CN109081322A - A kind of method that ihleite method extracts iron standby LiFePO4 in lateritic nickel ore - Google Patents
A kind of method that ihleite method extracts iron standby LiFePO4 in lateritic nickel ore Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/45—Phosphates containing plural metal, or metal and ammonium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/24—Sulfates of ammonium
- C01C1/245—Preparation from compounds containing nitrogen and sulfur
- C01C1/246—Preparation from compounds containing nitrogen and sulfur from sulfur-containing ammonium compounds
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
A kind of method that ihleite method extracts iron standby LiFePO4 in lateritic nickel ore.Method includes the following steps: (1) is levigate rear baking mixed with ammonium sulfate by lateritic nickel ore, roasting clinker is dissolved out, is filtered, and obtains silicon powder and filtrate；(2) dissolution filtrate obtains nickel pregnant solution and yellow ammonia siderotil after yellow ammonia iron alum and removing iron；(3) yellow ammonia siderotil obtains ammonium sulfate and di-iron trioxide after hydrolyzing, filtering；(4) di-iron trioxide and lithium carbonate, ammonium dihydrogen phosphate and glucose according to a certain percentage after mixing, in a hydrogen atmosphere, 750 DEG C, roast 6h, obtain anode material for lithium-ion batteries LiFePO4/C.The present invention fails the status rationally utilized for lateritic nickel ore, carries out the research of lateritic nickel ore high added value comprehensive utilization, and ihleite method extracts iron standby lithium ion battery anode material lithium iron phosphate, and three-waste free discharge realizes the high value added utilization of Fe element.
Description
Technical field:
The invention belongs to lateritic nickel ore technical field of wet metallurgy, and in particular to ihleite method is extracted in a kind of lateritic nickel ore
The method of iron standby LiFePO4.
Background technique:
The lateritic nickel ore for accounting for world's nickel resources 70% becomes the main resource for extracting nickel, and low-grade laterite nickel ore is due to nickel product
Position low (1% or so), iron content are high (20% or so), and hydrometallurgical processes is mainly taken to extract the valuable elements such as nickel.Compared to
Thermal process, wet processing is simple, at low cost, while can effectively recycle cobalt element in lateritic nickel ore.
Wet processing according to the difference of leaching agent and leaching condition can be divided into ammonia leaching process, the high pressure acid-hatching of young eggs, the normal pressure acid-hatching of young eggs,
Microorganism Leaching method etc..Normal pressure acidleach is the more popular direction of current Proress Technolgies of Laterite-nickel Ore research, normal pressure acidleach laterite
Nickel minerals, for the leaching rate of nickel up to 93%, the leaching rate of iron can be reduced to 30%；Extraction temperature is lower, pressure is lesser mild
Under the conditions of, nickel, cobalt and magnesium have sufficiently been recycled, the efficient Rational Utilization leached with magnesium of nickel cobalt is preferably resolved；Using
Pressure hydrometallurgical process potassium cloride, extraction of nickel (cobalt) iron separate, the technique of magnesium chloride pyrohydrolysis recycles nickel, cobalt, iron, magnesium, while real
The closed cycle of hydrochloric acid is showed.Microorganism Leaching method is the environmentally friendly Treatment method of laterite-nickel ore of comparison, by means of certain specific micro-
The bioactivity catalytic action of biology is dissolved out metallic element effectively from ore, but the leaching rate of industrial amplification process
Extremely unstable, the mineral low for leaching rate must re-start Chemical Leaching.Therefore, the industrialization of Microorganism Leaching is by serious
It hinders.
Wet process new process fully utilizes the elements such as nickel, cobalt, magnesium from the angle developed a circular economy, and considers
Raw material recycles, but the major impurity ferro element in low-grade laterite nickel ore, and answering for high added value is not obtained after removal of impurities
With.In addition, the higher silicon of content is not used in acid treatment technique ore, there is also waste sludge discharge problems.
Core material of the positive electrode as the big material of lithium-ion-power cell four, plays to pass the final performance of battery
Important role, the performance optimization of power battery often rely on the technological break-through of positive electrode, therefore the research of positive electrode
The plate paid close attention to the most as current lithium-ion-power cell.Especially with LiFePO4 (LiFePO4) be representative phosphate
Material is received significant attention due to stable chemical property and high safety, ferric phosphate lithium cell by extensively and
Large-scale application is in fields such as electric car, scale energy storage, backup power sources.
Ferric iron compound (such as FePO4、Fe2O3) have wide, cheap, the volatilizable component of raw material sources few etc. excellent
Point, therefore become commercialization preparation LiFePO4Preferable selection.FePO4Raw material is easy to moisture absorption, and chemical composition is unstable, is actually
FePO4·xH2O (0 < x < 2) is not easy quantitatively, to cause product unstable, heat treatment is typically necessary before use in production and application
Drainage technology increases energy consumption, and due to being complex salt, price is more expensive.
Summary of the invention:
It is an object of the invention to solve the problems, such as that lateritic nickel ore fails rationally to utilize, it is iron to propose the extraction of ihleite method
The method of standby lithium ion battery anode material lithium iron phosphate, realizes the high value added utilization of Fe element.
To achieve the above object, the invention adopts the following technical scheme:
A kind of method that ihleite method extracts iron standby LiFePO4 in lateritic nickel ore, includes the following steps:
(1) grind: lateritic nickel ore is through drying, broken, levigate to 200 mesh hereinafter, obtaining lateritic nickel ore powder；
(2) mixing: press the mass ratio of the material, lateritic nickel ore powder: ammonium sulfate=1:(0.8~1.6), lateritic nickel ore powder with
Ammonium sulfate uniformly mixes, and obtains mixed material；
(3) it roasts: by mixed material in 350 DEG C of roastings 2h, 550 DEG C of roasting 2h, obtaining roasting clinker, roasting process generates
Sulfur trioxide and ammonia sulfuric acid absorption, prepare ammonium sulfate after obtained ammonium sulfate evaporation, concentration, crystallization, return to roasting
Burn process；
(4) it dissolves out: roasting clinker and water 1:4 in mass ratio being dissolved out at 95 DEG C, dissolution time 60min；
(5) it filters: the material dissolved out in step (4) being filtered separation, obtains filtrate and filter residue, filtrate component are as follows:
Fe3+、Fe2+、Mg2+、NH4 +、Al3+、SO4 2-, filter residue main component is silica；
(6) yellow ammonia Jarosite process removes iron: the filtrate in step (5) being carried out yellow ammonia Jarosite process and removes iron, at room temperature into solution
Hydrogen peroxide oxidation Fe is added2+, complete filtrate heating will be aoxidized, temperature is 95 DEG C, and alkali formula regulator is added and controls solution ph
1.0~2.0,4h is stirred, iron-removal rate to 98% or more, filtering, filter residue is yellow ammonia siderotil, and filtrate is nickel enrichment solution；
(7) yellow ammonia siderotil hydrolysis: in mass ratio, yellow ammonia siderotil: water, stirring, heating is added in yellow ammonia siderotil in water=1:2
To 50 DEG C or more, ammonium hydroxide is added, adjusts pH value and reaches 12 or more, time 15min, yellow ammonia siderotil occurs hydrolysis, filters
To di-iron trioxide, filtrate is (NH4)2SO4Solution, filtrate evaporation, crystallization, recycling (NH4)2SO4；
(8)LiFePO4/ C precursor preparation: the mass ratio of the material, di-iron trioxide: lithium carbonate: ammonium dihydrogen phosphate: grape are pressed
Sugar=1:(1.0~1.3): (1.0~1.2): (8~12) mix di-iron trioxide and lithium carbonate, ammonium dihydrogen phosphate, glucose
It closes uniform；
(9)LiFePO4The roasting of/C presoma: the material mixed in step (8) is passed through hydrogen atmosphere and is calcined, is forged
Burning temperature is 750 DEG C, time 6h, and furnace cooling is sieved after cooling, obtains carbon containing lithium-ion battery lithium iron phosphate positive electrode.
In the step (2), lateritic nickel ore powder and ammonium sulfate the mass ratio of the material, with magnesia in lateritic nickel ore powder,
The amount that iron oxide reacts ammonium sulfate substance consumed by generation salt with ammonium sulfate completely is calculated as 1, lateritic nickel ore powder: ammonium sulfate=
1:(0.8~1.6).
In the step (6), the alkali formula regulator is sal volatile.
In the step (7), the heating temperature is 95 DEG C.
In the step (8), the mass ratio of the material of the di-iron trioxide, lithium carbonate, ammonium dihydrogen phosphate, glucose, with
Di-iron trioxide all generates glucose amount used in the LiFePO4 of phosphorus content 5% and is calculated as 1, di-iron trioxide: lithium carbonate: phosphoric acid
Ammonium dihydrogen: glucose=1:(1.0~1.3): (1.0~1.2): (8~15).
The chemical reaction that step (2)~(3) relate generally to are as follows:
MgO+2(NH4)2SO4→(NH4)2Mg(SO4)2+H2O↑+3NH3↑
Fe2O3+4(NH4)2SO4→2(NH4)2Fe(SO4)2+H2O↑+4NH3↑
NiO+2(NH4)2SO4→(NH4)2Ni(SO4)2+H2O↑+3NH3↑
Al2O3+4(NH4)2SO4→2(NH4)2Fe(SO4)2+H2O↑+4NH3↑
(NH4)2SO4→2NH3↑+SO3↑+2H2O↑
2NH3+SO3+2H2O→(NH4)2SO4
Step (6) Huang ammonia Jarosite process removes the chemical reaction that iron occurs are as follows:
6Fe3++2NH4 ++4SO4 2-+12H2O→(NH4)2Fe6(SO4)12↓+12H+
Step (7) Huang ammonia siderotil hydrolysis chemically reacts:
(NH4)2Fe6(SO4)12+22NH3·H2O→3Fe2O3+12(NH4)2SO4+11H2O
Beneficial effects of the present invention:
(1) technical solution of the present invention is simple and easy, propose comprehensive utilization of laterite nickel ore prepare polyanionic lithium from
Sub- cell positive material LiFePO4The novel process route of/C effectively solves major impurity ferro element in low-grade laterite nickel ore
Value added applications, for lateritic nickel ore resource high-efficiency, high added value comprehensive utilization open a new way；
(2) technique core of the invention is the carbon containing object that addition is more than carbon coating demand in the feed, utilizes carbon containing object
Reducibility gas is generated at high temperature, by Fe in raw material3+It is reduced to Fe2+, and ferric phosphate is formed in conjunction with lithium ion and phosphate radical
Lithium, extra carbon dust are coated on the particle surface of product, synthesize carbon-coated LiFePO 4 for lithium ion batteries, improve the electric conductivity of material.
Detailed description of the invention:
Ihleite method extracts the process flow chart of iron standby LiFePO4 in Fig. 1 lateritic nickel ore.
Specific embodiment:
Below with reference to embodiment, the present invention is described in further detail.
Chemical reagent employed in present example is the pure grade product of analysis；Using Japanese Nippon Jarrell-
Constituent content (analysis precision: 0.01wt%) in the IRIS Advantage type icp analysis instrument measurement sample of Ash company.
In conjunction with the process flow chart of Fig. 1.
Embodiment 1
Lateritic nickel ore used is mainly Fe 13.73%, Ni 1.24%, MgO 25.62%, Al2O34.67%, SiO2
43.28%, other 11.46%.
A kind of method that ihleite method extracts iron standby LiFePO4 in lateritic nickel ore, comprising the following steps:
(1) grind: lateritic nickel ore is through drying, broken, levigate to 200 mesh hereinafter, obtaining lateritic nickel ore powder；
(2) the mass ratio of the material, lateritic nickel ore powder: ammonium sulfate=1:0.8, lateritic nickel ore powder and ammonium sulfate mixing: are pressed
Uniformly mixing, obtains mixed material；
(3) it roasts: by mixed material in 350 DEG C of roastings 2h, 550 DEG C of roasting 2h, obtaining roasting clinker, roasting process generates
Sulfur trioxide and ammonia sulfuric acid absorption, prepare ammonium sulfate after obtained ammonium sulfate evaporation, concentration, crystallization, return to roasting
Burn process；
(4) it dissolves out: roasting clinker and water 1:4 in mass ratio being dissolved out at 95 DEG C, dissolution time 60min；
(5) it filters: the material in step (4) being filtered separation, obtains filtrate and filter residue, filtrate component are as follows: Fe3+、
Fe2+、Mg2+、NH4 +、Al3+、SO4 2-, filter residue main component is silica；
(6) yellow ammonia Jarosite process removes iron: the filtrate in step (5) being carried out yellow ammonia Jarosite process and removes iron, at room temperature into solution
Hydrogen peroxide oxidation Fe is added2+, complete filtrate heating will be aoxidized, temperature is 95 DEG C, and sal volatile is added and controls solution ph
1.0~2.0,4h is stirred, iron-removal rate to 98% or more, filtering, filter residue is yellow ammonia siderotil, and filtrate is nickel enrichment solution；
(7) yellow ammonia siderotil hydrolysis: in mass ratio, yellow ammonia siderotil: water, stirring, heating is added in yellow ammonia siderotil in water=1:2
To 50 DEG C or more, ammonium hydroxide is added, adjusts pH value and reaches 12 or more, time 15min, yellow ammonia siderotil occurs hydrolysis, filters
To di-iron trioxide, filtrate is (NH4)2SO4Solution, filtrate evaporation, crystallization, recycling (NH4)2SO4；
(8)LiFePO4/ C precursor preparation: the mass ratio of the material, di-iron trioxide: lithium carbonate: ammonium dihydrogen phosphate: grape are pressed
Di-iron trioxide is uniformly mixed by sugar=1:1.2:1.2:10 with lithium carbonate, ammonium dihydrogen phosphate, glucose；
(9)LiFePO4The roasting of/C presoma: being passed through hydrogen atmosphere for the material mixed in step (8) and calcine, temperature
Degree is 750 DEG C, time 6h, and furnace cooling is sieved after cooling, obtains carbon containing lithium-ion battery lithium iron phosphate positive electrode.
(10) appeal electrode material is assembled into button cell, reaches 162mAh/g in 0.1C multiplying power discharge capacity.
Embodiment 2
Lateritic nickel ore used is mainly Fe 13.73%, Ni 1.24%, MgO 25.62%, Al2O34.67%, SiO2
43.28%, other 11.46%.
A kind of method that ihleite method extracts iron standby LiFePO4 in lateritic nickel ore, comprising the following steps:
(1) grind: lateritic nickel ore is through drying, broken, levigate to 200 mesh hereinafter, obtaining lateritic nickel ore powder；
(2) the mass ratio of the material, lateritic nickel ore powder: ammonium sulfate=1:1.2, lateritic nickel ore powder and ammonium sulfate mixing: are pressed
Uniformly mixing, obtains mixed material；
(3) it roasts: by mixed material in 350 DEG C of roastings 2h, 550 DEG C of roasting 2h, obtaining roasting clinker, roasting process generates
Sulfur trioxide and ammonia sulfuric acid absorption, prepare ammonium sulfate after obtained ammonium sulfate evaporation, concentration, crystallization, return to roasting
Burn process；
(4) it dissolves out: roasting clinker and water 1:4 in mass ratio being dissolved out at 95 DEG C, dissolution time 60min；
(5) it filters: the material in step (4) being filtered separation, obtains filtrate and filter residue, filtrate component are as follows: Fe3+、
Fe2+、Mg2+、NH4 +、Al3+、SO4 2-, filter residue main component is silica；
(6) yellow ammonia Jarosite process removes iron: the filtrate in step (5) being carried out yellow ammonia Jarosite process and removes iron, at room temperature into solution
Hydrogen peroxide oxidation Fe is added2+, complete filtrate heating will be aoxidized, temperature is 95 DEG C, and sal volatile is added and controls solution ph
1.0~2.0,4h is stirred, iron-removal rate to 98% or more, filtering, filter residue is yellow ammonia siderotil, and filtrate is nickel enrichment solution；
(7) yellow ammonia siderotil hydrolysis: in mass ratio, yellow ammonia siderotil: water, stirring, heating is added in yellow ammonia siderotil in water=1:2
To 50 DEG C or more, ammonium hydroxide is added, adjusts pH value and reaches 12 or more, time 15min, yellow ammonia siderotil occurs hydrolysis, filters
To di-iron trioxide, filtrate is (NH4)2SO4Solution, filtrate evaporation, crystallization, recycling (NH4)2SO4；
(8)LiFePO4/ C precursor preparation: the mass ratio of the material, di-iron trioxide: lithium carbonate: ammonium dihydrogen phosphate: grape are pressed
Di-iron trioxide is uniformly mixed by sugar=1:1.2:1.2:10 with lithium carbonate, ammonium dihydrogen phosphate, glucose；
(9)LiFePO4The roasting of/C presoma: being passed through hydrogen atmosphere for the material mixed in step (8) and calcine, temperature
Degree is 750 DEG C, time 6h, and furnace cooling is sieved after cooling, obtains carbon containing lithium-ion battery lithium iron phosphate positive electrode.
(10) appeal electrode material is assembled into button cell, reaches 165mAh/g in 0.1C multiplying power discharge capacity.
Embodiment 3
Lateritic nickel ore used is mainly Fe 13.73%, Ni 1.24%, MgO 25.62%, Al2O34.67%, SiO2
43.28%, other 11.46%.
A kind of method that ihleite method extracts iron standby LiFePO4 in lateritic nickel ore, comprising the following steps:
(1) grind: lateritic nickel ore is through drying, broken, levigate to 200 mesh hereinafter, obtaining lateritic nickel ore powder；
(2) the mass ratio of the material, lateritic nickel ore powder: ammonium sulfate=1:1.6, lateritic nickel ore powder and ammonium sulfate mixing: are pressed
Uniformly mixing, obtains mixed material；
(3) it roasts: by mixed material in 350 DEG C of roastings 2h, 550 DEG C of roasting 2h, obtaining roasting clinker, roasting process generates
Sulfur trioxide and ammonia sulfuric acid absorption, prepare ammonium sulfate after obtained ammonium sulfate evaporation, concentration, crystallization, return to roasting
Burn process；
(4) it dissolves out: roasting clinker and water 1:4 in mass ratio being dissolved out at 95 DEG C, dissolution time 60min；
(5) it filters: the material in step (4) being filtered separation, obtains filtrate and filter residue, filtrate component are as follows: Fe3+、
Fe2+、Mg2+、NH4 +、Al3+、SO4 2-, filter residue main component is silica；
(6) yellow ammonia Jarosite process removes iron: the filtrate in step (5) being carried out yellow ammonia Jarosite process and removes iron, at room temperature into solution
Hydrogen peroxide oxidation Fe is added2+, complete filtrate heating will be aoxidized, temperature is 95 DEG C, and sal volatile is added and controls solution ph
1.0~2.0,4h is stirred, iron-removal rate to 98% or more, filtering, filter residue is yellow ammonia siderotil, and filtrate is nickel enrichment solution；
(7) yellow ammonia siderotil hydrolysis: in mass ratio, yellow ammonia siderotil: water, stirring, heating is added in yellow ammonia siderotil in water=1:2
To 50 DEG C or more, ammonium hydroxide is added, adjusts pH value and reaches 12 or more, time 15min, yellow ammonia siderotil occurs hydrolysis, filters
To di-iron trioxide, filtrate is (NH4)2SO4Solution, filtrate evaporation, crystallization, recycling (NH4)2SO4；
(8)LiFePO4/ C precursor preparation: the mass ratio of the material, di-iron trioxide: lithium carbonate: ammonium dihydrogen phosphate: grape are pressed
Di-iron trioxide is uniformly mixed by sugar=1:1.2:1.2:10 with lithium carbonate, ammonium dihydrogen phosphate, glucose；
(9)LiFePO4The roasting of/C presoma: being passed through hydrogen atmosphere for the material mixed in step (8) and calcine, temperature
Degree is 750 DEG C, time 6h, and furnace cooling is sieved after cooling, obtains carbon containing lithium-ion battery lithium iron phosphate positive electrode.
(10) appeal electrode material is assembled into button cell, reaches 163mAh/g in 0.1C multiplying power discharge capacity.
Embodiment 4
Lateritic nickel ore used is mainly Fe 13.73%, Ni 1.24%, MgO 25.62%, Al2O34.67%, SiO2
43.28%, other 11.46%.
A kind of method that ihleite method extracts iron standby LiFePO4 in lateritic nickel ore, comprising the following steps:
(1) grind: lateritic nickel ore is through drying, broken, levigate to 200 mesh hereinafter, obtaining lateritic nickel ore powder；
(2) the mass ratio of the material, lateritic nickel ore powder: ammonium sulfate=1:1.2, lateritic nickel ore powder and ammonium sulfate mixing: are pressed
Uniformly mixing, obtains mixed material；
(3) it roasts: by mixed material in 350 DEG C of roastings 2h, 550 DEG C of roasting 2h, obtaining roasting clinker, roasting process generates
Sulfur trioxide and ammonia sulfuric acid absorption, prepare ammonium sulfate after obtained ammonium sulfate evaporation, concentration, crystallization, return to roasting
Burn process；
(4) it dissolves out: roasting clinker and water 1:4 in mass ratio being dissolved out at 95 DEG C, dissolution time 60min；
(5) it filters: the material in step (4) being filtered separation, obtains filtrate and filter residue, filtrate component are as follows: Fe3+、
Fe2+、Mg2+、NH4 +、Al3+、SO4 2-, filter residue main component is silica；
(6) yellow ammonia Jarosite process removes iron: the filtrate in step (5) being carried out yellow ammonia Jarosite process and removes iron, at room temperature into solution
Hydrogen peroxide oxidation Fe is added2+, complete filtrate heating will be aoxidized, temperature is 95 DEG C, and sal volatile is added and controls solution ph
1.0~2.0,4h is stirred, iron-removal rate to 98% or more, filtering, filter residue is yellow ammonia siderotil, and filtrate is nickel enrichment solution；
(7) yellow ammonia siderotil hydrolysis: in mass ratio, yellow ammonia siderotil: water, stirring, heating is added in yellow ammonia siderotil in water=1:2
To 50 DEG C or more, ammonium hydroxide is added, adjusts pH value and reaches 12 or more, time 15min, yellow ammonia siderotil occurs hydrolysis, filters
To di-iron trioxide, filtrate is (NH4)2SO4Solution, filtrate evaporation, crystallization, recycling (NH4)2SO4；
(8)LiFePO4/ C precursor preparation: the mass ratio of the material, di-iron trioxide: lithium carbonate: ammonium dihydrogen phosphate: grape are pressed
Di-iron trioxide is uniformly mixed by sugar=1:1.0:1.0:8 with lithium carbonate, ammonium dihydrogen phosphate, glucose；
(9)LiFePO4The roasting of/C presoma: being passed through hydrogen atmosphere for the material mixed in step (8) and calcine, temperature
Degree is 750 DEG C, time 6h, and furnace cooling is sieved after cooling, obtains carbon containing lithium-ion battery lithium iron phosphate positive electrode.
(10) appeal electrode material is assembled into button cell, reaches 135mAh/g in 0.1C multiplying power discharge capacity.
Embodiment 5
Lateritic nickel ore used is mainly Fe 13.73%, Ni 1.24%, MgO 25.62%, Al2O34.67%, SiO2
43.28%, other 11.46%.
A kind of method that ihleite method extracts iron standby LiFePO4 in lateritic nickel ore, comprising the following steps:
(1) grind: lateritic nickel ore is through drying, broken, levigate to 200 mesh hereinafter, obtaining lateritic nickel ore powder；
(2) the mass ratio of the material, lateritic nickel ore powder: ammonium sulfate=1:1.2, lateritic nickel ore powder and ammonium sulfate mixing: are pressed
Uniformly mixing, obtains mixed material；
(3) it roasts: by mixed material in 350 DEG C of roastings 2h, 550 DEG C of roasting 2h, obtaining roasting clinker, roasting process generates
Sulfur trioxide and ammonia sulfuric acid absorption, prepare ammonium sulfate after obtained ammonium sulfate evaporation, concentration, crystallization, return to roasting
Burn process；
(4) it dissolves out: roasting clinker and water 1:4 in mass ratio being dissolved out at 95 DEG C, dissolution time 60min；
(5) it filters: the material in step (4) being filtered separation, obtains filtrate and filter residue, filtrate component are as follows: Fe3+、
Fe2+、Mg2+、NH4 +、Al3+、SO4 2-, filter residue main component is silica；
(6) yellow ammonia Jarosite process removes iron: the filtrate in step (5) being carried out yellow ammonia Jarosite process and removes iron, at room temperature into solution
Hydrogen peroxide oxidation Fe is added2+, complete filtrate heating will be aoxidized, temperature is 95 DEG C, and sal volatile is added and controls solution ph
1.0~2.0,4h is stirred, iron-removal rate to 98% or more, filtering, filter residue is yellow ammonia siderotil, and filtrate is nickel enrichment solution；
(7) yellow ammonia siderotil hydrolysis: in mass ratio, yellow ammonia siderotil: water, stirring, heating is added in yellow ammonia siderotil in water=1:2
To 50 DEG C or more, ammonium hydroxide is added, adjusts pH value and reaches 12 or more, time 15min, yellow ammonia siderotil occurs hydrolysis, filters
To di-iron trioxide, filtrate is (NH4)2SO4Solution, filtrate evaporation, crystallization, recycling (NH4)2SO4；
(8)LiFePO4/ C precursor preparation: the mass ratio of the material, di-iron trioxide: lithium carbonate: ammonium dihydrogen phosphate: grape are pressed
Di-iron trioxide is uniformly mixed by sugar=1:1.3:1.0:8 with lithium carbonate, ammonium dihydrogen phosphate, glucose；
(9)LiFePO4The roasting of/C presoma: being passed through hydrogen atmosphere for the material mixed in step (8) and calcine, temperature
Degree is 750 DEG C, time 6h, and furnace cooling is sieved after cooling, obtains carbon containing lithium-ion battery lithium iron phosphate positive electrode.
(10) appeal electrode material is assembled into button cell, reaches 142mAh/g in 0.1C multiplying power discharge capacity.
Embodiment 6
Lateritic nickel ore used is mainly Fe 13.73%, Ni 1.24%, MgO 25.62%, Al2O34.67%, SiO2
43.28%, other 11.46%.
A kind of method that ihleite method extracts iron standby LiFePO4 in lateritic nickel ore, comprising the following steps:
(1) grind: lateritic nickel ore is through drying, broken, levigate to 200 mesh hereinafter, obtaining lateritic nickel ore powder；
(2) the mass ratio of the material, lateritic nickel ore powder: ammonium sulfate=1:1.2, lateritic nickel ore powder and ammonium sulfate mixing: are pressed
Uniformly mixing, obtains mixed material；
(3) it roasts: by mixed material in 350 DEG C of roastings 2h, 550 DEG C of roasting 2h, obtaining roasting clinker, roasting process generates
Sulfur trioxide and ammonia sulfuric acid absorption, prepare ammonium sulfate after obtained ammonium sulfate evaporation, concentration, crystallization, return to roasting
Burn process；
(4) it dissolves out: roasting clinker and water 1:4 in mass ratio being dissolved out at 95 DEG C, dissolution time 60min；
(5) it filters: the material in step (4) being filtered separation, obtains filtrate and filter residue, filtrate component are as follows: Fe3+、
Fe2+、Mg2+、NH4 +、Al3+、SO4 2-, filter residue main component is silica；
(6) yellow ammonia Jarosite process removes iron: the filtrate in step (5) being carried out yellow ammonia Jarosite process and removes iron, at room temperature into solution
Hydrogen peroxide oxidation Fe is added2+, complete filtrate heating will be aoxidized, temperature is 95 DEG C, and sal volatile is added and controls solution ph
1.0~2.0,4h is stirred, iron-removal rate to 98% or more, filtering, filter residue is yellow ammonia siderotil, and filtrate is nickel enrichment solution；
(7) yellow ammonia siderotil hydrolysis: in mass ratio, yellow ammonia siderotil: water, stirring, heating is added in yellow ammonia siderotil in water=1:2
To 50 DEG C or more, ammonium hydroxide is added, adjusts pH value and reaches 12 or more, time 15min, yellow ammonia siderotil occurs hydrolysis, filters
To di-iron trioxide, filtrate is (NH4)2SO4Solution, filtrate evaporation, crystallization, recycling (NH4)2SO4；
(8)LiFePO4/ C precursor preparation: the mass ratio of the material, di-iron trioxide: lithium carbonate: ammonium dihydrogen phosphate: grape are pressed
Di-iron trioxide is uniformly mixed by sugar=1:1.3:1.2:8 with lithium carbonate, ammonium dihydrogen phosphate, glucose；
(9)LiFePO4The roasting of/C presoma: being passed through hydrogen atmosphere for the material mixed in step (8) and calcine, temperature
Degree is 750 DEG C, time 6h, and furnace cooling is sieved after cooling, obtains carbon containing lithium-ion battery lithium iron phosphate positive electrode.
(10) appeal electrode material is assembled into button cell, reaches 148mAh/g in 0.1C multiplying power discharge capacity.
Embodiment 7
Lateritic nickel ore used is mainly Fe 13.73%, Ni 1.24%, MgO 25.62%, Al2O34.67%, SiO2
43.28%, other 11.46%.
A kind of method that ihleite method extracts iron standby LiFePO4 in lateritic nickel ore, comprising the following steps:
(1) grind: lateritic nickel ore is through drying, broken, levigate to 200 mesh hereinafter, obtaining lateritic nickel ore powder；
(2) the mass ratio of the material, lateritic nickel ore powder: ammonium sulfate=1:1.2, lateritic nickel ore powder and ammonium sulfate mixing: are pressed
Uniformly mixing, obtains mixed material；
(3) it roasts: by mixed material in 350 DEG C of roastings 2h, 550 DEG C of roasting 2h, obtaining roasting clinker, roasting process generates
Sulfur trioxide and ammonia sulfuric acid absorption, prepare ammonium sulfate after obtained ammonium sulfate evaporation, concentration, crystallization, return to roasting
Burn process；
(4) it dissolves out: roasting clinker and water 1:4 in mass ratio being dissolved out at 95 DEG C, dissolution time 60min；
(5) it filters: the material in step (4) being filtered separation, obtains filtrate and filter residue, filtrate component are as follows: Fe3+、
Fe2+、Mg2+、NH4 +、Al3+、SO4 2-, filter residue main component is silica；
(6) yellow ammonia Jarosite process removes iron: the filtrate in step (5) being carried out yellow ammonia Jarosite process and removes iron, at room temperature into solution
Hydrogen peroxide oxidation Fe is added2+, complete filtrate heating will be aoxidized, temperature is 95 DEG C, and sal volatile is added and controls solution ph
1.0~2.0,4h is stirred, iron-removal rate to 98% or more, filtering, filter residue is yellow ammonia siderotil, and filtrate is nickel enrichment solution；
(7) yellow ammonia siderotil hydrolysis: in mass ratio, yellow ammonia siderotil: water, stirring, heating is added in yellow ammonia siderotil in water=1:2
To 50 DEG C or more, ammonium hydroxide is added, adjusts pH value and reaches 12 or more, time 15min, yellow ammonia siderotil occurs hydrolysis, filters
To di-iron trioxide, filtrate is (NH4)2SO4Solution, filtrate evaporation, crystallization, recycling (NH4)2SO4；
(8)LiFePO4/ C precursor preparation: the mass ratio of the material, di-iron trioxide: lithium carbonate: ammonium dihydrogen phosphate: grape are pressed
Di-iron trioxide is uniformly mixed by sugar=1:1.3:1.2:10 with lithium carbonate, ammonium dihydrogen phosphate, glucose；
(9)LiFePO4The roasting of/C presoma: being passed through hydrogen atmosphere for the material mixed in step (8) and calcine, temperature
Degree is 750 DEG C, time 6h, and furnace cooling is sieved after cooling, obtains carbon containing lithium-ion battery lithium iron phosphate positive electrode.
(10) appeal electrode material is assembled into button cell, reaches 158mAh/g in 0.1C multiplying power discharge capacity.
Embodiment 8
Lateritic nickel ore used is mainly Fe 13.73%, Ni 1.24%, MgO 25.62%, Al2O34.67%, SiO2
43.28%, other 11.46%.
A kind of method that ihleite method extracts iron standby LiFePO4 in lateritic nickel ore, comprising the following steps:
(1) grind: lateritic nickel ore is through drying, broken, levigate to 200 mesh hereinafter, obtaining lateritic nickel ore powder；
(2) the mass ratio of the material, lateritic nickel ore powder: ammonium sulfate=1:1.2, lateritic nickel ore powder and ammonium sulfate mixing: are pressed
Uniformly mixing, obtains mixed material；
(3) it roasts: by mixed material in 350 DEG C of roastings 2h, 550 DEG C of roasting 2h, obtaining roasting clinker, roasting process generates
Sulfur trioxide and ammonia sulfuric acid absorption, prepare ammonium sulfate after obtained ammonium sulfate evaporation, concentration, crystallization, return to roasting
Burn process；
(4) it dissolves out: roasting clinker and water 1:4 in mass ratio being dissolved out at 95 DEG C, dissolution time 60min；
(5) it filters: the material in step (4) being filtered separation, obtains filtrate and filter residue, filtrate component are as follows: Fe3+、
Fe2+、Mg2+、NH4 +、Al3+、SO4 2-, filter residue main component is silica；
(6) yellow ammonia Jarosite process removes iron: the filtrate in step (5) being carried out yellow ammonia Jarosite process and removes iron, at room temperature into solution
Hydrogen peroxide oxidation Fe is added2+, complete filtrate heating will be aoxidized, temperature is 95 DEG C, and sal volatile is added and controls solution ph
1.0~2.0,4h is stirred, iron-removal rate to 98% or more, filtering, filter residue is yellow ammonia siderotil, and filtrate is nickel enrichment solution；
(7) yellow ammonia siderotil hydrolysis: in mass ratio, yellow ammonia siderotil: water, stirring, heating is added in yellow ammonia siderotil in water=1:2
To 50 DEG C or more, ammonium hydroxide is added, adjusts pH value and reaches 12 or more, time 15min, yellow ammonia siderotil occurs hydrolysis, filters
To di-iron trioxide, filtrate is (NH4)2SO4Solution, filtrate evaporation, crystallization, recycling (NH4)2SO4；
(8)LiFePO4/ C precursor preparation: the mass ratio of the material, di-iron trioxide: lithium carbonate: ammonium dihydrogen phosphate: grape are pressed
Di-iron trioxide is uniformly mixed by sugar=1:1.2:1.2:12 with lithium carbonate, ammonium dihydrogen phosphate, glucose；
(9)LiFePO4The roasting of/C presoma: being passed through hydrogen atmosphere for the material mixed in step (8) and calcine, temperature
Degree is 750 DEG C, time 6h, and furnace cooling is sieved after cooling, obtains carbon containing lithium-ion battery lithium iron phosphate positive electrode.
(10) appeal electrode material is assembled into button cell, reaches 150mAh/g in 0.1C multiplying power discharge capacity.
Embodiment 9
Lateritic nickel ore used is mainly Fe 13.73%, Ni 1.24%, MgO 25.62%, Al2O34.67%, SiO2
43.28%, other 11.46%.
A kind of method that ihleite method extracts iron standby LiFePO4 in lateritic nickel ore, comprising the following steps:
(1) grind: lateritic nickel ore is through drying, broken, levigate to 200 mesh hereinafter, obtaining lateritic nickel ore powder；
(2) the mass ratio of the material, lateritic nickel ore powder: ammonium sulfate=1:1.2, lateritic nickel ore powder and ammonium sulfate mixing: are pressed
Uniformly mixing, obtains mixed material；
(3) it roasts: by mixed material in 350 DEG C of roastings 2h, 550 DEG C of roasting 2h, obtaining roasting clinker, roasting process generates
Sulfur trioxide and ammonia sulfuric acid absorption, prepare ammonium sulfate after obtained ammonium sulfate evaporation, concentration, crystallization, return to roasting
Burn process；
(4) it dissolves out: roasting clinker and water 1:4 in mass ratio being dissolved out at 95 DEG C, dissolution time 60min；
(5) it filters: the material in step (4) being filtered separation, obtains filtrate and filter residue, filtrate component are as follows: Fe3+、
Fe2+、Mg2+、NH4 +、Al3+、SO4 2-, filter residue main component is silica；
(6) yellow ammonia Jarosite process removes iron: the filtrate in step (5) being carried out yellow ammonia Jarosite process and removes iron, at room temperature into solution
Hydrogen peroxide oxidation Fe is added2+, complete filtrate heating will be aoxidized, temperature is 95 DEG C, and sal volatile is added and controls solution ph
1.0~2.0,4h is stirred, iron-removal rate to 98% or more, filtering, filter residue is yellow ammonia siderotil, and filtrate is nickel enrichment solution；
(7) yellow ammonia siderotil hydrolysis: in mass ratio, yellow ammonia siderotil: water, stirring, heating is added in yellow ammonia siderotil in water=1:2
To 50 DEG C or more, ammonium hydroxide is added, adjusts pH value and reaches 12 or more, time 15min, yellow ammonia siderotil occurs hydrolysis, filters
To di-iron trioxide, filtrate is (NH4)2SO4Solution, filtrate evaporation, crystallization, recycling (NH4)2SO4；
(8)LiFePO4/ C precursor preparation: the mass ratio of the material, di-iron trioxide: lithium carbonate: ammonium dihydrogen phosphate: grape are pressed
Di-iron trioxide is uniformly mixed by sugar=1:1.3:1.2:15 with lithium carbonate, ammonium dihydrogen phosphate, glucose；
(9)LiFePO4The roasting of/C presoma: being passed through hydrogen atmosphere for the material mixed in step (8) and calcine, temperature
Degree is 750 DEG C, time 6h, and furnace cooling is sieved after cooling, obtains carbon containing lithium-ion battery lithium iron phosphate positive electrode.
(10) appeal electrode material is assembled into button cell, reaches 138mAh/g in 0.1C multiplying power discharge capacity.
Embodiment 10
Lateritic nickel ore used is mainly Fe 13.73%, Ni 1.24%, MgO 25.62%, Al2O34.67%, SiO2
43.28%, other 11.46%.
A kind of method that ihleite method extracts iron standby LiFePO4 in lateritic nickel ore, comprising the following steps:
(1) grind: lateritic nickel ore is through drying, broken, levigate to 200 mesh hereinafter, obtaining lateritic nickel ore powder；
(2) the mass ratio of the material, lateritic nickel ore powder: ammonium sulfate=1:1.2, lateritic nickel ore powder and ammonium sulfate mixing: are pressed
Uniformly mixing, obtains mixed material；
(3) it roasts: by mixed material in 350 DEG C of roastings 2h, 550 DEG C of roasting 2h, obtaining roasting clinker, roasting process generates
Sulfur trioxide and ammonia sulfuric acid absorption, prepare ammonium sulfate after obtained ammonium sulfate evaporation, concentration, crystallization, return to roasting
Burn process；
(4) it dissolves out: roasting clinker and water 1:4 in mass ratio being dissolved out at 95 DEG C, dissolution time 60min；
(5) it filters: the material in step (4) being filtered separation, obtains filtrate and filter residue, filtrate component are as follows: Fe3+、
Fe2+、Mg2+、NH4 +、Al3+、SO4 2-, filter residue main component is silica；
(6) yellow ammonia Jarosite process removes iron: the filtrate in step (5) being carried out yellow ammonia Jarosite process and removes iron, at room temperature into solution
Hydrogen peroxide oxidation Fe is added2+, complete filtrate heating will be aoxidized, temperature is 95 DEG C, and sal volatile is added and controls solution ph
1.0~2.0,4h is stirred, iron-removal rate to 98% or more, filtering, filter residue is yellow ammonia siderotil, and filtrate is nickel enrichment solution；
(7) yellow ammonia siderotil hydrolysis: in mass ratio, yellow ammonia siderotil: water, stirring, heating is added in yellow ammonia siderotil in water=1:2
To 50 DEG C or more, ammonium hydroxide is added, adjusts pH value and reaches 12 or more, time 15min, yellow ammonia siderotil occurs hydrolysis, filters
To di-iron trioxide, filtrate is (NH4)2SO4Solution, filtrate evaporation, crystallization, recycling (NH4)2SO4；
(8)LiFePO4/ C precursor preparation: the mass ratio of the material, di-iron trioxide: lithium carbonate: ammonium dihydrogen phosphate: grape are pressed
Di-iron trioxide is uniformly mixed by sugar=1:1.2:1.2:15 with lithium carbonate, ammonium dihydrogen phosphate, glucose；
(9)LiFePO4The roasting of/C presoma: being passed through hydrogen atmosphere for the material mixed in step (8) and calcine, temperature
Degree is 750 DEG C, time 6h, and furnace cooling is sieved after cooling, obtains carbon containing lithium-ion battery lithium iron phosphate positive electrode.
(10) appeal electrode material is assembled into button cell, reaches 142mAh/g in 0.1C multiplying power discharge capacity.
Claims (5)
1. a kind of method that ihleite method extracts iron standby LiFePO4 in lateritic nickel ore, which comprises the steps of:
(1) grind: lateritic nickel ore is through drying, broken, levigate to 200 mesh hereinafter, obtaining lateritic nickel ore powder；
(2) the mass ratio of the material, lateritic nickel ore powder: ammonium sulfate=1:(0.8~1.6 mixing: are pressed), lateritic nickel ore powder and sulfuric acid
Ammonium uniformly mixes, and obtains mixed material；
(3) it roasts: by mixed material in 350 DEG C of roastings 2h, 550 DEG C of roasting 2h, obtaining roasting clinker, the three of roasting process generation
Sulfur oxide and ammonia sulfuric acid absorption prepare ammonium sulfate after obtained ammonium sulfate evaporation, concentration, crystallization, return to roasting work
Sequence；
(4) it dissolves out: roasting clinker and water 1:4 in mass ratio being dissolved out at 95 DEG C, dissolution time 60min；
(5) it filters: the material dissolved out in step (4) being filtered separation, obtains filtrate and filter residue, filtrate component Fe3+、
Fe2+、Mg2+、NH4 +、Al3+、SO4 2-, filter residue main component is silica；
(6) yellow ammonia Jarosite process removes iron: the filtrate in step (5) being carried out yellow ammonia Jarosite process and removes iron, is added at room temperature into solution
Hydrogen peroxide oxidation Fe2+, complete filtrate will be aoxidized and be warming up to 95 DEG C, alkali formula regulator is added and controls solution ph 1.0~2.0,
4h is stirred, iron-removal rate to 98% or more, filtering, filter residue is yellow ammonia siderotil, and filtrate is nickel enrichment solution；
(7) yellow ammonia siderotil hydrolysis: in mass ratio, yellow ammonia siderotil: water=1:2 is added water in yellow ammonia siderotil, stirs, is heated to 50
DEG C or more, ammonium hydroxide is added, adjusts pH value and reaches 12 or more, time 15min, yellow ammonia siderotil occurs hydrolysis, is obtained by filtration three
Two iron are aoxidized, filtrate is (NH4)2SO4Solution, filtrate evaporation, crystallization, recycling (NH4)2SO4；
(8)LiFePO4/ C precursor preparation: the mass ratio of the material is pressed, di-iron trioxide: lithium carbonate: ammonium dihydrogen phosphate: glucose=
1:(1.0~1.3): (1.0~1.2): (8~15) mix di-iron trioxide with lithium carbonate, ammonium dihydrogen phosphate, glucose
It is even；
(9)LiFePO4The roasting of/C presoma: the material mixed in step (8) is calcined in a hydrogen atmosphere, temperature 750
DEG C, time 6h, furnace cooling is sieved after cooling, obtains carbon containing lithium-ion battery lithium iron phosphate positive electrode.
2. the method according to claim 1, wherein in the step (2), lateritic nickel ore powder and ammonium sulfate object
The amount ratio of matter is reacted completely with ammonium sulfate with magnesia, iron oxide in lateritic nickel ore powder and generates ammonium sulfate object consumed by salt
The amount of matter is calculated as 1, lateritic nickel ore powder: ammonium sulfate=1:(0.8~1.6).
3. the method according to claim 1, wherein the alkali formula regulator is ammonium carbonate in the step (6)
Solution.
4. the method according to claim 1, wherein the heating temperature is 95 DEG C in the step (7).
5. the method according to claim 1, wherein in the step (8), the di-iron trioxide, lithium carbonate,
The mass ratio of the material of ammonium dihydrogen phosphate, glucose all generates grape used in the LiFePO4 of phosphorus content 5% with di-iron trioxide
Sugar amount is calculated as 1, di-iron trioxide: lithium carbonate: ammonium dihydrogen phosphate: glucose=1:(1.0~1.3): (1.0~1.2): (8~
15)。
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