CN109305663A - Battery-grade anhydrous iron phosphate and preparation method thereof - Google Patents

Battery-grade anhydrous iron phosphate and preparation method thereof Download PDF

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Publication number
CN109305663A
CN109305663A CN201810931479.9A CN201810931479A CN109305663A CN 109305663 A CN109305663 A CN 109305663A CN 201810931479 A CN201810931479 A CN 201810931479A CN 109305663 A CN109305663 A CN 109305663A
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battery
iron
phosphoric acid
phosphate
grade anhydrous
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颜小雄
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Sichuan Yingda lithium battery new material Co.,Ltd.
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Hunan Yue Yue Battery Material Co Ltd
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Priority to CN201810931479.9A priority Critical patent/CN109305663A/en
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/58Selection 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
    • H01M4/5825Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B25/00Phosphorus; Compounds thereof
    • C01B25/16Oxyacids of phosphorus; Salts thereof
    • C01B25/26Phosphates
    • C01B25/37Phosphates of heavy metals
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B25/00Phosphorus; Compounds thereof
    • C01B25/16Oxyacids of phosphorus; Salts thereof
    • C01B25/26Phosphates
    • C01B25/45Phosphates containing plural metal, or metal and ammonium
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01CAMMONIA; CYANOGEN; COMPOUNDS THEREOF
    • C01C1/00Ammonia; Compounds thereof
    • C01C1/24Sulfates of ammonium
    • C01C1/242Preparation from ammonia and sulfuric acid or sulfur trioxide
    • CCHEMISTRY; METALLURGY
    • C05FERTILISERS; MANUFACTURE THEREOF
    • C05CNITROGENOUS FERTILISERS
    • C05C3/00Fertilisers containing other salts of ammonia or ammonia itself, e.g. gas liquor
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/11Powder tap density
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The present invention relates to a kind of battery-grade anhydrous iron phosphate and preparation method thereof, anhydrous phosphoric acid iron powder body is made of the monodisperse olive shape particle of morphological rules, and tap density is up to 1.5-1.6g/cm3;Use the oxidation-precipitation method using air as oxidant, pH adjusting agent solution is added in divalent iron salt and phosphoric acid or phosphatic mixture aqueous solution and controls pH value, it is passed through air, stirring, reaction generates the crystalline state compound containing ammonium root, hydroxyl and the crystallization water, then obtains NH4Fe2 (OH) (PO4) 22H2O powder through separation of solid and liquid, washing, drying;The powder roasts in air atmosphere, decomposes and removes ammonium root, hydroxyl and the crystallization water, obtains battery-grade anhydrous iron phosphate.Battery-grade anhydrous iron phosphate quality of the present invention is high, and simple production process reduces cost and pollution.

Description

Battery-grade anhydrous iron phosphate and preparation method thereof
Technical field
The present invention relates to battery material preparations, specifically disclose a kind of preparation method of battery-grade anhydrous iron phosphate.
Background technique
It will likely be solar energy, wind energy, tidal power system by the lithium-ion energy storage battery of positive electrode of LiFePO4 The perfect match of system.Therefore, the research of lithium iron phosphate positive material not only has important value in field of lithium ion battery, to the sun The development and application of the new energy technologies such as energy, wind energy, tide energy also has a very important significance.
At present apparently, LiFePO4 is most possible really large-scale application in power type and accumulation energy type lithium ion battery Ideal material.Since John professor B.Goodenough in the U.S. in 1997 proposes this material, both at home and abroad to this into Extensive and in-depth research is gone.People are by mixing conductive materials, crystal grain nanosizing to material progress surface packet conductive carbon, inside Etc. means improve material electric conductivity;The bulk density of material is improved by the particle shape of optimal control powder, particles size and distribution. People develop a variety of preparation processes, some have been applied to reality.
The mainstream process of preparing of LiFePO4 haves the shortcomings that common:
First is that reaction process has byproduct salt generation, such as NaNO3, NaCl, Na2SO4, byproduct salt is present in It reacts in the mother liquor generated, also largely exists in the cleaning solution of phosphoric acid iron product, direct emission will seriously pollute environment, waste liquid Processing will cause increased costs, and by-product is low-value product again;
Second is that the ferric phosphate generated all contains certain crystallization water, usually two, as FePO42H2O;Product removes Outside the crystallization water, usually also containing a small amount of absorption water;Since containing the crystallization water and absorption water, the actual constituent of ferric phosphate is not very It determines reliably, brings certain difficulty for accurate dosing when producing LiFePO4;
In addition, the product containing the crystallization water is in the long-term storage process, it is possible to create the moisture absorption or weathering phenomenon, make product at Divide and generate variation at any time, has an adverse effect to the stability and homogeneity of product of technique;Therefore, FePO42H2O is uncomfortable In the raw material for being directly used as production lithium iron phosphate positive material, necessary pretreatment is generally carried out.
And industrially production FePO42H2O generallys use ferrous sulfate (FeSO4) as raw material, and cost is relatively low.But it adopts With prior art, it is necessary to consume a large amount of oxidants such as hydrogen peroxide (H2O2), sodium hypochlorite (NaClO), sodium chlorate (NaClO3), mistake Ammonium sulfate ((NH4) 2S2O8) etc., increases cost to a certain extent.
In conclusion preparing lithium iron phosphate positive material using the ferric phosphate containing the crystallization water, there is at high cost, pollution greatly And in production process accurate dosing difficulty shortcoming.
Summary of the invention
It is an object of the invention to: a kind of battery-grade anhydrous iron phosphate to solve the above problem, quality is high, produces work Skill is simple, reduces cost and pollution.
The technical solution adopted by the present invention is that such:
Battery-grade anhydrous iron phosphate, anhydrous phosphoric acid iron powder body are made of the monodisperse olive shape particle of morphological rules, jolt ramming Density is up to 1.5-1.6g/cm3.Specific step is as follows for preparation method:
A, divalent iron salt and phosphoric acid or phosphate mixed aqueous solution are prepared;
B, secure ph adjusts agent solution;
C, by above-mentioned prepared divalent iron salt and phosphoric acid or phosphate mixed aqueous solution, pH adjusting agent solution pump point Be not successively inputted to stirring reactor in, by air compressor, with certain flow into reactor input air;Pass through Water bath with thermostatic control controls to adjust the temperature of reaction solution in reactor and is maintained at constant within the scope of 40-98 DEG C;Constant divalent iron salt with The flow of phosphoric acid or phosphate mixed aqueous solution and air, control to adjust reactor in reaction solution pH value be 0.5-7.5 simultaneously It keeps constant;Charging is completed, and is continued stirring and is aged and is continually fed into air oxidation, generates crystalline state compound NH4Fe2 (OH) (PO4)2·2H2O;
D, upper step resulting material is transferred in solid-liquid separator and is separated by solid-liquid separation, be washed with deionized and be separated by solid-liquid separation institute The solid product obtained, until using BaCl2Solution inspection does not measure the SO42- in washing water, or uses AgNO3Solution inspection does not measure washing Cl in water-Until;Product after washing is 2~10 hours dry in 80~120 DEG C in an oven, obtains NH4Fe2 (OH) (PO4) 22H2O powder;
E, by NH4Fe2 (OH) (PO4) 22H2O powder in air atmosphere, 500-700 DEG C is roasted 20~24 hours, point Solution removes ammonium root, hydroxyl and the crystallization water, obtains with battery-grade anhydrous iron phosphate.
Further, in the divalent iron salt and phosphoric acid or phosphate mixed aqueous solution the concentration of iron be 0.2-2 moles/ It rises, the molar ratio of phosphorus and iron is 0.95-1.05: 1 in the aqueous solution.
Further, the divalent iron salt is frerrous chloride, and the frerrous chloride, which is reacted by hydrochloric acid with metallic iron, to be made.
In conclusion due to the adoption of the above technical scheme, the beneficial effects of the present invention are:
The present invention prepares the battery-grade anhydrous phosphoric acid of high-quality using cheap divalent iron salt ferrous sulfate, frerrous chloride as raw material Iron only contains ammonium salt in the mother liquor and cleaning solution of generation, can be used as nitrogenous fertilizer and be directly used in agricultural and forestry production, do not pollute the environment, nothing Need liquid waste processing;
Preparation process is using air as oxidant, can significant save the cost without consuming additional oxidant;
Preparation gained is the anhydrous iron phosphate without containing the crystallization water and absorption water, and crystallinity and reactivity are high, and ingredient is true It is fixed reliable, stablize save-resistant, is the desirable feedstock for preparing LiFePO4, the stability for being conducive to improve technique is consistent with product Property;
This preparation method is suitable for the scale, economy, stabilization, reliable production of high-quality battery-grade iron phosphate, has apparent Advantage, it is very with practical value.
Specific embodiment
Battery-grade anhydrous iron phosphate, anhydrous phosphoric acid iron powder body are made of the monodisperse olive shape particle of morphological rules, accumulation Density is high, and tap density is up to 1.5-1.6g/cm3.
Embodiment 1
Battery-grade anhydrous iron phosphate preparation method,
Prepare ferrous sulfate, phosphoric acid, diammonium hydrogen phosphate mixed aqueous solution, wherein ferrous sulfate concentration be 1.0 mol/Ls, Phosphoric acid concentration is 0.5 mol/L, diammonium hydrogen phosphate concentration is 0.5 mol/L;
Compound concentration is the ammonia spirit of 4.0 mol/Ls as pH adjusting agent;
Add 1 liter of deionized water in advance in the reaction kettle that volume is 7 liters, it is strong to stir, and be passed through into reacting kettle jacketing Thermostatted water, controlling water temperature in reaction kettle is 45 DEG C;
By air compressor, using 10 liters/min of flow into reaction kettle input air as oxidant;
By ferrous sulfate, phosphoric acid, diammonium hydrogen phosphate mixed aqueous solution, ammonia spirit is successively inputted to reaction kettle with pump respectively In, control ferrous sulfate, phosphoric acid, diammonium hydrogen phosphate mixed aqueous solution flow be 20 ml/mins, adjust the stream of ammonia spirit Amount, the pH value for controlling reaction solution in reaction kettle is 2.30 ± 0.05;By water bath with thermostatic control, reaction solution in reaction kettle is controlled to adjust Temperature is simultaneously maintained within the scope of 44-46 DEG C;After 2 liters of ferrous sulfate, phosphoric acid, diammonium hydrogen phosphate mixed aqueous solution is added toward reaction kettle Stop charging;
It is passed through high-temperature constant warm water into reacting kettle jacketing, material in reactor is heated up, controls material in reactor temperature Within the scope of 94-96 DEG C, to continue stirring ageing 10 hours, while being continually fed into air;
After ageing, the material in reaction kettle is discharged, is separated by solid-liquid separation with centrifuge, with 60 DEG C of deionized water Washing is separated by solid-liquid separation resulting solid product, until not measuring the SO42- in washing water with BaCl2 inspection;
By the product after washing, condition is 4 hours dry at 120 DEG C in an oven, obtains NH4Fe2 (OH) (PO4) 2 2H2O powder;
NH4Fe2 (OH) (PO4) 22H2O powder is placed in corundum crucible, 500 DEG C of roastings in air atmosphere muffle furnace It burns 24 hours, decomposes and remove ammonium root, hydroxyl and the crystallization water, obtain that there is the battery-grade anhydrous phosphoric acid of the high-quality of rhombic form Iron.
The ammonia that Roasting Decomposition generates can use sulfuric acid absorption, generate ammonium sulfate;In mother liquor and cleaning solution after centrifuge separation Only contain ammonium sulfate;After two batches ammonium sulfate ammonia spirit tune pH value to neutrality, it can be used directly as nitrogenous fertilizer.
Embodiment 2
Battery-grade anhydrous iron phosphate preparation method,
Ferrous sulfate and ammonium dihydrogen phosphate mixed aqueous solution are prepared, wherein ferrous sulfate concentration is 1.5 mol/Ls, phosphoric acid Dihydro ammonium concentration is 1.5 mol/Ls;
Compound concentration is the urea liquid of 2.5 mol/Ls as pH adjusting agent;
Add 2 liters of deionized waters in advance in the reaction kettle that volume is 7 liters, it is strong to stir, and be passed through into reacting kettle jacketing Thermostatted water, controlling water temperature in reaction kettle is 90 DEG C.By air compressor, inputted with 10 liters/min of flow into reaction kettle Air is as oxidant;
Ferrous sulfate and ammonium dihydrogen phosphate mixed aqueous solution, urea liquid are successively inputted in reaction kettle respectively with pump, The flow for controlling ferrous sulfate and ammonium dihydrogen phosphate mixed aqueous solution is 20 ml/mins, adjusts the flow of urea liquid, is controlled The pH value of reaction solution is 5.00 ± 0.05 in reaction kettle processed;By water bath with thermostatic control, the temperature of reaction solution in reaction kettle is controlled to adjust And it is maintained within the scope of 89-91 DEG C;
Stop charging after 2 liters of ferrous sulfate and ammonium dihydrogen phosphate mixed aqueous solution are added toward reaction kettle, continues stirring ageing 8 Hour, while being continually fed into air;In ageing process, it should remain that the temperature of reaction solution within the scope of 89-91 DEG C, and is fitted When add urea liquid, the pH value for controlling reaction solution in reaction kettle is 5.00 ± 0.05;
After ageing, the material in reaction kettle is discharged, is separated by solid-liquid separation with centrifuge, with 60 DEG C of deionized water Washing is separated by solid-liquid separation resulting solid product, until not measuring the SO42- in washing water with the inspection of BaCl2 solution;
Product after washing is 4 hours dry under conditions of 105 DEG C in an oven, obtain NH4Fe2 (OH) (PO4) 22H2O powder;
NH4Fe2 (OH) (PO4) 22H2O powder is placed in corundum crucible, 600 DEG C of roastings in air atmosphere muffle furnace It burns 6 hours, decomposes and remove ammonium root, hydroxyl and the crystallization water, obtain the battery-grade anhydrous iron phosphate with rhombic form.
The ammonia that Roasting Decomposition generates can use sulfuric acid absorption, generate ammonium sulfate;In mother liquor and cleaning solution after centrifuge separation Only contain ammonium sulfate;After two batches ammonium sulfate ammonia spirit tune pH value to neutrality, it can be used directly as nitrogenous fertilizer.

Claims (4)

1. battery-grade anhydrous iron phosphate, it is characterised in that: anhydrous phosphoric acid iron powder body by morphological rules monodisperse olive shape particle Composition, tap density are up to 1.5-1.6g/cm3.
2. a kind of preparation method of battery-grade anhydrous iron phosphate as described in claim 1, it is characterised in that:
Specific step is as follows:
A, divalent iron salt and phosphoric acid or phosphate mixed aqueous solution are prepared;
B, secure ph adjusts agent solution;
C, above-mentioned prepared divalent iron salt and phosphoric acid or phosphate mixed aqueous solution, pH adjusting agent solution pump are connected respectively It is continuous to be input in the reactor that band stirs, by air compressor, with certain flow into reactor input air;Pass through constant temperature Water-bath controls to adjust the temperature of reaction solution in reactor and is maintained at constant within the scope of 40-98 DEG C;Constant divalent iron salt and phosphoric acid Or the flow of phosphate mixed aqueous solution and air, the pH value for controlling to adjust reaction solution in reactor are 0.5-7.5 and keep It is constant;Charging is completed, and is continued stirring and is aged and is continually fed into air oxidation, generates crystalline state compound NH4Fe2 (OH) (PO4) 2·2H2O;
D, upper step resulting material is transferred in solid-liquid separator and is separated by solid-liquid separation, it is resulting that separation of solid and liquid is washed with deionized Solid product, until using BaCl2Solution inspection does not measure the SO42- in washing water, or uses AgNO3Solution inspection does not measure in washing water Cl-Until;Product after washing is 2~10 hours dry in 80~120 DEG C in an oven, obtains NH4Fe2 (OH) (PO4) 2 2H2O powder;
E, by NH4Fe2 (OH) (PO4) 22H2O powder in air atmosphere, 500-700 DEG C is roasted 20~24 hours, and decomposition removes Ammonium root, hydroxyl and the crystallization water are removed, is obtained with battery-grade anhydrous iron phosphate.
3. a kind of preparation method of battery-grade anhydrous iron phosphate according to claim 2, it is characterised in that: the ferrous iron The concentration of iron is 0.2-2 mol/L in salt and phosphoric acid or phosphate mixed aqueous solution, and the molar ratio of phosphorus and iron is in the aqueous solution 0.95-1.05∶1。
4. a kind of preparation method of battery-grade anhydrous iron phosphate according to claim 2, it is characterised in that: the ferrous iron Salt is frerrous chloride, and the frerrous chloride, which is reacted by hydrochloric acid with metallic iron, to be made.
CN201810931479.9A 2018-08-15 2018-08-15 Battery-grade anhydrous iron phosphate and preparation method thereof Pending CN109305663A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110002420A (en) * 2019-05-07 2019-07-12 江西赣锋锂业股份有限公司 A method of anhydrous iron phosphate is prepared using steel plant's pickle liquor
CN112265974A (en) * 2020-10-27 2021-01-26 安徽同心新材料科技有限公司 Preparation method and application of amorphous iron phosphate
CN113336212A (en) * 2021-07-08 2021-09-03 河南佰利新能源材料有限公司 Method for preparing iron phosphate by recycling mother liquor
CN115259124A (en) * 2021-04-29 2022-11-01 四川大学 Preparation method and application of battery-grade iron phosphate precursor
CN115571864A (en) * 2022-09-05 2023-01-06 六盘水师范学院 Method for preparing battery-grade iron phosphate by using high-iron type fly ash as raw material

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CN101244813A (en) * 2007-02-15 2008-08-20 比亚迪股份有限公司 Alkali type iron ammonium phosphate and production method, production method of iron phosphate and production method of ferrous lithium phosphate
CN102491302A (en) * 2011-12-15 2012-06-13 湖北万润新能源科技发展有限公司 Battery-grade anhydrous iron phosphate and preparation method thereof
US20120237425A1 (en) * 2009-09-09 2012-09-20 Takahisa Nishio Ferric phosphate hydrate particles and process for producing the same, olivine type lithium iron phosphate particles and process for producing the same, and non-aqueous electrolyte secondary battery
CN102694169A (en) * 2012-03-07 2012-09-26 湖北万润新能源科技发展有限公司 FePO4/high polymer cracked carbon composite material and preparation method thereof, and NH4Fe2(OH)(PO4)2.2H2O/high polymer composite material and preparation method thereof
JP2014065641A (en) * 2012-09-27 2014-04-17 Murata Mfg Co Ltd Method for manufacturing iron phosphate, lithium iron phosphate, electrode active material, and secondary battery
CN103825024A (en) * 2014-02-24 2014-05-28 宁波工程学院 Battery-grade ferric phosphate and preparation method

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CN101244813A (en) * 2007-02-15 2008-08-20 比亚迪股份有限公司 Alkali type iron ammonium phosphate and production method, production method of iron phosphate and production method of ferrous lithium phosphate
US20120237425A1 (en) * 2009-09-09 2012-09-20 Takahisa Nishio Ferric phosphate hydrate particles and process for producing the same, olivine type lithium iron phosphate particles and process for producing the same, and non-aqueous electrolyte secondary battery
CN102491302A (en) * 2011-12-15 2012-06-13 湖北万润新能源科技发展有限公司 Battery-grade anhydrous iron phosphate and preparation method thereof
CN102694169A (en) * 2012-03-07 2012-09-26 湖北万润新能源科技发展有限公司 FePO4/high polymer cracked carbon composite material and preparation method thereof, and NH4Fe2(OH)(PO4)2.2H2O/high polymer composite material and preparation method thereof
JP2014065641A (en) * 2012-09-27 2014-04-17 Murata Mfg Co Ltd Method for manufacturing iron phosphate, lithium iron phosphate, electrode active material, and secondary battery
CN103825024A (en) * 2014-02-24 2014-05-28 宁波工程学院 Battery-grade ferric phosphate and preparation method

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110002420A (en) * 2019-05-07 2019-07-12 江西赣锋锂业股份有限公司 A method of anhydrous iron phosphate is prepared using steel plant's pickle liquor
CN112265974A (en) * 2020-10-27 2021-01-26 安徽同心新材料科技有限公司 Preparation method and application of amorphous iron phosphate
CN115259124A (en) * 2021-04-29 2022-11-01 四川大学 Preparation method and application of battery-grade iron phosphate precursor
CN113336212A (en) * 2021-07-08 2021-09-03 河南佰利新能源材料有限公司 Method for preparing iron phosphate by recycling mother liquor
CN115571864A (en) * 2022-09-05 2023-01-06 六盘水师范学院 Method for preparing battery-grade iron phosphate by using high-iron type fly ash as raw material

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