CN102912124B - Method for recovering nickel, cobalt, manganese and iron by hydrochloric acid leaching of nickel oxide ore - Google Patents
Method for recovering nickel, cobalt, manganese and iron by hydrochloric acid leaching of nickel oxide ore Download PDFInfo
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Abstract
The invention relates to a method for recovering nickel, cobalt, manganese and iron by hydrochloric acid leaching of nickel oxide ore. The method comprises the following steps of: firstly performing ball milling on the nickel oxide ore to obtain ore powder; then adding ore powder additives into the ore powder; further using hydrochloric acid to perform leaching treatment on an ore powder mixture to obtain hydrochloric acid leachate of the nickel oxide ore; and adding an oxidant into the hydrochloric acid leachate for treatment so as to obtain a co-precipitate of a cobalt oxide and a manganeseoxide, and adding calcium oxide or sodium hydroxide into filtrate for treatment so as to obtain a precipitate of the mixture containing nickel and iron. The method disclosed by the invention has the advantages of reasonable process design and strong operability, and has the effects of effectively utilizing mineral resources, realizing large-scale industrial production, realizing the recycling of four elements, namely nickel, cobalt, manganese and iron from the hydrochloric acid leachate of the nickel oxide ore, and saving the production cost.
Description
Technical field
The present invention relates to a kind of metallurgical method, particularly a kind of hydrochloric acid leaches the method that nickel oxide ore reclaims nickel cobalt ferromanganese.
Background technology
Nickel oxide ore is a kind of mineral association that contains the first rope of multiple metal.It contains iron, nickel, cobalt, manganese, aluminium and magnesium etc.In order to recycle these true valency metallic elements, people have adopted methods such as pyrometallurgy and hydrometallurgy.Traditional nickel oxide ore pyrometallurgy treatment technology has the thick reduction of rotary kiln drying-electric furnace reduction melting to produce ferronickel; Sintering-blast furnace sulfiding smelting is produced low nickel matte; And the nickel pig iron is produced in sintering-blast furnace retailoring.The melting of rotary kiln drying prereduction electric furnace reduction is the classical technology of handling nickel oxide ore, technological process is as follows: moisture about 30% nickel oxide ore through rotary kiln after 800 ~ 900 ℃ of following drying and dehydratings and thick reduction are handled, send into ore-smelting furnace again, the retailoring output is nickeliferous under about 1550～1600 ℃ high temperature〉10% ferronickel, be enriched to more than 25% through the further refining of converter again and sell, for producing stainless steel.This method has characteristics such as Technological adaptability is strong, flow process is brief, nickel recovery height.
The blast furnace sulfiding smelting be with nickel oxide ore after allocating an amount of calcium oxide and silicon-dioxide into, under about 1100 ℃, sinter piece (or push agglomerating, dry naturally) into, allocate 10～20% pyrite and about 20～30% coke again into, 1300 ℃ of following meltings in blast furnace, the low nickel matte product of output nickeliferous 8～15%.Because every kind of valuable metal constituent content is less relatively in nickel oxide ore, so the energy consumption that adopts pyrometallurgy to smelt is higher, this is the main drawback of nickel oxide ore pyrometallurgical smelting.So people adopt the method for hydrometallurgy, optionally extract valuable metal wherein.In recent years, nickel oxide ore sulfuric acid wet process extractive technique obtains to develop rapidly.
Nickel minerals sulfuric acid wet process extractive technique commonly used has: sulfuric acid pressurization leaching, the leaching of sulfuric acid normal pressure, sulfuric acid dump leaching and reduction roasting-ammonia leaching etc.The sulfuric acid pressurization is leached and is handled nickel oxide ore, is to leach under 230 ~ 260 ℃ of high temperature and 4-5Mpa high pressure, and nickel, cobalt leaching yield can reach about 95%.Reducing roasting ammonia soaking technology has reagent N H
3Can be recycled, consumption is little, can comprehensive recovery nickel, advantages such as brill, iron, and nickel, the cobalt leaching yield is on the low side is its main drawback.The sulfuric acid normal pressure leaches nickel oxide ore, is that the mineral composition according to handled nickel oxide ore prepares leach liquor under normal pressure, and giving up usually in the resulting leach liquor has the iron of 10～30g/L, the nickel of 3～5g/L, the cobalt of 0.1～0.3g/L, the magnesium of 30～40g/L.Usually adopt calcium oxide or calcium hydroxide to neutralize in advance, precipitation removes iron and the aluminium in the leach liquor; And then neutralization precipitation nickel and cobalt or with carbonate deposition nickel and cobalt or with sulfide precipitation nickel and brill; Again use calcium oxide neutralization precipitation magnesium thereafter.The emphasis of above-mentioned technology is nickel and the cobalt of recycling in the solution, and all handles valuable element iron, magnesium etc. discarded as impurity unit rope.In addition, in the first step of this technology, namely remove in iron and the aluminium process neutralizing in advance with calcium oxide or oxygen calcium oxide since with the adsorption coprecipitation of iron and aluminium, and local basicity is too high, often causes valuable nickel and cobalt to lose in a large number.
Summary of the invention
Technical problem to be solved by this invention is at the deficiencies in the prior art, and the hydrochloric acid that provides a kind of technological design to reclaim multiple element, the raising rate of recovery and product purity in the nickel oxide ore more rationally, effectively leaches the method that nickel oxide ore reclaims nickel cobalt ferromanganese.
Technical problem to be solved by this invention is to realize by following technical scheme.The present invention is that a kind of hydrochloric acid leaches the method that nickel oxide ore reclaims nickel cobalt ferromanganese, is characterized in that its step is as follows:
(1) ball milling: nickel oxide ore is carried out ball milling in wet-type ball mill, account for more than 60% for-100 orders to ore powder granularity, get breeze;
(2) mix: the additive that adds powdered ore quality 5～30% in the breeze; Described additive is that first component of 1:4～20 and second component are mixed and formed by mass ratio, and first component is selected from least a in sodium-chlor, magnesium chloride or the calcium chloride, and second component is selected from least a in coke powder, coke, coal or the carbon; Get the breeze mixture;
(3) leach: use hydrochloric acid that the breeze mixture is leached processing, obtain the hydrochloric acid leachate of nickel oxide ore; The temperature that leaches when handling is 20～100 ℃, and the time is 30～180min, and the hydrochloric acid add-on accounts for 10～250% of breeze weight; In the nickel oxide ore hydrochloric acid leachate that obtains, principal element content is generally as follows in g/L: Fe5～35, Ni0.5～10, Co0.1～1, Mn0.5～10, Mg5～45, Al0.5～5;
(4) enriching and recovering cobalt and manganese: add at least a in sodium chlorate, hypochlorous acid, hypochlorite, chlorine, black nickel or the potassium permanganate in the hydrochloric acid leachate and handle as oxygenant, the oxygenant usage quantity is precipitate cobalt and the required theoretical amount of manganese 1～5 times, under the condition of 30～100 ℃ of temperature, stir during processing, the stirring linear velocity is 3～6m/s, reaction times 30n～120min, filter the co-precipitation that obtains cobalt/cobalt oxide and Mn oxide, filtrate for later use;
(5) in and co-precipitation nickel and iron: add calcium oxide in the filtrate that makes to step (4) or sodium hydroxide is handled, the usage quantity of described calcium oxide or sodium hydroxide is 1～3 times of the required theoretical amount of iron nickel aluminium in the filtrate; Under the condition of 30～100 ℃ of temperature, stir, reaction times 30～120min, the mixture precipitation that obtains nickeliferous and iron is filtered in terminal point pH=7～9.
Hydrochloric acid of the present invention leaches in the method and technology scheme of nickel oxide ore recovery nickel cobalt ferromanganese, and further optimized technical scheme is as follows:
1. in the step (2): the additive that adds powdered ore quality 15～20% in the breeze; Described additive is that first component of 1:10～15 and second component are mixed and formed by mass ratio.
2. in the step (3): the temperature that leaches when handling is 20～45 ℃, and the time is 60～120min, and the hydrochloric acid add-on accounts for 50～100% of breeze weight.
3. in the step (4): the oxygenant usage quantity is precipitate cobalt and the required theoretical amount of manganese 2～3 times, stirs under the condition of 50～70 ℃ of temperature during processing, and the stirring linear velocity is 4～5m/s, reaction times 60～90min,
4. in the step (5): the usage quantity of described calcium oxide or sodium hydroxide is 2 times of the required theoretical amount of iron nickel aluminium in the filtrate.
5. in the step (5): under the condition of 40 ℃～60 ℃ of temperature, stir reaction times 60～90min, terminal point pH=8.
In the inventive method, the chemical ingredients of raw ore nickel oxide ore % meter by weight is generally: Ni0.5～5, Co0.05～0.15, Fe10～30, Mn0.5～5, MgO 5～30, SiO
25～45, Al
2O
33～15, CaO 0.1～5.
Compared with prior art, the technique effect of the inventive method is as follows:
1. the inventive method has realized nickel, cobalt, manganese and the iron recycling of totally 4 kinds of elements in the nickel oxide ore hydrochloric acid leachate;
2. the inventive method has been produced the mixture of the mixture that contains cobalt/cobalt oxide and Mn oxide, nickeliferous and iron, and multiple product has possessed various industrial uses;
3. the inventive method can improve the rate of recovery and the purity of the mix product of nickeliferous, manganese, cobalt and iron; Saved production cost;
4. the inventive method technological design is reasonable, and is workable, can effectively utilize Mineral resources, can realize extensive workerization production.
Embodiment
Below further describe concrete technical scheme of the present invention, so that those skilled in the art understands the present invention further, and do not constitute the restriction to its right.
Embodiment 1, and a kind of hydrochloric acid leaches the method that nickel oxide ore reclaims nickel cobalt ferromanganese, and its step is as follows:
(1) ball milling: nickel oxide ore is carried out ball milling in wet-type ball mill, account for more than 60% for-100 orders to ore powder granularity, get breeze;
(2) mix: the additive that adds powdered ore quality 5% in the breeze; Described additive is that first component of 1:4 and second component are mixed and formed by mass ratio, and first component is selected from least a in sodium-chlor, magnesium chloride or the calcium chloride, and second component is selected from least a in coke powder, coke, coal or the carbon; Get the breeze mixture;
(3) leach: use hydrochloric acid that the breeze mixture is leached processing, obtain the hydrochloric acid leachate of nickel oxide ore; The temperature that leaches when handling is 20 ℃, and the time is 30min, and the hydrochloric acid add-on accounts for 10% of breeze weight;
(4) enriching and recovering cobalt and manganese: add at least a in sodium chlorate, hypochlorous acid, hypochlorite, chlorine, black nickel or the potassium permanganate in the hydrochloric acid leachate and handle as oxygenant, the oxygenant usage quantity is precipitate cobalt and the required theoretical amount of manganese 1 times, under the condition of 30 ℃ of temperature, stir during processing, the stirring linear velocity is 3m/s, reaction times 30min, filter the co-precipitation that obtains cobalt/cobalt oxide and Mn oxide, filtrate for later use;
(5) in and co-precipitation nickel and iron: add calcium oxide in the filtrate that makes to step (4) or sodium hydroxide is handled, the usage quantity of described calcium oxide or sodium hydroxide is 1 times of the required theoretical amount of iron nickel aluminium in the filtrate; Under the condition of 30～100 ℃ of temperature, stir, reaction times 30min, terminal point pH=7 filters the mixture precipitation that obtains nickeliferous and iron.
Embodiment 2, and a kind of hydrochloric acid leaches the method that nickel oxide ore reclaims nickel cobalt ferromanganese, and its step is as follows:
(1) ball milling: nickel oxide ore is carried out ball milling in wet-type ball mill, account for more than 60% for-100 orders to ore powder granularity, get breeze;
(2) mix: the additive that adds powdered ore quality 30% in the breeze; Described additive is that first component of 1:20 and second component are mixed and formed by mass ratio, and first component is selected from least a in sodium-chlor, magnesium chloride or the calcium chloride, and second component is selected from least a in coke powder, coke, coal or the carbon; Get the breeze mixture;
(3) leach: use hydrochloric acid that the breeze mixture is leached processing, obtain the hydrochloric acid leachate of nickel oxide ore; The temperature that leaches when handling is 100 ℃, and the time is 180min, and the hydrochloric acid add-on accounts for 250% of breeze weight;
(4) enriching and recovering cobalt and manganese: add at least a in sodium chlorate, hypochlorous acid, hypochlorite, chlorine, black nickel or the potassium permanganate in the hydrochloric acid leachate and handle as oxygenant, the oxygenant usage quantity is precipitate cobalt and the required theoretical amount of manganese 5 times, under the condition of 100 ℃ of temperature, stir during processing, the stirring linear velocity is 6m/s, reaction times 120min, filter the co-precipitation that obtains cobalt/cobalt oxide and Mn oxide, filtrate for later use;
(5) in and co-precipitation nickel and iron: add calcium oxide in the filtrate that makes to step (4) or sodium hydroxide is handled, the usage quantity of described calcium oxide or sodium hydroxide is 3 times of the required theoretical amount of iron nickel aluminium in the filtrate; Under the condition of 100 ℃ of temperature, stir, reaction times 120min, terminal point pH=9 filters the mixture precipitation that obtains nickeliferous and iron.
Embodiment 3, and a kind of hydrochloric acid leaches the method that nickel oxide ore reclaims nickel cobalt ferromanganese, and its step is as follows:
(1) ball milling: nickel oxide ore is carried out ball milling in wet-type ball mill, account for more than 60% for-100 orders to ore powder granularity, get breeze;
(2) mix: the additive that adds powdered ore quality 15% in the breeze; Described additive is that first component of 1:100 and second component are mixed and formed by mass ratio, and first component is selected from least a in sodium-chlor, magnesium chloride or the calcium chloride, and second component is selected from least a in coke powder, coke, coal or the carbon; Get the breeze mixture;
(3) leach: use hydrochloric acid that the breeze mixture is leached processing, obtain the hydrochloric acid leachate of nickel oxide ore; The temperature that leaches when handling is 30 ℃, and the time is 120min, and the hydrochloric acid add-on accounts for 100% of breeze weight;
(4) enriching and recovering cobalt and manganese: add at least a in sodium chlorate, hypochlorous acid, hypochlorite, chlorine, black nickel or the potassium permanganate in the hydrochloric acid leachate and handle as oxygenant, the oxygenant usage quantity is precipitate cobalt and the required theoretical amount of manganese 3 times, under the condition of 60 ℃ of temperature, stir during processing, the stirring linear velocity is 4m/s, reaction times 60min, filter the co-precipitation that obtains cobalt/cobalt oxide and Mn oxide, filtrate for later use;
(5) in and co-precipitation nickel and iron: add calcium oxide in the filtrate that makes to step (4) or sodium hydroxide is handled, the usage quantity of described calcium oxide or sodium hydroxide is 2 times of the required theoretical amount of iron nickel aluminium in the filtrate; Under the condition of 50 ℃ of temperature, stir, reaction times 60min, terminal point pH=8 filters the mixture precipitation that obtains nickeliferous and iron.
Embodiment 4, and a kind of hydrochloric acid leaches the method experiment one that nickel oxide ore reclaims nickel cobalt ferromanganese:
Used nickel oxide ore consists of (weight %): Ni 1.4, Fe 14, Co 0.08, MgO18.5, SiO
235.7, Mn 1.2, CaO0.3, Al
2O
36.08, Cr1.02.
Additive add-on (weight %): 20%; The magnesium chloride of 1:5 and coke powder;
Leaching condition: raw meal particle size-74 μ m accounts for 70%, 2.0 times of theoretical amount of hydrochloric acid consumption, 85 ℃ of extraction temperatures, extraction time 60min, liquid-solid ratio 3:1, stir linear velocity 4.5m/s.Leaching yield: nickel 99%, cobalt 94%, iron 99%, manganese 85%.
Nickel oxide ore hydrochloric acid leachate principal element content following (g/L): Fe 25, Ni 4.5, Co 0.25, Mg 35, Mn 3, Al 1.5, pH=1.
Cobalt manganese oxidation and coprecipitation processing condition: add oxidation precipitation cobalt+sodium chlorate of 2 times of manganese theoretical amount, 60 ℃ of oxidation precipitation temperature, oxidation precipitation time 60min.Deposition rate: cobalt 82%, manganese 96%.The cobalt manganese mixture weight percentage composition that obtains is: Fe 3%, Ni 0.3%, Co 2.2%, Mn 32%.
In the ferronickel and the coprecipitation technology condition: 60 ℃ of neutralization precipitation temperature, add calcium hydroxide slurry, control terminal point pH=8.5, iron deposition rate 99.9%, nickel deposition rate 99.5%.The weight percentage of ferronickel enriched substance is: nickel 7%, iron 50 %, MgO 4%.
Embodiment 5, and a kind of hydrochloric acid leaches the method experiment two that nickel oxide ore reclaims nickel cobalt ferromanganese:
Used nickel oxide ore is formed (weight %): Ni 1.6, Fe 16 Co 0.07, MgO15.8, SiO
241.2, Mn1.1, CaO0.2, Al
2O
35.28, Cr0.92.
Additive add-on (weight %): 28%; The sodium-chlor of 1:15 and coke;
Leaching condition: raw meal particle size-74 μ m accounts for 70%, 2.25 times of theoretical amount of hydrochloric acid consumption, 88 ℃ of extraction temperatures, extraction time 60min, liquid-solid ratio 3:1, stir linear velocity 5m/s.Leaching yield: nickel 99%, cobalt 96%, iron 99%.
Nickel oxide ore hydrochloric acid leachate principal element content following (g/L): Fe 28, Ni 5.2, Co 0.22, Mg 30, Mn 2.93, Al 1, pH=0.5.
Cobalt manganese oxidation and coprecipitation processing condition: add oxidation precipitation cobalt+manganese theoretical amount 3 times of De Guo ?nickel, 50 ℃ of oxidation precipitation temperature, oxidation precipitation time 90min.Deposition rate: cobalt 88%, manganese 98%.The cobalt manganese mixture weight percentage composition that obtains is: Fe 4%, Ni 0.35%, Co 2.6%, Mn 38%.
In the ferronickel and the coprecipitation technology condition: 60 ℃ of neutralization precipitation temperature, add calcium hydroxide slurry, control terminal point pH=9, iron deposition rate 99.9%, nickel deposition rate 99.5%.The weight percentage of ferronickel enriched substance is: nickel 8.5%, iron 55%, MgO5%.
Embodiment 6, and a kind of hydrochloric acid leaches the method experiment three that nickel oxide ore reclaims nickel cobalt ferromanganese:
Used nickel oxide ore is formed (weight %): Ni 1.8, Fe 13, Co 0.08, MgO16.5, SiO
238.2, Mn1.8, CaO0.32, Al
2O
34.57, Cr1.15.
Additive add-on (weight %): 18%; The calcium chloride of 1:8 and coal;
Leaching condition: raw meal particle size-74 μ m accounts for 60%, 2.5 times of theoretical amount of hydrochloric acid consumption, 90 ℃ of extraction temperatures, extraction time 60min, liquid-solid ratio 3:1, stir linear velocity 5m/s.Leaching yield: nickel 99.5%, cobalt 99.5%, iron 99%.
Nickel oxide ore hydrochloric acid leachate principal element content following (g/L): Fe 24, Ni 5.9, Co 0.26, Mg 31.5, Mn 4, Al 1.2, pH=0.6.
Cobalt manganese oxidation and coprecipitation processing condition: add oxidation precipitation cobalt+clorox of 3 times of manganese theoretical amount, 40 ℃ of oxidation precipitation temperature, oxidation precipitation time 60min.Deposition rate: cobalt 80%, manganese 92%.The cobalt manganese mixture weight percentage composition that obtains is: Fe 3%, Ni 0.15%, Co 1.6%, Mn 28%.
In the ferronickel and the coprecipitation technology condition: 40 ℃ of neutralization precipitation temperature, add sodium hydroxide slurry, control terminal point pH=9, iron deposition rate 99.9%, nickel deposition rate 99.5%.The weight percentage of ferronickel enriched substance is: nickel 12%, iron 60%, MgO3%.
Claims (6)
1. a hydrochloric acid leaches the method that nickel oxide ore reclaims nickel cobalt ferromanganese, it is characterized in that its step is as follows:
(1) ball milling: nickel oxide ore is carried out ball milling in wet-type ball mill, account for more than 60% for-100 orders to ore powder granularity, get breeze;
(2) mix: the additive that adds powdered ore quality 5～30% in the breeze; Described additive is that first component of 1:4～20 and second component are mixed and formed by mass ratio, and first component is selected from least a in sodium-chlor, magnesium chloride or the calcium chloride, and second component is selected from least a in coke powder, coke, coal or the carbon; Get the breeze mixture;
(3) leach: use hydrochloric acid that the breeze mixture is leached processing, obtain the hydrochloric acid leachate of nickel oxide ore; The temperature that leaches when handling is 20～100 ℃, and the time is 30～180min, and the hydrochloric acid add-on accounts for 10～250% of breeze weight;
(4) enriching and recovering cobalt and manganese: add at least a in sodium chlorate, hypochlorous acid, hypochlorite, chlorine, black nickel or the potassium permanganate in the hydrochloric acid leachate and handle as oxygenant, the oxygenant usage quantity is precipitate cobalt and the required theoretical amount of manganese 1～5 times, under the condition of 30～100 ℃ of temperature, stir during processing, the stirring linear velocity is 3～6m/s, reaction times 30～120min, filter the co-precipitation that obtains cobalt/cobalt oxide and Mn oxide, filtrate for later use;
(5) in and co-precipitation nickel and iron: add calcium oxide in the filtrate that makes to step (4) or sodium hydroxide is handled, the usage quantity of described calcium oxide or sodium hydroxide is 1～3 times of the required theoretical amount of iron nickel aluminium in the filtrate; Under the condition of 30～100 ℃ of temperature, stir, reaction times 30～120min, the mixture precipitation that obtains nickeliferous and iron is filtered in terminal point pH=7～9.
2. hydrochloric acid according to claim 1 leaches the method that nickel oxide ore reclaims nickel cobalt ferromanganese, it is characterized in that, in the step (2): the additive that adds powdered ore quality 15～20% in the breeze; Described additive is that first component of 1:10～15 and second component are mixed and formed by mass ratio.
3. hydrochloric acid according to claim 1 leaches the method that nickel oxide ore reclaims nickel cobalt ferromanganese, it is characterized in that, in the step (3): the temperature that leaches when handling is 20～45 ℃, and the time is 60～120min, and the hydrochloric acid add-on accounts for 50～100% of breeze weight.
4. hydrochloric acid according to claim 1 leaches the method that nickel oxide ore reclaims nickel cobalt ferromanganese, it is characterized in that, in the step (4): the oxygenant usage quantity is precipitate cobalt and the required theoretical amount of manganese 2～3 times, under the condition of 50～70 ℃ of temperature, stir during processing, the stirring linear velocity is 4～5m/s, reaction times 60～90min.
5. hydrochloric acid according to claim 1 leaches the method that nickel oxide ore reclaims nickel cobalt ferromanganese, it is characterized in that, in the step (5): the usage quantity of described calcium oxide or sodium hydroxide is 2 times of the required theoretical amount of iron nickel aluminium in the filtrate.
6. hydrochloric acid according to claim 1 leaches the method that nickel oxide ore reclaims nickel cobalt ferromanganese, it is characterized in that, in the step (5): stir reaction times 60～90min, terminal point pH=8 under the condition of 40 ℃～60 ℃ of temperature.
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