CN104775027A - Method for recovering nickel, iron, silicon and magnesium from low grade laterite-nickel ore - Google Patents

Method for recovering nickel, iron, silicon and magnesium from low grade laterite-nickel ore Download PDF

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CN104775027A
CN104775027A CN201410845470.8A CN201410845470A CN104775027A CN 104775027 A CN104775027 A CN 104775027A CN 201410845470 A CN201410845470 A CN 201410845470A CN 104775027 A CN104775027 A CN 104775027A
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nickel
composition
pressure leaching
silicon
solid
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王永前
刘玉强
杨志强
许永武
王少华
刘世和
赵志虎
沙滨
李正禄
马永刚
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Jinchuan Group Co Ltd
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Jinchuan Group Co Ltd
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Abstract

The invention relates to a method for recovering nickel, iron, silicon and magnesium from low grade laterite-nickel ore, and relates to the technical field of wet metallurgy. The method has the following advantage: iron and silicon in the low grade laterite-nickel ore can be effectively recovered when nickel is obtained, and the recovered iron and silicon can be reused or used in smelting only through simple treatment; magnesium oxide as an intermediate reaction product can also be effectively recovered, so the waste of the intermediate reaction product is avoided; the method disclosed in the invention has lower apparatus requirements, lower reaction material temperature requirement and lower reaction environment pressure requirement than a high pressure acid leaching method; and nickel and cobalt are mutually associated metals, refined nickel contains a certain amount of cobalt, and cobalt associated in nickel can be recovered in a hydroxide manner, so later stage nickel purification and cobalt separation are convenient.

Description

A kind of method reclaiming nickel, iron, silicon and magnesium from low-grade laterite nickel ore
Technical field
The present invention relates to technical field of wet metallurgy, specifically a kind of method reclaiming nickel, iron, silicon and magnesium from low-grade laterite nickel ore.
Background technology
Low-grade laterite nickel ore refers to the native nickel minerals mixing and have large volume nugget and breeze in small, broken bits, and native nickel minerals is rich in the elements such as nickel, iron, silicon, to the smelting of laterite mainly based on thermal process and the large class of wet processing two.During fire metallurgy process process laterite, usually can only produce ferronickel, can not silicon be reclaimed.And existing wet processing heap Leaching leaching yield is lower, be only applicable to the laterite processing high Mg content.Need in existing wet processing to carry out in Ore Leaching to ore pulp, treatment process is divided into normal pressure to heat acidleach and high pressure-temperature acidleach, normal pressure is heated in the leach liquor that produces after acidleach containing each metal ion species, later separation operation becomes complicated, need a large amount of sulfuric acid for acidleach, the usage quantity of the vitriol oil is more than 3 times of acidleach thing simultaneously; Although high pressure-temperature acidleach is less with acid, but need the vitriol oil to be heated to more than 300 DEG C, react under the condition of force value 50MPa, under high temperature, condition of high voltage, the metalliferous mineral in ore almost dissolves completely, and the requirement of whole acidleach process to reactor is high, simultaneously the method a large amount of slags that can generate, in slag, iron can not be separated completely with silicon, cannot recycle, and can only work as waste disposal.
Summary of the invention
Main purpose of the present invention is to provide a kind of method reclaiming nickel, iron, silicon and magnesium from low-grade laterite nickel ore, the pressure that the method effectively can overcome vitriol oil large usage quantity in prior art, the vitriol oil needs heat, reaction process needs are higher, the problem that after reaction, in slag, iron silicon cannot be separated completely.
In order to solve the problem, present invention employs a kind of method reclaiming nickel, iron, silicon and magnesium from low-grade laterite nickel ore, the method comprises the following steps.
1 washing classification: with 80 orders for washing grade scale is to low-grade laterite nickel ore washing classification, obtains more than 80 Large stone compared with breeze in small, broken bits below nugget and 80 orders.
2 prepare ore pulp: Large stone washing in step 1 gone out grinds to form the powder of below 80 orders compared with nugget, mix, obtain one-level ore pulp with the volume mass of water with solid matter 0.8 ~ 1.5:1 than by water with the powder of grinding; Mix with the breeze in small, broken bits that washing in step 1 is gone out than Jiang Shui with the volume mass of solid matter 0.8 ~ 1.5:1 with water, obtain secondary ore pulp.
3 vitriol oil normal pressure leaching and solid-liquid separation, reclaim silicon: the one-level ore pulp of preparation in step 2 is heated to 60 ~ 90 DEG C, the vitriol oil is heated to 100 ~ 180 DEG C.The one-level ore pulp of heating and the vitriol oil are passed into steel lining alloy reaction tank react, until form cellular lotion.Water is mixed with the ratio of 1 ~ 1.5:1 with cellular lotion, at the uniform velocity stirs 20 ~ 70 minutes, obtain mixing solutions.Carry out solid-liquid separation to mixing solutions, obtain normal pressure leaching slag A and normal pressure leaching liquid B, described normal pressure leaching slag A is silicon-dioxide.
4 normal pressure leaching liquid B pressure leaching and solid-liquid separation: by normal pressure leaching liquid B with add compressive reaction still to secondary ore pulp with the volume ratio of 1:2 ~ 3 and react, temperature of reaction maintains 150 ~ 240 DEG C; Reaction continues 30 ~ 60 minutes; PH value maintains between 0.5 ~ 1.5; Reaction pressure maintains 1.5 ~ 4Mpa.Solid-liquid separation is carried out to reacted solution, obtains pressure leaching slag C and pressureleaching solution D.
5 reclaim iron: the basic solution with 10% washs pressure leaching slag C.Drying and processing is carried out to the solid particulate after washing, obtains Iron concentrate particle.
6 reclaim nickel: in pressureleaching solution D, add magnesium oxide react, until pH value maintains between 7 ~ 8; Solid-liquid separation is carried out to reacted solution, obtains nickel hydroxide solid particulate and Adlerika; Conventional processing is carried out to nickel hydroxide solid particulate and can obtain nickel.
7 reclaim magnesium: carry out evaporative crystallization to the Adlerika produced in step 6, obtain solid sulphuric acid magnesium granules.
In step 3 use sulfuric acid with pulp volume than 0.8 ~ 1.8:1.
Of the present inventionly effectively to be: while acquisition nickel, can iron in efficient recovery low-grade laterite nickel ore and silicon, the iron of recovery and silicon only need simple process just can again utilize or smelt.Of the present inventionly can also be used as the magnesium oxide of intermediate reaction thing by efficient recovery, avoid the waste of intermediate reaction thing.Relatively for high pressure acid leaching process, the requirement to equipment of the present invention is low, low to reactant feed temperature requirement, low to reaction environment pressure requirements.Because nickel cobalt is mutual associated metal, while refinement nickel, also mix and have a certain amount of cobalt, the present invention can reclaim the cobalt of association in nickel in the lump, and is all reclaim with the form of oxyhydroxide, facilitates the purification of later stage nickel and the separation of cobalt.
Accompanying drawing explanation
Fig. 1 is FB(flow block) of the present invention.
Specifically mode
Below in conjunction with specific embodiment, the present invention will be further described.The 1# ore used in following example is from laterite mineral deposit, New Caledonia, and washing classification obtains 2# and 3# ore; 4# ore is from Indonesia's laterite mineral deposit, and washing classification obtains 5# and 6# ore.The main component of ore is in table 1.
Table 1 laterite component list
Numbering Ore type Ni(％) Co(％) Fe(％) MgO(％) SiO 2(％))
1# New noise made in coughing or vomiting laterite 1.25 0.14 45.84 0.27 8.43
2# Xin Kagao silicon magnesium ore deposit 1.56 0.07 16.72 11.36 33.60
3# New noise made in coughing or vomiting low silicon magnesium ore deposit 1.17 0.16 49.28 0.14 2.48
4# Indonesia's laterite 1.38 0.21 43.37 0.31 10.38
5# Indonesia's height silicon magnesium ore deposit 1.62 0.14 15.87 8.07 38.76
6# Indonesia's low silicon magnesium ore deposit 1.32 0.08 47.33 0.23 2.14
Embodiment 1
1 washing classification.
For washing grade scale, washing classification is carried out to 1# with 80 orders, obtain the 2# of more than 80; 3# below 80 orders.
2 prepare ore pulp.
Take the 2# of 500kg weight, be mixed to get one-level ore pulp with the water of 500L;
3 vitriol oil normal pressure leaching and solid-liquid separation, reclaim silicon.
The one-level ore pulp of preparation in step 2 is heated to 90 DEG C, the vitriol oil is heated to 180 DEG C;
The one-level ore pulp of heating and the vitriol oil are passed into steel lining alloy reaction tank react, react after 10 minutes, in steel lining alloy reaction tank, loose cellular lotion can be formed;
The water adding 1500kg in steel lining alloy reaction tank mixes with cellular lotion, at the uniform velocity stirs 20 minutes, obtains mixing solutions.Mixing solutions is pumped into plate-and-frame filter press and carry out solid-liquid separation and residue washing, obtain 205Kg normal pressure leaching slag A 1, 1450L normal pressure leaching liquid B 1, 1150L washings E 1(wherein normal pressure acidleach filter residue A 1, normal pressure acidleach liquor B 1, washings E 1composition in Table 1-1, table 1-2, table 1-3).
Get 300g normal pressure leaching slag A 1carry out hydrocyclone separation technology, obtain the silicon dioxide powder H being less than the heavy 144g of 100 orders 1and be greater than the fine sand I of the heavy 149g of 100 orders 1(silicon dioxide powder H 1with fine sand I 1composition is in Table 1-8 and table 1-9).
4 normal pressure leaching liquid B 1pressure leaching and solid-liquid separation.
Get the 3# of 4000g, add 8000ml washings E 1be prepared into secondary ore pulp, washings E 1water content is about more than 90%.The secondary ore pulp prepared being passed into volume is that the PARR4557 of 17L pressurizes in anti-still, afterwards again to the normal pressure acidleach liquor B adding 3000ml during PARR4557 pressurizes anti-still 1.Temperature of reaction maintains 240 DEG C, and reaction continues 30 minutes, and pH value maintains between 1.5; Reaction pressure maintains 4Mpa.From autoclave, shift out reaction paste after being cooled to 80 DEG C carry out solid-liquid separation and wash filter residue, obtain 3550g pressure leaching slag C 1, 9400ml pressureleaching solution D 1, 5480ml washings F 1(pressure leaching slag C 1, pressureleaching solution D 1with washings F 1composition in Table 1-4, table 1-5 and table 1-6).
5 reclaim iron.
Get 300g pressure leaching slag C 1add and fill 1000ml, concentration is in the beaker of 10% sodium carbonate solution, is heated to 60 DEG C and stirs 30 minutes.Solid-liquid separation washing leaching cake, oven dry, obtain 290g rhombohedral iron ore G 1(rhombohedral iron ore G 1composition is in Table 1-7).
6 reclaim nickel.
Get 500ml pressureleaching solution D 1put into beaker, stir and heating in water bath to 85 DEG C, slowly add 30% milk of magnesia adjust ph to 8 afterwards, stablize after 45 minutes and filter and washing leaching cake, obtain 6.93g nickel hydroxide (cobalt) J 1nickel (cobalt) liquid K is afterwards sunk with 490ml 1(nickel hydroxide (cobalt) J 1with heavy nickel (cobalt) liquid K afterwards 1composition is in Table 1-10 and table 1-11).
7 reclaim magnesium.
Get 450ml and sink liquid K after nickel 1put into beaker, stir and heating in water bath, mixing speed 250r/min, it is 80 DEG C that temperature controls.Add 5%NaClO solution and instill milk of magnesia adjust ph in 7 scopes.Alternate operation repeatedly, when instilling NaClO solution again, when pH value goes up not down, continue heating and within 1 hour, make Manganse Dioxide crystal grow up, pH value is finally 7.5.Be cooled to after room temperature and filter and washing leaching cake, obtain liquid 450ml after manganese dioxide precipitate demanganization.To liquid condensing crystal after demanganization and separation of lowering the temperature, obtain 75g magnesium sulfate L 1with system tail washings (magnesium sulfate L 1composition is in Table 1-12).
Based on the component content of residue, calculate nickel, cobalt leaching yield, slag rate and acid consumption data as follows: normal pressure acidleach nickel leaching yield: 98.51%; Normal pressure acidleach cobalt leaching yield: 96.83; Pressure leaching nickel leaching yield: 95.66%; Pressure leaching cobalt leaching yield: 92.73; Amount to nickel leaching yield 96.38%; Cobalt leaching yield 93.10%; Iron recovery >96%; Sulfuric acid consumption: 200Kg sulfuric acid/t ore deposit; Amount to slag rate: 41g white residue/1000g laterite.
Table 1-1 normal pressure acidleach filter residue A 1composition cartogram
Composition Ni Co Fe MgO SiO 2
Content (%) 0.057 0.005 1.04 2.03 81.95
Table 1-2 normal pressure acidleach liquor B 1composition cartogram
Composition Ni Co Fe MgO
Content (g/L) 3.96 0.17 42.13 27.21
Table 1-3 washings E 1composition cartogram
Composition Ni Co Fe MgO Composition Ni
Content (g/L) 1.63 0.07 17.73 11.40 Content (g/L) 1.63
Table 1-4 pressure leaching slag C 1composition cartogram
Composition Ni Co Fe MgO SiO 2 S
Content (%) 0.057 0.013 63.10 0.022 2.794 1.073
Table 1-5 pressure leaching filtrate D 1composition cartogram
Composition Ni Co Fe MgO
Content (g/L) 5.93 0.73 1.67 15.11
Table 1-6 washings F 1composition cartogram
Composition Ni Co Fe MgO
Content (g/L) 2.54 0.26 1.26 6.68
Table 1-7 rhombohedral iron ore G 1composition cartogram
Composition Ni Co Fe MgO SiO 2
Content (%) 0.061 0.009 64.12 0.018 2.684
Table 1-8 silicon dioxide powder H 1composition cartogram
Composition Ni Co Fe MgO SiO 2
Content (%) 0.053 0.006 1.012 2.145 94.118
table 1-9 fine sand I 1composition cartogram
Composition Ni Co Fe MgO SiO 2
Content (%) 0.062 0.008 1.117 3.158 77.343
Table 1-10 nickel hydroxide (cobalt) J 1composition cartogram
Composition Ni Co Fe MgO
Content (%) 42.38 5.13 0.79 2.34
Table 1-11 sinks liquid K after nickel 1composition cartogram
Composition Ni Co Fe MgO
Content (g/L) 0.024 0.006 0.002 25.36
Table 1-12 magnesium sulfate L 1composition cartogram
Composition Ni Co Fe MgO
Content (%) 0.025 0.003 0.002 15.11
embodiment 2
1 washing classification.
For washing grade scale, washing classification is carried out to 4# with 80 orders, obtain the 5# of more than 80; 6# below 80 orders.
2 prepare ore pulp.
Take the 5# of 500kg weight, be mixed to get one-level ore pulp with the water of 500L;
3 vitriol oil normal pressure leaching and solid-liquid separation, reclaim silicon.
The one-level ore pulp of preparation in step 2 is heated to 60 DEG C, the vitriol oil is heated to 100 DEG C;
The one-level ore pulp of heating and the vitriol oil are passed into normal pressure duplex reactor be uniformly mixed;
The one-level ore pulp of heating and the vitriol oil are passed into steel lining alloy reaction tank react, react after 10 minutes, in steel lining alloy reaction tank, loose cellular lotion can be formed;
The water adding 1500kg in steel lining alloy reaction tank mixes with cellular lotion, at the uniform velocity stirs 70 minutes, obtains mixing solutions.Mixing solutions is pumped into plate-and-frame filter press and carry out solid-liquid separation and residue washing, obtain 230Kg normal pressure leaching slag A 2, 1400L normal pressure leaching liquid B 2, 1180L washings E 2(wherein normal pressure acidleach filter residue A 2, normal pressure acidleach liquor B 2, washings E 2composition in Table 2-1, table 2-2, table 2-3).
Get 300g normal pressure leaching slag A 2carry out hydrocyclone separation technology, obtain the silicon dioxide powder H being less than the heavy 156g of 100 orders 2and be greater than the fine sand I of the heavy 138g of 100 orders 2(silicon dioxide powder H 2with fine sand I 2composition is in Table 2-8 and table 2-9).
4 normal pressure leaching liquid B 1pressure leaching and solid-liquid separation.
Get the 6# of 4000g, add 8000ml washings E 2be prepared into secondary ore pulp, washings E 2water content is about more than 90%.The secondary ore pulp prepared being passed into volume is that the PARR4557 of 17L pressurizes in anti-still, afterwards again to the normal pressure acidleach liquor B adding 3000ml during PARR4557 pressurizes anti-still 2.Temperature of reaction maintains 150 DEG C, and reaction continues 60 minutes, and pH value maintains between 0.5; Reaction pressure maintains 1.5Mpa.From autoclave, shift out reaction paste after being cooled to 80 DEG C carry out solid-liquid separation and wash filter residue, obtain 3565g pressure leaching slag C 2, 9500ml pressureleaching solution D 2, 5500ml washings F 2(pressure leaching slag C 2, pressureleaching solution D 2with washings F 2composition in Table 2-4, table 2-5 and table 2-6).
5 reclaim iron.
Get 300g pressure leaching slag C 2add and fill 1000ml, concentration is in the beaker of 10% sodium carbonate solution, is heated to 60 DEG C and stirs 30 minutes.Solid-liquid separation washing leaching cake, oven dry, obtain 294g rhombohedral iron ore G 2(rhombohedral iron ore G 2composition is in Table 2-7).
6 reclaim nickel.
Get 500ml pressureleaching solution D 2put into beaker, stir and heating in water bath to 85 DEG C, slowly add 30% milk of magnesia adjust ph to 8 afterwards, stablize after 45 minutes and filter and washing leaching cake, obtain 7.39g nickel hydroxide (cobalt) J 2nickel (cobalt) liquid K is afterwards sunk with 500ml 2(nickel hydroxide (cobalt) J 2with heavy nickel (cobalt) liquid K afterwards 2composition is in Table 2-10 and table 2-11).
7 reclaim magnesium.
Get 450ml and sink liquid K after nickel 2put into beaker, stir and heating in water bath, mixing speed 250r/min, it is 80 DEG C that temperature controls.Add 5%NaClO solution and instill milk of magnesia adjust ph in 7 scopes.Alternate operation repeatedly, when instilling NaClO solution again, when pH value goes up not down, continue heating and within 1 hour, make Manganse Dioxide crystal grow up, pH value is finally 7.5.Be cooled to after room temperature and filter and washing leaching cake, obtain liquid 450ml after manganese dioxide precipitate demanganization.To liquid condensing crystal after demanganization and separation of lowering the temperature, obtain 75g magnesium sulfate L 2with system tail washings (magnesium sulfate L 2composition is in Table 2-12).
Normal pressure acidleach nickel leaching yield: 97.63%; Normal pressure acidleach cobalt leaching yield: 95.47%.Pressure leaching nickel leaching yield: 94.57%; Pressure leaching cobalt leaching yield: 93.16%.Amount to nickel leaching yield 95.29%; Cobalt leaching yield 93.04%.Iron recovery >96%.Sulfuric acid consumption: 200Kg sulfuric acid/t ore deposit.Amount to slag rate: 92.0g white residue/1000g laterite.
Table 2-1 normal pressure acidleach filter residue (A 2) composition cartogram
Composition Ni Co Fe MgO SiO 2
Content (%) 0.083 0.014 2.00 1.50 83.36
Table 2-2 normal pressure acidleach filtrate (B 2) composition cartogram
Composition Ni Co Fe MgO
Content (g/L) 4.06 0.34 38.84 18.96
Table 2-3 washings (E 2) composition cartogram
Composition Ni Co Fe MgO
Content (g/L) 1.63 0.07 21.65 7.82
Table 2-4 pressure leaching slag (C 2) composition cartogram
Composition Ni Co Fe MgO SiO 2 S
Content (%) 0.082 0.006 62.91 0.034 2.428 1.243
Table 2-5 pressure leaching filtrate (D 2) composition cartogram
Composition Ni Co Fe MgO
Content (g/L) 6.38 0.37 1.15 10.75
Table 2-6 washings (F 2) composition cartogram
Composition Ni Co Fe MgO
Content (g/L) 2.76 0.15 0.47 4.83
Table 2-7 rhombohedral iron ore (G 2) composition cartogram
Composition Ni Co Fe MgO SiO 2 S
Content (%) 0.076 0.009 63.04 0.028 2.420 0.312
table 2-8 silicon dioxide powder (H 2) composition cartogram
Composition Ni Co Fe MgO SiO 2
Content (%) 0.079 0.011 1.243 0.987 92.894
Table 2-9 fine sand (I 2) composition cartogram
Composition Ni Co Fe MgO SiO 2
Content (%) 0.081 0.009 3.356 2.668 72.136
Table 2-10 nickel hydroxide (cobalt) (J 2) composition cartogram
Composition Ni Co Fe MgO
Content (%) 43.17 2.48 1.23 2.84
Table 2-11 sinks liquid (K after nickel 2) composition cartogram
Composition Ni Co Fe MgO
Content (g/L) 0.027 0.003 0.001 18.36
Table 2-12 magnesium sulfate (L 2) composition cartogram
Composition Ni Co Fe MgO
Content (%) 0.009 0.001 0.002 14.38
embodiment 3
1,2,3 steps of the present embodiment are identical with embodiment 1, and namely the normal pressure acid leaching stage of the present embodiment is identical with embodiment 1, changed new for 3# noise made in coughing or vomiting low silicon magnesium ore deposit into 6# Indonesia low silicon magnesium ore deposit in the pressure leaching stage.
4 normal pressure leaching liquid pressure leaching and solid-liquid separation.
Get the 6# of 4000g, add 8000ml washings E 3be prepared into secondary ore pulp, washings E 3water content is about more than 90%.The secondary ore pulp prepared being passed into volume is that the PARR4557 of 17L pressurizes in anti-still, afterwards again to the normal pressure acidleach filtrate adding 3000ml during PARR4557 pressurizes anti-still.Temperature of reaction maintains 225 DEG C, and reaction continues 45 minutes, and pH value maintains between 1; Reaction pressure maintains 2.9Mpa.From autoclave, shift out reaction paste after being cooled to 80 DEG C carry out solid-liquid separation and wash filter residue, obtain 3440g pressure leaching slag C 3, 9430ml pressureleaching solution D 3, 5540ml washings F 3(pressure leaching slag C 3, pressureleaching solution D 3, washings F 3composition in Table 3-1, table 3-2 and table 3-3).
5 reclaim iron.
Get 300g pressure leaching slag C 3add and fill 1000ml, concentration is in the beaker of 10% sodium carbonate solution, is heated to 60 DEG C and stirs 30 minutes.Solid-liquid separation washing leaching cake, oven dry, obtain 291g rhombohedral iron ore G 3(rhombohedral iron ore G 3composition is in Table 3-4).
6 reclaim nickel.
Get 500ml pressureleaching solution D 3put into beaker, stir and heating in water bath to 80 DEG C, slowly add 30% milk of magnesia adjust ph to 7.5 afterwards, stablize after 45 minutes and filter and washing leaching cake, obtain 7.67g nickel hydroxide (cobalt) J 3nickel (cobalt) liquid K is afterwards sunk with 490ml 3(nickel hydroxide (cobalt) J 3with heavy nickel (cobalt) liquid K afterwards 3composition is in Table 3-5, table 3-6).
7 reclaim magnesium.
Get 450ml and sink liquid K after nickel 3put into beaker, stir and heating in water bath, mixing speed 250r/min, it is 80 DEG C that temperature controls.Add 5%NaClO solution and instill milk of magnesia adjust ph in 7 scopes.Alternate operation repeatedly, when instilling NaClO solution again, when pH value goes up not down, continue heating and within 1 hour, make Manganse Dioxide crystal grow up, pH value is finally 7.5.Be cooled to after room temperature and filter and washing leaching cake, obtain liquid 420ml after manganese dioxide precipitate demanganization.To liquid condensing crystal after demanganization and separation of lowering the temperature, obtain 58g magnesium sulfate L 3with system tail washings (magnesium sulfate L 3composition is in Table 3-7).
Based on the component content of residue, calculate nickel, cobalt leaching yield, slag rate and acid consumption data as follows: pressure leaching nickel leaching yield: 95.66%; Pressure leaching cobalt leaching yield: 96.12%.Amount to nickel leaching yield 96.30%; Cobalt leaching yield 96.26%.Iron recovery >96%.Sulfuric acid consumption: 200Kg sulfuric acid/t ore deposit.Amount to slag rate: 82.0g white residue/1000g laterite.Table 3-1 pressure leaching slag (C 3) composition cartogram
Composition Ni Co Fe MgO SiO 2 S
Content (%) 0.067 0.004 62.82 0.027 2.493 1.276
Table 3-2 pressure leaching filtrate (D 3) composition cartogram
Composition Ni Co Fe MgO
Content (g/L) 6.46 0.35 0.98 12.91
Table 3-3 washings (F 3) composition cartogram
Composition Ni Co Fe MgO
Content (g/L) 2.72 0.16 0.37 4.33
Table 3-4 pressure leaching slag (G 3) composition cartogram
Composition Ni Co Fe MgO SiO 2 S
Content (%) 0.058 0.006 62.27 0.021 2.386 0.287
Table 3-5 nickel hydroxide (cobalt) (J 3) composition cartogram
Composition Ni Co Fe MgO
Content (%) 42.11 2.24 1.04 2.43
Table 3-6 sinks liquid (K after nickel 3) composition cartogram
Composition Ni Co Fe MgO
Content (g/L) 0.017 0.003 0.001 21.08
Table 3-7 magnesium sulfate (L 3) composition cartogram
Composition Ni Co Fe MgO
Content (%) 0.021 0.002 0.002 14.68
embodiment 4
1,2,3 steps of the present embodiment are identical with embodiment 2, and namely the normal pressure acid leaching stage of the present embodiment is identical with embodiment 2, changed low for 6# Indonesia silicon magnesium ore deposit into the new noise made in coughing or vomiting of 3# low silicon magnesium ore deposit in the pressure leaching stage.
4 normal pressure leaching liquid pressure leaching and solid-liquid separation.
Get the 6# of 4000g, add 8000ml washings E 4be prepared into secondary ore pulp, washings E 4water content is about more than 90%.The secondary ore pulp prepared being passed into volume is that the PARR4557 of 17L pressurizes in anti-still, afterwards again to the normal pressure acidleach filtrate adding 3000ml during PARR4557 pressurizes anti-still.Temperature of reaction maintains 233 DEG C, and reaction continues 49 minutes, and pH value maintains between 1.2; Reaction pressure maintains 3.23Mpa.From autoclave, shift out reaction paste after being cooled to 80 DEG C carry out solid-liquid separation and wash filter residue, obtain 3470g pressure leaching slag C 4, 9460ml pressureleaching solution D 4, 5380ml washings F 4(pressure leaching slag C 4, pressureleaching solution D 4, washings F 4composition in Table 4-1, table 4-2 and table 4-3).
5 reclaim iron.
Get 300g pressure leaching slag C 4add and fill 1000ml, concentration is in the beaker of 10% sodium carbonate solution, is heated to 60 DEG C and stirs 30 minutes.Solid-liquid separation washing leaching cake, oven dry, obtain 291g rhombohedral iron ore G 4(rhombohedral iron ore G 4composition is in Table 4-4).
6 reclaim nickel.
Get 500ml pressureleaching solution D 4put into beaker, stir and heating in water bath to 80 DEG C, slowly add 30% milk of magnesia adjust ph to 7.3 afterwards, stablize after 45 minutes and filter and washing leaching cake, obtain 6.80g nickel hydroxide (cobalt) J 4nickel (cobalt) liquid K is afterwards sunk with 500ml 4(nickel hydroxide (cobalt) J 4with heavy nickel (cobalt) liquid K afterwards 4composition is in Table 4-5, table 4-6).
7 reclaim magnesium.
Get 450ml and sink liquid K after nickel 4put into beaker, stir and heating in water bath, mixing speed 250r/min, it is 80 DEG C that temperature controls.Add 5%NaClO solution and instill milk of magnesia adjust ph in 7 scopes.Alternate operation repeatedly, when instilling NaClO solution again, when pH value goes up not down, continue heating and within 1 hour, make Manganse Dioxide crystal grow up, pH value is finally 7.5.Be cooled to after room temperature and filter and washing leaching cake, obtain liquid 430ml after manganese dioxide precipitate demanganization.To liquid condensing crystal after demanganization and separation of lowering the temperature, obtain 58g magnesium sulfate L 4with system tail washings (magnesium sulfate L 4composition is in Table 4-7).
Based on the component content of residue, calculate nickel, cobalt leaching yield, slag rate and acid consumption data as follows: pressure leaching nickel leaching yield: 95.66%; Pressure leaching cobalt leaching yield: 96.12%.Amount to nickel leaching yield 96.30%; Cobalt leaching yield 96.26%.Iron recovery >96%.Sulfuric acid consumption: 200Kg sulfuric acid/t ore deposit.Amount to slag rate: 82.0g white residue/1000g laterite.Table 4-1 pressure leaching slag (C 4) composition cartogram
Composition Ni Co Fe MgO SiO 2 S
Content (%) 0.071 0.015 62.82 0.047 2.86 1.272
Table 4-2 pressure leaching filtrate (D 4) composition cartogram
Composition Ni Co Fe MgO
Content (g/L) 5.83 0.63 1.21 10.15
Table 4-3 washings (F 4) composition cartogram
Composition Ni Co Fe MgO
Content (g/L) 2.58 0.28 1.10 4.47
Table 4-4 rhombohedral iron ore (G 4) composition cartogram
Composition Ni Co Fe MgO SiO 2 S
Content (%) 0.066 0.012 63.13 0.056 2.91 0.254
Table 4-5 nickel hydroxide (cobalt) (J 4) composition cartogram
Composition Ni Co Fe MgO
Content (%) 42.78 4.14 0.89 2.12
Table 4-6 sinks liquid (K after nickel 4) composition cartogram
Composition Ni Co Fe MgO
Content (g/L) 0.019 0.002 0.001 18.64
Table 4-7 magnesium sulfate (L 4) composition cartogram
Composition Ni Co Fe MgO
Content (%) 0.025 0.003 0.001 15.02
embodiment 5
1,2,3 steps of the present embodiment are identical with embodiment 1, and namely the normal pressure acid leaching stage of the present embodiment is identical with embodiment 1, changed new for 3# noise made in coughing or vomiting low silicon magnesium ore deposit into 4# Indonesia laterite in the pressure leaching stage.
4 normal pressure leaching liquid pressure leaching and solid-liquid separation.
Get the 4# of 4000g, add 8000ml washings E 5be prepared into secondary ore pulp, washings E 5water content is about more than 90%.The secondary ore pulp prepared being passed into volume is that the PARR4557 of 17L pressurizes in anti-still, afterwards again to the normal pressure acidleach filtrate adding 3000ml during PARR4557 pressurizes anti-still.Temperature of reaction maintains 230 DEG C, and reaction continues 51 minutes, and pH value maintains between 1.1; Reaction pressure maintains 3.6Mpa.From autoclave, shift out reaction paste after being cooled to 80 DEG C carry out solid-liquid separation and wash filter residue, obtain 3750g pressure leaching slag C 5, 9350ml pressureleaching solution D 5, 5920ml washings F 5(pressure leaching slag C 5, pressureleaching solution D 5, washings F 5composition in Table 5-1, table 5-2 and table 5-3).
5 reclaim iron.
Get 300g pressure leaching slag C 5add and fill 1000ml, concentration is in the beaker of 10% sodium carbonate solution, is heated to 60 DEG C and stirs 30 minutes.Solid-liquid separation washing leaching cake, oven dry, obtain 290g rhombohedral iron ore G 5(rhombohedral iron ore G 5composition is in Table 5-4).
6 reclaim nickel.
Get 500ml pressureleaching solution D 5put into beaker, stir and heating in water bath to 80 DEG C, slowly add 30% milk of magnesia adjust ph to 7.1 afterwards, stablize after 45 minutes and filter and washing leaching cake, obtain 7.10g nickel hydroxide (cobalt) J 5nickel (cobalt) liquid K is afterwards sunk with 480ml 5(nickel hydroxide (cobalt) J 5with heavy nickel (cobalt) liquid K afterwards 5composition is in Table 5-5, table 5-6).
7 reclaim magnesium.
Get 450ml and sink liquid K after nickel 5put into beaker, stir and heating in water bath, mixing speed 250r/min, it is 80 DEG C that temperature controls.Add 5%NaClO solution and instill milk of magnesia adjust ph in 7 scopes.Alternate operation repeatedly, when instilling NaClO solution again, when pH value goes up not down, continue heating and within 1 hour, make Manganse Dioxide crystal grow up, pH value is finally 7.5.Be cooled to after room temperature and filter and washing leaching cake, obtain liquid 440ml after manganese dioxide precipitate demanganization.To liquid condensing crystal after demanganization and separation of lowering the temperature, obtain 58g magnesium sulfate L 5with system tail washings (magnesium sulfate L 5composition is in Table 5-7).
Based on the component content of residue, calculate nickel, cobalt leaching yield, slag rate and acid consumption data as follows: pressure leaching nickel leaching yield: 94.98%; Pressure leaching cobalt leaching yield: 92.78%.Amount to nickel leaching yield 95.52%; Cobalt leaching yield 92.83%.Iron recovery >96%.Sulfuric acid consumption: 200Kg sulfuric acid/t ore deposit.Amount to slag rate: 82.0g white residue/1000g laterite.
Table 5-1 pressure leaching slag (C 5) composition cartogram
Composition Ni Co Fe MgO SiO 2 S
Content (%) 0.087 0.016 53.87 0.038 11.171 1.194
Table 5-2 pressure leaching filtrate (D 5) composition cartogram
Composition Ni Co Fe MgO
Content (g/L) 6.03 0.75 1.34 10.45
Table 5-3 washings (F 5) composition cartogram
Composition Ni Co Fe MgO
Content (g/L) 3.17 0.39 0.98 5.50
Table 5-4 rhombohedral iron ore (G 5) composition cartogram
Composition Ni Co Fe MgO SiO 2 S
Content (%) 0.079 0.017 53.82 0.031 12.565 0.356
Table 5-5 nickel hydroxide (cobalt) (J 5) composition cartogram
Composition Ni Co Fe MgO
Content (%) 42.34 5.04 0.94 2.11
Table 5-6 sinks liquid (K after nickel 5) composition cartogram
Composition Ni Co Fe MgO
Content (g/L) 0.016 0.001 0.001 18.56
Table 5-7 magnesium sulfate (L 5) composition cartogram
Composition Ni Co Fe MgO
Content (%) 0.014 0.002 0.002 14.69

Claims (2)

1. from low-grade laterite nickel ore, reclaim a method for nickel, iron, silicon and magnesium, comprise the following steps:
A) washing classification:
With 80 orders for washing grade scale is to low-grade laterite nickel ore washing classification, obtain more than 80 Large stone compared with breeze in small, broken bits below nugget and 80 orders;
B) ore pulp is prepared:
By step a) in the Large stone that goes out of washing to grind to form the powder of below 80 orders compared with nugget, mix with the powder of grinding than by water with the volume mass of water with solid matter 0.8 ~ 1.5:1, obtain one-level ore pulp;
With the volume mass of water and solid matter 0.8 ~ 1.5:1 than Jiang Shui with by step a) in the breeze in small, broken bits that goes out of washing mix, obtain secondary ore pulp;
C) vitriol oil normal pressure leaching and solid-liquid separation, reclaims silicon:
By step b) in preparation one-level ore pulp be heated to 60 ~ 90 DEG C, the vitriol oil is heated to 100 ~ 180 DEG C;
The one-level ore pulp of heating and the vitriol oil are passed into steel lining alloy reaction tank react, until form cellular lotion;
Water is mixed with the ratio of 1 ~ 1.5:1 with cellular lotion, at the uniform velocity stirs 20 ~ 70 minutes, obtain mixing solutions;
Carry out solid-liquid separation to mixing solutions, obtain normal pressure leaching slag A and normal pressure leaching liquid B, described normal pressure leaching slag A is silicon-dioxide;
D) normal pressure leaching liquid B pressure leaching and solid-liquid separation:
By normal pressure leaching liquid B with add compressive reaction still to secondary ore pulp with the volume ratio of 1:2 ~ 3 and react, temperature of reaction maintains 150 ~ 240 DEG C; Reaction continues 30 ~ 60 minutes; PH value maintains between 0.5 ~ 1.5; Reaction pressure maintains 1.5 ~ 4Mpa;
Solid-liquid separation is carried out to reacted solution, obtains pressure leaching slag C and pressureleaching solution D;
E) iron is reclaimed:
Basic solution with 10% washs pressure leaching slag C;
Drying and processing is carried out to the solid particulate after washing, obtains Iron concentrate particle;
F) nickel is reclaimed:
In pressureleaching solution D, add magnesium oxide react, until pH value maintains between 7 ~ 8;
Solid-liquid separation is carried out to reacted solution, obtains nickel hydroxide solid particulate and Adlerika;
Conventional processing is carried out to nickel hydroxide solid particulate and can obtain nickel;
G) magnesium is reclaimed:
Evaporative crystallization is carried out to the Adlerika produced in step f, obtains solid sulphuric acid magnesium granules.
2. a kind of method reclaiming nickel, iron, silicon and magnesium from low-grade laterite nickel ore according to claim 1, is characterized in that: the sulfuric acid used in described step c and pulp volume are than 0.8 ~ 1.8:1.
CN201410845470.8A 2014-12-31 2014-12-31 Method for recovering nickel, iron, silicon and magnesium from low grade laterite-nickel ore Pending CN104775027A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109836002A (en) * 2017-11-24 2019-06-04 常州第六元素材料科技股份有限公司 The hierarchical processing method of the spent acid containing manganese
WO2019210350A1 (en) * 2018-04-30 2019-11-07 Silica Technology Pty Ltd Processing of silicate minerals
WO2019210351A1 (en) * 2018-04-30 2019-11-07 Silica Technology Pty Ltd Improved mica processing
CN113088723A (en) * 2021-04-06 2021-07-09 吴家明 Method and system for smelting laterite-nickel ore

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109836002A (en) * 2017-11-24 2019-06-04 常州第六元素材料科技股份有限公司 The hierarchical processing method of the spent acid containing manganese
CN109836002B (en) * 2017-11-24 2021-12-03 常州第六元素材料科技股份有限公司 Grading treatment method for manganese-containing waste acid
WO2019210350A1 (en) * 2018-04-30 2019-11-07 Silica Technology Pty Ltd Processing of silicate minerals
WO2019210351A1 (en) * 2018-04-30 2019-11-07 Silica Technology Pty Ltd Improved mica processing
CN113088723A (en) * 2021-04-06 2021-07-09 吴家明 Method and system for smelting laterite-nickel ore

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