milling, the ore pulp mass concentration is 40%, adds the vitriol oil of massfraction 98%, and adding the acid amount is 300 kg/t butt ore deposits, is heated to 70 ℃, preimpregnation 1.5 h; Preimpregnation finishes the back and adds the regeneration magnesium nitrate solution, amounts to magnesium nitrate solid add-on 40 kg/t butt ore deposits, is warmed up to 260 ℃ of leachings of pressurizeing then; Leaching pressure is 4.8 Mpa, and extraction time is 1 h, and liquid-solid ratio is 3:1 ml/g; Mixing speed is 600 rpm; Wherein the nickel leaching yield 91.2%, cobalt leaching yield 91.4%, and the iron leaching yield then is low to moderate 0.4%; Gas reactor use mass concentration is 25% Natural manganese dioxide slurry absorption; Leaching ore pulp use mass concentration is 20% Natural manganese dioxide slurry adjust pH to 4.0; After 7 grades of dense washings of dense separation and liquid-solid ratio 3:1 ml/g, get rich scum, leach liquor and washings, wherein rich scum iron content 55.9% then; Transfer pH of leaching solution to 8.0 with dry powder Natural manganese dioxide, wherein nickel cobalt carried out neutralization precipitation, nickel hydroxide cobalt slag and mother liquor, mother liquor behind evaporative crystallization magnesium sulfate crystals and evaporated liquor, evaporated liquor returns dense washing procedure, washings then returns brokenly the grinder preface.
Embodiment 5
Raw ore obtains particle diameter and accounts for 70% red soil nickel ore less than 74 μ m after fragmentation, wet-milling, the ore pulp mass concentration is 50%, adds the vitriol oil of massfraction 98%, and adding the acid amount is 200 kg/t butt ore deposits, is heated to 90 ℃, preimpregnation 1.5 h; Preimpregnation finishes the back and adds the magnesium nitrate solid, and add-on is 50 kg/t butt ore deposits, is warmed up to 280 ℃ of leachings of pressurizeing then; Leaching pressure is 6.5 Mpa, and extraction time is 0.5 h, and liquid-solid ratio is 2:1 ml/g; Mixing speed is 400 rpm; Wherein the nickel leaching yield 90.2%, cobalt leaching yield 90.4%, and the iron leaching yield then is low to moderate 0.2%; Gas reactor use mass concentration is 15% Natural manganese dioxide slurry absorption; Leaching ore pulp use mass concentration is 15% Natural manganese dioxide slurry adjust pH to 3.8; After 8 grades of dense washings of dense separation and liquid-solid ratio 3:1 ml/g, get rich scum, leach liquor and washings, wherein rich scum iron content 55.8% then; The use mass concentration is 15% Natural manganese dioxide slurry accent pH of leaching solution to 8.0; Nickel cobalt to wherein carries out neutralization precipitation, gets nickel hydroxide cobalt slag and mother liquor, and mother liquor gets magnesium sulfate crystals and evaporated liquor behind evaporative crystallization; Evaporated liquor returns dense washing procedure, and washings then returns brokenly the grinder preface.
Claims (13)
1. the leaching method of a brown iron type nickel laterite ore is characterized in that the step of its technological process comprises:
(1) after the brown iron type nickel laterite ore raw ore is levigate, the slurrying, adds sulfuric acid and heat preextraction;
(2) ore pulp after the preimpregnation is added Mg (NO
3)
2, under agitation carry out heating and pressurizing and leach;
(3) leach to finish after, ore pulp through in deironing aluminium after, separation obtaining leach liquor and leached mud;
(4) leached mud gets washings and rich scum after washing; Leach liquor obtains the nickel cobalt hydroxide through the heavy nickel cobalt that neutralizes, and the mother liquor behind the separating nickel cobalt is through the comprehensive sal epsom that reclaims wherein of evaporative crystallization.
2. the leaching method of a kind of brown iron type nickel laterite ore according to claim 1; It is characterized in that principal element quality percentage composition is in the described brown iron type nickel laterite ore raw ore of step (1): total iron ∑ Fe 40%～50%, wherein ferrous Fe (II) 1.0～25%, nickel 0.5%～2.0%; Cobalt Co 0.01%～0.2%; Magnesium Mg 0.3%～5%, aluminium Al 0.5%～3%, silicon SiO
23%～10%.
3. the leaching method of a kind of brown iron type nickel laterite ore according to claim 1; The levigate process that it is characterized in that said step (1) is wet-milling; The ratio that granularity accounts for whole ore deposits amount less than the ore deposit of 74 μ m after the wet-milling is greater than 70%, after the slurrying in the ore pulp mass concentration of brown iron type nickel laterite ore be 20%～50%.
4. the leaching method of a kind of brown iron type nickel laterite ore according to claim 1 is characterized in that the sulfuric acid that adds in the said step (1) is the vitriol oil of mass concentration 98%, and add-on is 200～450 kg/t butt ore deposits.
5. the leaching method of a kind of brown iron type nickel laterite ore according to claim 1 is characterized in that the temperature of the heating preextraction process of said step (1) is 60～90 ℃, time 0.5～1.5 h.
6. the leaching method of a kind of brown iron type nickel laterite ore according to claim 1 is characterized in that the gas of the heating and pressurizing leaching process generation of said step (2) absorbs with the MgO slurry, absorbs back liquid and returns step (2).
7. the leaching method of a kind of brown iron type nickel laterite ore according to claim 1 is characterized in that the Mg (NO of described step (2)
3)
2Total add-on is 2～80 kg/t butt ore deposits.
8. the leaching method of a kind of brown iron type nickel laterite ore according to claim 1, the extraction temperature that it is characterized in that described step (2) is 200～280 ℃; Leaching pressure is 1.5～6.5Mpa; Extraction time is 0.5～5 h.
9. the leaching method of a kind of brown iron type nickel laterite ore according to claim 1, the leaching liquid-solid ratio that it is characterized in that described step (2) is 1:1～6:1 ml/g.
10. the leaching method of a kind of brown iron type nickel laterite ore according to claim 6 is characterized in that the MgO mass concentration in the MgO slurry that gas that described absorption heating and pressurizing leaching process produces uses is 15%～30%.
11. the leaching method of a kind of brown iron type nickel laterite ore according to claim 1, it is characterized in that described step (3) adopt the MgO slurry carry out in deironing aluminium, the mass concentration of MgO slurry is 15%～30%.
12. the leaching method of a kind of brown iron type nickel laterite ore according to claim 1 is characterized in that the leached mud washing process of described step (4) adopts the washing of 5～8 stage countercurrents, the washing liquid-solid ratio is 2:1～4:1 ml/g.
13. the leaching method of a kind of brown iron type nickel laterite ore according to claim 1 is characterized in that it is that 15%～40%MgO starches the heavy nickel cobalt that neutralizes that described step (4) adopts MgO dry powder or mass concentration.
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| CN115125393A (en) * | 2022-06-21 | 2022-09-30 | 四川顺应动力电池材料有限公司 | Low-carbon treatment method for acid-base recycling of limonite type laterite-nickel ore |
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