CN110002421A - A method of battery-grade iron phosphate is prepared using sulfate slag - Google Patents
A method of battery-grade iron phosphate is prepared using sulfate slag Download PDFInfo
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- CN110002421A CN110002421A CN201910410771.0A CN201910410771A CN110002421A CN 110002421 A CN110002421 A CN 110002421A CN 201910410771 A CN201910410771 A CN 201910410771A CN 110002421 A CN110002421 A CN 110002421A
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- sulfate slag
- phosphoric acid
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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
- C01B25/37—Phosphates of heavy metals
- C01B25/375—Phosphates of heavy metals of iron
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention discloses a kind of methods for preparing battery-grade iron phosphate using sulfate slag, it is characterised in that: by sulfate slag after ball-milling treatment, is separated using high-gradient magnetic separation；Gained magnetic separation product is leached after dehydration using phosphoric acid；Gained leached mud is phosphate dihydrate iron crude product, and phosphate dihydrate iron crude product, which is placed in phosphoric acid-hydrofluoric acid mixed acid, leaches removal of impurities, and solid product obtains battery-grade iron phosphate product by washing, drying；This method obtains the battery-grade iron phosphate of high value using sulfate slag industrial residue as raw material, not only realizes waste utilization, and obtain higher economic value, and this method is easy to operate, production cost is low, environmental-friendly, meets industrialization production requirements.
Description
Technical field
The present invention relates to a kind of preparation methods of high-purity phosphoric acid iron, in particular to prepare LITHIUM BATTERY phosphorus by raw material of sulfate slag
The method of sour iron belongs to mineral processing and field of hydrometallurgy.
Background technique
Sulfate slag, also known as pyrite cinder are to produce the industrial residue generated in sulfuric acid process.Containing abundant in sulfate slag
Iron and the elements such as part calcium, silicon, copper, sulphur, but non-ferrous metal content is low in sulfate slag, metalliferous mineral and gangue mineral are mutual
Package, the comprehensive utilization of sulfate slag are restricted.Chinese about 80,000,000 tons of sulfate slags of discharge, national proved reserve every year cross hundred million
Ton.The accumulation of a large amount of sulfate slags wastes land resource, and causes serious pollution to environment.In addition, some developed country's sulphur
The utilization rate of acid sludge has been approached 100%, and China is less than 50%.
Currently, raw material of the comprehensive Utilization Ways of sulfate slag primarily as agglomerates of sintered pellets.However, this method is only applicable to
Certain higher sulfate slags of Iron grade, China's major part sulfate slag Iron grade are low, it is difficult to meet the requirement of agglomerates of sintered pellets factory.In order to
The grade for improving sulfate slag generallys use the method processing sulfate slag of direct ore dressing, due to the metal and arteries and veins in pyrite cinder
Stone is mosaic texture, further increases Iron grade and has difficulties, and limits the utilization of sulfate slag.In addition to above-mentioned two main synthesis
Outside using route, sulfate slag is also used to prepare iron pigment, cement, construction material and extracts non-ferrous metal therein, but by
The reasons such as non-ferrous metal content is low in sulfate slag, process corrosion equipment and utility value are low, the comprehensive benefit of sulfate slag
With being restricted.
Ferric phosphate lithium cell has the advantages such as excellent charge-discharge performance, longer service life, preferable thermal stability,
Thus occupy the important market share in the market.Ferric phosphate is to prepare one of most important raw material of ferric phosphate, preparation method
Mainly solution synthetic method is that raw material forms phosphate dihydrate iron product using molysite and phosphoric acid.But existing ferric phosphate prepares work
Skill higher cost needs good iron material.
Summary of the invention
For exist in the prior art sulfate slag comprehensive utilization, increment processing technology economic value it is low the problems such as, the present invention
Purpose be to be to provide a kind of method for utilizing the preparation of sulfate slag industrial residue that there is high added value battery-grade iron phosphate, the party
Method is easy to operate, production cost is low, environmental-friendly, meets industrialization production requirements.
In order to achieve the above technical purposes, the present invention provides a kind of sides that battery-grade iron phosphate is prepared using sulfate slag
Method, this method are to be separated by sulfate slag after ball-milling treatment using high-gradient magnetic separation；Gained magnetic separation product passes through dehydration
Afterwards, it is leached using phosphoric acid；Gained leached mud is phosphate dihydrate iron crude product, and phosphate dihydrate iron crude product is placed in phosphoric acid-hydrogen fluorine
Removal of impurities is leached in sour mixed acid to get battery-grade iron phosphate product.
Preferred scheme, the sulfate slag are milled to fineness and meet the grade mass percentage content for being less than 0.037mm
Higher than 80%.Mechanical milling process can use ball milling means common in the art, such as wet ball grinding.In preferred ball milling condition
Under closely embedding cloth relationship can be destroyed in sulfate slag between different component by mechanicals efforts, be conducive to the leaching of subsequent iron
Out and conversion process, the rate of recovery of iron is improved.
Preferred scheme, the magnetic field strength of the high-gradient magnetic separation are 1.0~2.5T.According to the main object phase of iron in sulfate slag
For di-iron trioxide, belong to weak magnetic mineral, iron mineral high efficiente callback and enrichment preferentially may be implemented using high-gradient magnetic separation.
Preferred scheme, the condition that the phosphoric acid leaches are as follows: phosphoric acid concentration is 1.5~4.5mol/L, and leaching liquid-solid ratio is 8
~16mL/g, extraction temperature are 80~160 DEG C, and extraction time is 4~12h.Concentration by controlling phosphoric acid can guarantee to leach
Ferriferous oxide dissolution is then converted into Iron phosphate (FePO4) dihydrate form precipitating and is enriched in slag phase in the process, and other impurities metal ion
Still it is present in leachate with metal ion form, so that iron and other metal ions can be realized by being simply separated by solid-liquid separation
Separation.
Preferred scheme, the mass percent concentration of hydrofluoric acid is 1.0~2.5% in the phosphoric acid-hydrofluoric acid mixed acid,
The mass percent concentration of phosphoric acid is 2.0~4.5%.The phosphoric acid and incorporation for using concentration diluter in leaching dedoping step are a small amount of
Hydrofluoric acid, hydrofluoric acid can play the role of destroying silicate mineral in sulfate slag, while may advantageously facilitate by silicate etc.
Dissociation, the dissolution of the metal ion of gangue mineral package, and a small amount of phosphoric acid can guarantee the metal conversion that these new dissolutions come
At Iron phosphate (FePO4) dihydrate, thus not only remove the gangues such as a small amount of silicate after leaching removing impurities, and can dissolve out
A small amount of iron conversion, further increases the purity of product.
Preferred scheme, the condition for leaching removal of impurities are as follows: leaching liquid-solid ratio is 3~10mL/g, and extraction temperature is room temperature,
Extraction time is 3~10h.The mineral such as remaining silicate can sufficiently be dissociated under the conditions of preferred leaching removal of impurities, and will
The metal ion of leaching is converted to Iron phosphate (FePO4) dihydrate, further improves product purity.
Sulfate slag of the invention is the waste residue handled by high temperature oxidation roasting, and wherein iron is mainly with bloodstone (three oxidations
Two iron) form exist, other valuable metals such as calcium, magnesium, copper, nickel, cobalt, lead, zinc etc. mostly in the form of an oxide or doping shape
Formula enters iron oxide lattice, and silicon, aluminium element primarily form silicate and aluminate etc., and close embedding cloth and mutually package is presented
Relationship also contains a small amount of sulfate and sulfide in sulfate slag.Impurity is first in sulfate slag in order to realize for technical solution of the present invention
The separation of element destroys in sulfate slag close embedding cloth relationship between different component first by ball-milling treatment using mechanical energy,
Iron mineral is promoted to realize that monomer dissociation passes through High-gradient Magnetic since iron mineral mainly mutually exists with weak magnetic di-iron trioxide object
The recycling of iron mineral, enrichment may be implemented in choosing, in the process, part granularity it is thinner or in the form of lattice substitution existing for
Impurity metallic elements are appointed and are so remained in the ferriferous oxide after being mixed in magnetic separation.On this basis, it is first leached, is utilized using phosphoric acid
The difference of solubility under the conditions of different phosphoric acid concentrations and pH such as ferric phosphate, cupric phosphate, nickel phosphate, cobalt phosphate, in leaching process
In by control phosphoric acid concentration adjustment, di-iron trioxide and other metal oxides can be promoted to dissolve, digestion of metallic ion into
Enter solution, and then selectivity is precipitated iron ion in the form of Iron phosphate (FePO4) dihydrate, and other metal ions still exist in the form of an ion,
To which the separation of iron Yu other metal ions may be implemented by being simply separated by solid-liquid separation.But the Iron phosphate (FePO4) dihydrate in acquisition is thick
It also comprising the silicate mineral etc. being mingled in product, and is also possible to wrap up part iron ore, Iron phosphate (FePO4) dihydrate purity is much
Lower than LITHIUM BATTERY requirement, therefore, technical solution of the present invention is leached using phosphoric acid-hydrofluoric acid mixed acid, and a small amount of hydrofluoric acid can
To play the role of destroying remaining silicate mineral, further promote the solution for the valuable metal ions being wrapped in gangue mineral
From, dissolution, and dissolve out iron ion can be converted to Iron phosphate (FePO4) dihydrate in time, greatly improve Iron phosphate (FePO4) dihydrate as a result,
Purity reaches LITHIUM BATTERY requirement.
Compared with the prior art, technical solution of the present invention bring the utility model has the advantages that
1) present invention obtains the battery-grade iron phosphate of high value using sulfate slag industrial residue as raw material, not only realizes useless
Object utilizes, and obtains higher economic value.
2) present invention can remove the impurity compositions such as main metal and silicate in sulfate slag by ore grinding-magnetic separation, after
It is continuous to be regulated and controled by phosphoric acid leaching process, the separation and recovery of ferric phosphate and principal metal impurities element is realized, finally by hydrofluoric acid-
The removal of impurities of phosphoric acid mixed solution, removes the oxide containing silicon in synthetic product, is finally prepared into LITHIUM BATTERY Iron phosphate (FePO4) dihydrate product.
3) the ferric phosphate preparation method of offer of the invention is easy to operate, low energy consumption, at low cost, it is easy to accomplish industrial metaplasia
It produces, realizes solid waste comprehensive utilization while realizing sulfate slag increment processing.
Detailed description of the invention
Process flow chart Fig. 1 of the invention；
Fig. 2 embodiment 1 prepares product XRD diagram；
Fig. 3 embodiment 1 prepares the separation of product scanning electron microscope.
Specific embodiment
Following embodiment is intended to further illustrate the content of present invention, rather than limits the protection model of the claims in the present invention
It encloses.
Comparative example 1
With certain sulfate slag in sulfuric acid plant, (Iron grade 60.3%, aluminium, calcium, silicon, magnesium, zinc, copper, cobalt, sulphur, potassium, sodium content are respectively
1.2%, it is 0.8%, 2.3%, 1.2%, 0.8%, 0.6%, 0.4%, 1.0%, 0.1%, 0.1%) raw material, carries out phosphoric acid leaching
Out, phosphoric acid concentration 1.5mol/L, liquid-solid ratio 16ml/g, 80 DEG C of extraction temperature, extraction time is 12 hours, mistake after leaching
Filter is separated by solid-liquid separation；Secondary leaching removal of impurities is carried out to solid product, hydrofluoric acid concentration is 1.0% in cleaner, phosphoric acid concentration
It is 4.5%, leaching liquid-solid ratio is 3ml/g, and extraction temperature is room temperature, extraction time 10h；Filtering is separated by solid-liquid separation again
Afterwards, synthetic product is washed to filtrate pH > 5 with distilled water, obtains primary phosphate dihydrate iron, ferric phosphate purity 89.3%, middle position
10.3 μm of granularity, the rate of recovery of iron is 97.3% in entire process flow, product calcium, magnesium, zinc, cobalt, sulphur, potassium, sodium impurity content
It is below 0.005%, copper, aluminium content are more than 0.1%, and silicone content is higher than 1.0%.
Comparative example 2
With certain sulfate slag in sulfuric acid plant, (Iron grade 60.3%, aluminium, calcium, silicon, magnesium, zinc, copper, cobalt, sulphur, potassium, sodium content are respectively
It 1.2%, is 0.8%, 2.3%, 1.2%, 0.8%, 0.6%, 0.4%, 1.0%, 0.1%, 0.1%) raw material, first by sulfuric acid
Slag is milled to -0.037mm ratio higher than 80%, then is placed in the high gradient magnetic separator that magnetic field strength is 1.0T and carries out magnetic separation point
From, after magnetic separation product is dehydrated, progress phosphoric acid leaching, phosphoric acid concentration 1.5mol/L, liquid-solid ratio 16ml/g, extraction temperature 80
DEG C, extraction time is 12 hours, and filtering is separated by solid-liquid separation after leaching；Synthetic product is washed to filtrate pH with distilled water
> 5, obtains primary phosphate dihydrate iron, 6.21 μm of ferric phosphate purity 90.2%, median particle size, the recycling of iron in entire process flow
Rate is 95.3%, and product aluminium, calcium, magnesium, zinc, copper, cobalt, sulphur, potassium, sodium impurity content are below 0.005%, and silicone content is lower than
2.0%.
Embodiment 1:
With certain sulfate slag in sulfuric acid plant, (Iron grade 60.3%, aluminium, calcium, silicon, magnesium, zinc, copper, cobalt, sulphur, potassium, sodium content are respectively
It 1.2%, is 0.8%, 2.3%, 1.2%, 0.8%, 0.6%, 0.4%, 1.0%, 0.1%, 0.1%) raw material, first by sulfuric acid
Slag is milled to -0.037mm ratio higher than 80%, and ball milling pulp density is 40%；It is placed in the high gradient that magnetic field strength is 1.0T again
Magnetic separation separation is carried out in magnetic separator, after magnetic separation product is dehydrated, carries out phosphoric acid leaching, phosphoric acid concentration 1.5mol/L, liquid-solid ratio
16ml/g, 80 DEG C of extraction temperature, extraction time is 12 hours, and filtering is separated by solid-liquid separation after leaching；To solid product into
The secondary leaching of row cleans, and hydrofluoric acid concentration is 1.0% in cleaner, phosphoric acid concentration 4.5%, and leaching liquid-solid ratio is 3ml/g, leaching
Temperature is room temperature, extraction time 10h out；After filtering is separated by solid-liquid separation again, synthetic product is washed to filter with distilled water
Liquid pH > 5, obtaining product is LITHIUM BATTERY phosphate dihydrate iron, 5.32 μm of ferric phosphate purity 99.5%, median particle size, entire technique
The rate of recovery of iron is 95.3% in process, and product aluminium, calcium, magnesium, zinc, copper, cobalt, sulphur, potassium, sodium impurity content are below 0.005%,
Silicone content is lower than 0.1%.
Embodiment 2:
With certain sulfate slag in sulfuric acid plant, (Iron grade 60.3%, aluminium, calcium, silicon, magnesium, zinc, copper, cobalt, sulphur, potassium, sodium content are respectively
It 1.2%, is 0.8%, 2.3%, 1.2%, 0.8%, 0.6%, 0.4%, 1.0%, 0.1%, 0.1%) raw material, first by sulfuric acid
Slag is milled to -0.037mm ratio higher than 90%, and ball milling pulp density is 50%；It is placed in the high gradient that magnetic field strength is 2.5T again
Magnetic separation separation is carried out in magnetic separator, after magnetic separation product is dehydrated, carries out phosphoric acid leaching, phosphoric acid concentration 4.5mol/L, liquid-solid ratio
8ml/g, 160 DEG C of extraction temperature, extraction time is 4 hours, and filtering is separated by solid-liquid separation after leaching；Solid product is carried out
Secondary leaching cleans, and hydrofluoric acid concentration is 2.5% in cleaner, phosphoric acid concentration 2.0%, and leaching liquid-solid ratio is 10ml/g, leaching
Temperature is room temperature, extraction time 10h out；After filtering is separated by solid-liquid separation again, synthetic product is washed to filter with distilled water
Liquid pH > 6, obtaining product is LITHIUM BATTERY phosphate dihydrate iron, 4.68 μm of ferric phosphate purity 99.2%, median particle size, entire technique
The rate of recovery of iron is 90.2% in process, and product aluminium, calcium, magnesium, zinc, copper, cobalt, sulphur, potassium, sodium impurity content are below 0.005%,
Silicone content is lower than 0.05%.
Embodiment 3:
With certain sulfate slag in sulfuric acid plant, (Iron grade 55.6%, aluminium, calcium, silicon, magnesium, zinc, copper, cobalt, sulphur, potassium, sodium content are respectively
It 2.5%, is 4.3%, 4.3%, 2.1%, 0.4%, 0.3%, 0.1%, 1.3%, 0.1%, 0.1%) raw material, first by sulfuric acid
Slag is milled to -0.037mm ratio higher than 95%, and ball milling pulp density is 55%；It is placed in the high gradient that magnetic field strength is 1.0T again
Magnetic separation separation is carried out in magnetic separator, after magnetic separation product is dehydrated, carries out phosphoric acid leaching, phosphoric acid concentration 3.0mol/L, liquid-solid ratio
10ml/g, 160 DEG C of extraction temperature, extraction time is 4 hours, and filtering is separated by solid-liquid separation after leaching；To solid product into
The secondary leaching of row cleans, and hydrofluoric acid concentration is 2.5% in cleaner, phosphoric acid concentration 3.0%, and leaching liquid-solid ratio is 8ml/g, leaching
Temperature is room temperature, extraction time 10h out；After filtering is separated by solid-liquid separation again, synthetic product is washed to filter with distilled water
Liquid pH > 5, obtaining product is LITHIUM BATTERY phosphate dihydrate iron, 3.98 μm of ferric phosphate purity 99.3%, median particle size, entire technique
The rate of recovery of iron is 85.3% in process, and product aluminium, calcium, magnesium, zinc, copper, cobalt, sulphur, potassium, sodium impurity content are below 0.005%,
Silicone content is lower than 0.1%.
Embodiment 4:
With certain sulfate slag in sulfuric acid plant, (Iron grade 55.6%, aluminium, calcium, silicon, magnesium, zinc, copper, cobalt, sulphur, potassium, sodium content are respectively
It 2.5%, is 4.3%, 4.3%, 2.1%, 0.4%, 0.3%, 0.1%, 1.3%, 0.1%, 0.1%) raw material, first by sulfuric acid
Slag is milled to granularity 100% less than 0.037mm, and ball milling pulp density is 50%；It is placed in the high gradient that magnetic field strength is 2.0T again
Magnetic separation separation is carried out in magnetic separator, after magnetic separation product is dehydrated, carries out phosphoric acid leaching, phosphoric acid concentration 2.0mol/L, liquid-solid ratio
16ml/g, 100 DEG C of extraction temperature, extraction time is 4 hours, and filtering is separated by solid-liquid separation after leaching；To solid product into
The secondary leaching of row cleans, and hydrofluoric acid concentration is 2.5% in cleaner, phosphoric acid concentration 3.0%, and leaching liquid-solid ratio is 8ml/g, leaching
Temperature is room temperature, extraction time 6h out；After filtering is separated by solid-liquid separation again, synthetic product is washed to filtrate with distilled water
PH > 5, obtaining product is LITHIUM BATTERY phosphate dihydrate iron, 4.68 μm of ferric phosphate purity 99.5%, median particle size, entire technique stream
The rate of recovery of Cheng Zhongtie is 89.8%, and product aluminium, calcium, magnesium, zinc, copper, cobalt, sulphur, potassium, sodium impurity content are below 0.005%, silicon
Content is lower than 0.08%.
Claims (6)
1. a kind of method for preparing battery-grade iron phosphate using sulfate slag, it is characterised in that: by sulfate slag after ball-milling treatment,
It is separated using high-gradient magnetic separation；Gained magnetic separation product is leached after dehydration using phosphoric acid；Gained leached mud is two water
Ferric phosphate crude product, phosphate dihydrate iron crude product, which is placed in phosphoric acid-hydrofluoric acid mixed acid, leaches removal of impurities to get battery-grade iron phosphate
Product.
2. a kind of method for preparing battery-grade iron phosphate using sulfate slag according to claim 1, it is characterised in that: described
The ball milling fineness of sulfate slag meets the grade mass percentage content less than 0.037mm and is higher than 80%.
3. a kind of method for preparing battery-grade iron phosphate using sulfate slag according to claim 1, it is characterised in that: described
The magnetic field strength of high-gradient magnetic separation is 1.0~2.5T.
4. a kind of method for preparing battery-grade iron phosphate using sulfate slag according to claim 1, it is characterised in that: described
The condition that phosphoric acid leaches are as follows: phosphoric acid concentration is 1.5~4.5mol/L, and leachings liquid-solid ratio is 8~16mL/g, extraction temperature for 80~
160 DEG C, extraction time is 4~12h.
5. a kind of method for preparing battery-grade iron phosphate using sulfate slag according to claim 1, it is characterised in that: described
The mass percent concentration of hydrofluoric acid is 1.0~2.5% in phosphoric acid-hydrofluoric acid mixed acid, and the mass percent concentration of phosphoric acid is
2.0~4.5%.
6. a kind of method for preparing battery-grade iron phosphate using sulfate slag according to claim 1 or 5, it is characterised in that:
The condition for leaching removal of impurities are as follows: leaching liquid-solid ratio is 3~10mL/g, and extraction temperature is room temperature, and extraction time is 3~10h.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110304617A (en) * | 2019-08-01 | 2019-10-08 | 湖北昊瑞新能源有限公司 | A kind of preparation method of low cost ferric orthophosphate |
| CN114604837A (en) * | 2022-03-30 | 2022-06-10 | 湖北宇浩高科新材料有限公司 | Preparation method of iron phosphate and preparation method of lithium iron phosphate |
| CN115611250A (en) * | 2021-07-16 | 2023-01-17 | 中国科学院过程工程研究所 | Method for recovering high-purity iron phosphate from waste lithium iron phosphate anode powder |
| CN116425136A (en) * | 2023-05-06 | 2023-07-14 | 浙江南化防腐设备有限公司 | Method for purifying and recycling battery-grade ferric phosphate from lithium-extracted ferrophosphorus slag |
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| CN116425136B (en) * | 2023-05-06 | 2023-12-19 | 浙江南化防腐设备有限公司 | Method for purifying and recycling battery-grade ferric phosphate from lithium-extracted ferrophosphorus slag |
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