CN102786096A - Iron oxide for lithium iron phosphate battery, and its preparation method - Google Patents
Iron oxide for lithium iron phosphate battery, and its preparation method Download PDFInfo
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- CN102786096A CN102786096A CN2011101274700A CN201110127470A CN102786096A CN 102786096 A CN102786096 A CN 102786096A CN 2011101274700 A CN2011101274700 A CN 2011101274700A CN 201110127470 A CN201110127470 A CN 201110127470A CN 102786096 A CN102786096 A CN 102786096A
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Abstract
The invention discloses iron oxide for a lithium iron phosphate battery material, and its preparation method. The preparation method mainly comprises the following steps: 1, removing impurities from a steel plate pickling waste liquid to reduce the contents of impurities comprising SiO2, P2O5, Al2O3 and the like in iron oxide; 2, carrying out low temperature roasting of the impurities removed pickling waste liquid to improve physical performances of the iron oxide; 3, grinding with a pearl mill until the average particle size of the iron oxide reaches below 0.5mum; and 4, washing the iron oxide slurry obtained after the grinding with desalinized water, and carrying out treatments comprising press filtration, drying, crushing and the like. According to the invention, the contents of the impurities comprising SiO2, P2O5, Al2O3, Cl<->, Ca<2+>, K<+>, Na<+>, SO4<2-> and the like in the iron oxide are greatly reduced; and the physical performances comprising the specific surface area (BET), the loose specific weight, the average particle size particle size reduction and the like of the iron oxide are improved,
Description
Technical field
The present invention relates to a kind of ferric phosphate lithium cell with red stone and preparation method thereof, belong to the battery material field.
Background technology
Continually developing of new forms of energy is the important foundation and the inevitable outcome of human social; The lithium ion battery of exploitation has obtained using widely in recent years, has also represented the topmost new forms of energy developing direction in fields such as following power truck, electric bicycle, power tool and generating and energy storage device.Particularly LiFePO 4 material because have that security is good, cycle performance is excellent, characteristics such as environmental friendliness, raw material resources are abundant; Be acknowledged as the first-selected positive electrode material of lithium-ion-power cell of new generation, become each national research emphasis and developing direction in the world today.Require high purity and high reactive behavior owing to be used for the red stone of ferric phosphate lithium cell material, the red stone that therefore is used for the ferric phosphate lithium cell material generally adopts coprecipitation method and nano-pulverization technology to obtain highly purified red stone.But coprecipitation method and nano-pulverization technical costs height and exhaust emission are serious.The content of the present invention research is through acquisition red stone that the steel plate acid-washing spent acid is regenerated, and red stone purified and grind obtains high purity and the good red stone of reactive behavior, can be used for the production of ferric phosphate lithium cell material positive electrode material.
Summary of the invention
The objective of the invention is in order to provide a kind of ferric phosphate lithium cell to use red stone.Another object of the present invention provides the preparation method of this ferric phosphate lithium cell with red stone, to satisfy the stable requirement that reaches high conformity of less energy-consumption, high yield, product performance that suitability for industrialized production requires.
The object of the invention can be realized through following technical scheme.
A kind of ferric phosphate lithium cell is used red stone, wherein, and SiO
2<0.005%, Cl
-<0.03%, Ca
2+<0.01%, K
+<0.005%, Na
+<0.005%, SO
4 2-<0.01%; Wherein: specific surface area is 5.0m
2/ g is above, the pine dress is than being 0.35～0.75g/cm
3, median size is 0.3～0.5um; Can be used for producing the ferric phosphate lithium cell positive electrode material.
A kind of ferric phosphate lithium cell the steps include: with the preparation method of red stone
A) at first spent acid behind the steel plate acid-washing is heated, after the heating spent acid solution is beaten to lixator, add the scrap iron limit in the lixator simultaneously, spent acid gets into from the lixator bottom, and in uphill process, free acid in the spent acid and iron reaction generate ferrous chloride;
B) spent acid flow to retort certainly from the lixator top through water cooler; For improving the pH value in the spent acid; Ammonia soln by the continuous adding 20% in the ammonia react jar of ammonia volume pump; Spent acid is constantly passing through to add pressurized air under the condition of stirring, and the part ferrous chloride is oxidized to iron trichloride and changes into ironic hydroxide, and iron hydroxide particle is with the SiO in the spent acid
2Particle wraps up and combines to generate short grained flco;
C) for making flco grow up to macrobead, add flocculation agent again, the retort overflow makes iron hydroxide particle and SiO to settling bath
2Particle flocking settling in sedimentary deposit tank separates with spent acid, and the pot bottom bulky ferric hydroxide precipitate is squeezed into plate-and-frame filter press with steam piano, filters, and filtered liq flows into holding tank, and filter cake is drained as industrial refuse;
D) the clear liquid overflow of settling bath top has been removed SiO to holding tank in the holding tank
2The spent acid of spent acid after with silica removal be pumped to the spent acid jar behind the silica removal;
E) spent acid solution behind the silica removal gets into the stoving oven low-temp reaction after preconcentrator concentrates, and generates Fe
2O
3And Cl
2Gas, Cl
2Gas absorbs generation HCl through water and returns steel plate acid-washing.
F) red stone after the roasting uses the pearl mill to grind 6～12 hours;
G) slip after will grinding was washed 1～6 hour, and the de-salted water of washing usefulness is 2～10 times of red iron oxide dry powder weight;
H) slip after will washing precipitates 1～7 day, makes the supernatant overflow, and the mud of post precipitation carries out filter-press dehydration, and the filter cake moisture content after the control dehydration is less than 15%;
I) broken filter cake is rotated expansion drying, and the water ratio of controlling dried red iron oxide is less than 0.3%;
J) with dried red iron oxide through vacuum fan suction red iron oxide finished product bin, get final product after the cooling.
Spent acid behind the steel plate acid-washing described in the step a) is heated to 50 ~ 90 ℃.
In the step b) after overcooling the spent acid temperature be 20 ~ 50 ℃.
Waste acid liquor pH value in the step b) after the process retort is 4.0 ~ 5.0.
Maturing temperature in the step e) is 500 ℃ ~ 600 ℃.
In the step f), the grinding medium that grinds is a zirconia ball, and sphere diameter is 0.8～5mm.
In the step g), mixing speed is 120 ~ 200 rev/mins when washing.
The filter cloth that press filtration is used is the polypropylene fibre filter cloth as filter cloth, and model is 108C.
The model of described flocculation agent is N8173.
Compared with prior art, beneficial effect of the present invention is following:
The red stone that adopts aftertreatment technology of the present invention to obtain, impurities have obtained reducing significantly, and particularly metals ion has had control preferably, wherein: SiO
2<0.005%, Cl
-<0.03%, Ca
2+<0.01%, K
+<0.005%, Na
+<0.005%, SO
4 2-<0.01%; And improved the physicals of red iron oxide, wherein: specific surface area reaches 5.0m
2/ g is above, the pine dress is than being 0.35～0.75g/cm
3, median size is 0.3～0.5um; Can be used for producing the ferric phosphate lithium cell positive electrode material.In addition, technology of the present invention has that energy consumption is low, yield is high, product performance are stable and advantage such as high conformity, meets the suitability for industrialized production requirement.
Embodiment
Further set forth technical characterstic of the present invention below in conjunction with specific embodiment.
Embodiment 1
A) at first spent acid behind the steel plate acid-washing is heated to 70 ℃, after the heating spent acid solution is beaten to lixator, add the scrap iron limit in the lixator simultaneously, spent acid gets into from the lixator bottom, and in uphill process, free acid in the spent acid and iron reaction generate ferrous chloride.
B) spent acid is cooled to 30 ℃ from the lixator top through water cooler, and the cooling back is from flowing to retort.Ammonia soln by the continuous adding 20% in the ammonia react jar of ammonia volume pump; Improve the pH value to 5.0 in the spent acid; Spent acid is constantly passing through to add pressurized air under the condition of stirring, and the part ferrous chloride is oxidized to iron trichloride and changes into ironic hydroxide, and iron hydroxide particle is with the SiO in the spent acid
2Particle wraps up and combines to generate short grained flco.
C) for making flco grow up to macrobead, add N8173 again, the retort overflow makes iron hydroxide particle and SiO to settling bath
2Particle flocking settling in sedimentary deposit tank separates with spent acid, and the pot bottom bulky ferric hydroxide precipitate is squeezed into plate-and-frame filter press with steam piano, filters, and filtered liq flows into holding tank, and filter cake is drained as industrial refuse.
D) the clear liquid overflow of settling bath top is to holding tank.Removed SiO in the holding tank
2The spent acid of spent acid after with silica removal be pumped to the spent acid jar behind the silica removal.
E) spent acid solution behind the silica removal gets into stoving oven after preconcentrator concentrates, and maturing temperature is 600 ℃, generates Fe
2O
3And Cl
2Gas, Cl
2Gas absorbs generation HCl through water and returns steel plate acid-washing.
F) red stone after the roasting uses the pearl mill to grind 12 hours; Grinding medium is 5mm.
G) slip after will grinding adds 10 times de-salted water and stirs fast, and the stirrer rotating speed is 120 rev/mins, and churning time is 6 hours;
H) slip after will stirring precipitates 7 days, makes the supernatant overflow, and the mud of post precipitation carries out filter-press dehydration, and the filter cake moisture content after the control dehydration is less than 15%;
I) broken filter cake is rotated expansion drying, and the water ratio of controlling dried red iron oxide is less than 0.3%;
J) with dried red iron oxide through vacuum fan suction red iron oxide finished product bin, get final product after the cooling.
Learn through check and analysis, in the red iron oxide after handling through present embodiment: SiO
2: P 0.003%,
2O
5: Al 0.004%,
2O
3: Cl 0.01%,
-: Ca 0.03%,
2+: K 0.01%,
+: Na 0.005%,
+: SO 0.005%,
4 2-: 0.01%; Specific surface area: 6.5m
2/ g, pine dress are than being 0.70g/cm
3, median size is: 0.5um.
Embodiment 2
A) at first spent acid behind the steel plate acid-washing is heated to 60 ℃, after the heating spent acid solution is beaten to lixator, add the scrap iron limit in the lixator simultaneously, spent acid gets into from the lixator bottom, and in uphill process, free acid in the spent acid and iron reaction generate ferrous chloride.
B) spent acid is cooled to 40 ℃ from the lixator top through water cooler, and the cooling back is from flowing to retort.Ammonia soln by the continuous adding 20% in the ammonia react jar of ammonia volume pump; Improve the pH value to 4.5 in the spent acid; Spent acid is constantly passing through to add pressurized air under the condition of stirring; The part ferrous chloride is oxidized to iron trichloride and changes into ironic hydroxide, and iron hydroxide particle wraps up the SiO2 particle in the spent acid and combines to generate short grained flco.
C) for making flco grow up to macrobead, add N8173 again, the retort overflow makes iron hydroxide particle and SiO to settling bath
2Particle flocking settling in sedimentary deposit tank separates with spent acid, and the pot bottom bulky ferric hydroxide precipitate is squeezed into plate-and-frame filter press with steam piano, filters, and filtered liq flows into holding tank, and filter cake is drained as industrial refuse.
D) the clear liquid overflow of settling bath top is to holding tank.Removed SiO in the holding tank
2The spent acid of spent acid after with silica removal be pumped to the spent acid jar behind the silica removal.
E) spent acid solution behind the silica removal gets into stoving oven after preconcentrator concentrates, and maturing temperature is 550 ℃, generates Fe
2O
3And Cl
2Gas, Cl
2Gas absorbs generation HCl through water and returns steel plate acid-washing.
F) red stone after the roasting uses the pearl mill to grind 6 hours; Grinding medium is 3mm.
G) slip after will grinding adds 8 times de-salted water and stirs fast, and the stirrer rotating speed is 200 rev/mins, and churning time is 4 hours;
H) slip after will stirring precipitates 5 days, makes the supernatant overflow, and the mud of post precipitation carries out filter-press dehydration, and the filter cake moisture content after the control dehydration is less than 15%;
I) broken filter cake is rotated expansion drying, and the water ratio of controlling dried red iron oxide is less than 0.3%;
J) with dried red iron oxide through vacuum fan suction red iron oxide finished product bin, get final product after the cooling.
Learn through check and analysis, in the red iron oxide after handling through present embodiment: SiO
2: P 0.004%,
2O
5: Al 0.005%,
2O
3: Cl 0.01%,
-: Ca 0.04%,
2+: K 0.01%,
+: Na 0.005%,
+: SO 0.005%,
4 2-: 0.01%; Specific surface area: 6.0m
2/ g, pine dress are than being 0.60g/cm
3, median size is: 0.5um.
Embodiment 3
A) at first spent acid behind the steel plate acid-washing is heated to 80 ℃, after the heating spent acid solution is beaten to lixator, add the scrap iron limit in the lixator simultaneously, spent acid gets into from the lixator bottom, and in uphill process, free acid in the spent acid and iron reaction generate ferrous chloride.
B) spent acid is cooled to 20 ℃ from the lixator top through water cooler, and the cooling back is from flowing to retort.Ammonia soln by the continuous adding 20% in the ammonia react jar of ammonia volume pump; Improve the pH value to 4.0 in the spent acid; Spent acid is constantly passing through to add pressurized air under the condition of stirring; The part ferrous chloride is oxidized to iron trichloride and changes into ironic hydroxide, and iron hydroxide particle wraps up the SiO2 particle in the spent acid and combines to generate short grained flco.
C) for making flco grow up to macrobead, add N8173 again, the retort overflow makes iron hydroxide particle and SiO to settling bath
2Particle flocking settling in sedimentary deposit tank separates with spent acid, and the pot bottom bulky ferric hydroxide precipitate is squeezed into plate-and-frame filter press with steam piano, filters, and filtered liq flows into holding tank, and filter cake is drained as industrial refuse.
D) the clear liquid overflow of settling bath top is to holding tank.Removed SiO in the holding tank
2The spent acid of spent acid after with silica removal be pumped to the spent acid jar behind the silica removal.
E) spent acid solution behind the silica removal gets into stoving oven after preconcentrator concentrates, and maturing temperature is 500 ℃, generates Fe
2O
3And Cl
2Gas, Cl
2Gas absorbs generation HCl through water and returns steel plate acid-washing.
F) red stone after the roasting uses the pearl mill to grind 10 hours; Grinding medium is 0.8mm.
G) slip after will grinding adds 5 times de-salted water and stirs fast, and the stirrer rotating speed is 180 rev/mins, and churning time is 2 hours;
H) slip after will stirring precipitates 3 days, makes the supernatant overflow, and the mud of post precipitation carries out filter-press dehydration, and the filter cake moisture content after the control dehydration is less than 15%;
I) broken filter cake is rotated expansion drying, and the water ratio of controlling dried red iron oxide is less than 0.3%;
J) with dried red iron oxide through vacuum fan suction red iron oxide finished product bin, get final product after the cooling.
Learn through check and analysis, in the red iron oxide after handling through present embodiment: SiO
2: P 0.002%,
2O
5: Al 0.003%,
2O
3: Cl 0.01%,
-: Ca 0.03%,
2+: K 0.01%,
+: Na 0.005%,
+: SO 0.005%,
4 2-: 0.01%; Specific surface area: 6.5m
2/ g, pine dress are than being 0.70g/cm
3, median size is: 0.5um.
Claims (10)
1. a ferric phosphate lithium cell is used red stone, it is characterized in that: wherein, and SiO
2<0.005%, Cl
-<0.03%, Ca
2+<0.01%, K
+<0.005%, Na
+<0.005%, SO
4 2-<0.01%; Specific surface area is 5.0m
2/ g is above, the pine dress is than being 0.35～0.75g/cm
3, median size is 0.3～0.5um; Can be used for producing the ferric phosphate lithium cell positive electrode material.
2. the described ferric phosphate lithium cell of claim 1 is characterized in that: the steps include: with the preparation method of red stone
A) at first spent acid behind the steel plate acid-washing is heated, after the heating spent acid solution is beaten to lixator, add the scrap iron limit in the lixator simultaneously, spent acid gets into from the lixator bottom, and in uphill process, free acid in the spent acid and iron reaction generate ferrous chloride;
B) spent acid flow to retort certainly from the lixator top through water cooler; Ammonia soln by the continuous adding 20% in the ammonia react jar of ammonia volume pump; Spent acid is constantly passing through to add pressurized air under the condition of stirring; The part ferrous chloride is oxidized to iron trichloride and changes into ironic hydroxide, and iron hydroxide particle is with the SiO in the spent acid
2Particle wraps up and combines to generate short grained flco;
C) add flocculation agent again, the retort overflow makes iron hydroxide particle and SiO to settling bath
2Particle flocking settling in sedimentary deposit tank separates with spent acid, and the pot bottom bulky ferric hydroxide precipitate is squeezed into plate-and-frame filter press with steam piano, filters, and filtered liq flows into holding tank, and filter cake is drained as industrial refuse;
D) the clear liquid overflow of settling bath top has been removed SiO to holding tank in the holding tank
2The spent acid of spent acid after with silica removal be pumped to the spent acid jar behind the silica removal;
E) spent acid solution behind the silica removal gets into the stoving oven low-temp reaction after preconcentrator concentrates, and generates Fe
2O
3And Cl
2Gas, Cl
2Gas absorbs generation HCl through water and returns steel plate acid-washing;
F) red stone after the roasting uses the pearl mill to grind 6～12 hours;
G) slip after will grinding was washed 1～6 hour, and the de-salted water of washing usefulness is 2～10 times of red iron oxide dry powder weight;
H) slip after will washing precipitates 1～7 day, makes the supernatant overflow, and the mud of post precipitation carries out filter-press dehydration, and the filter cake moisture content after the control dehydration is less than 15%;
I) broken filter cake is rotated expansion drying, and the water ratio of controlling dried red iron oxide is less than 0.3%;
J) with dried red iron oxide through vacuum fan suction red iron oxide finished product bin, get final product after the cooling.
3. preparation method according to claim 2 is characterized in that: the spent acid behind the steel plate acid-washing described in the step a) is heated to 50 ~ 90 ℃.
4. preparation method according to claim 2 is characterized in that: in the step b) after overcooling the spent acid temperature be 20 ~ 50 ℃.
5. preparation method according to claim 2 is characterized in that: the waste acid liquor pH value in the step b) after the process retort is 4.0 ~ 5.0.
6. preparation method according to claim 2 is characterized in that: the maturing temperature in the step e) is 500 ℃ ~ 600 ℃.
7. preparation method according to claim 2 is characterized in that: in the step f), the grinding medium that grinds is a zirconia ball, and sphere diameter is 0.8～5mm.
8. preparation method according to claim 2 is characterized in that: in the step g), mixing speed is 120 ~ 200 rev/mins when washing.
9. preparation method according to claim 2 is characterized in that: the filter cloth that press filtration is used is the polypropylene fibre filter cloth as filter cloth, and model is for being 108C.
10.1 preparation method according to claim 2 is characterized in that: described flocculation agent is N8173.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105399143A (en) * | 2015-12-15 | 2016-03-16 | 上海宝钢磁业有限公司 | Iron oxide red for lithium iron phosphate and preparation method and application thereof |
| CN108046230A (en) * | 2017-12-16 | 2018-05-18 | 蒋央芳 | A kind of method that one-step method prepares nanometer anhydrous iron phosphate |
| CN109019547A (en) * | 2018-08-29 | 2018-12-18 | 郑忆依 | A kind of utilization method of waste battery grade ferric phosphate |
| CN109576511A (en) * | 2018-12-05 | 2019-04-05 | 核工业北京化工冶金研究院 | A kind of In Pregnant Solution From In-situ Leaching method for removing iron |
| CN110021747A (en) * | 2019-04-25 | 2019-07-16 | 东北大学秦皇岛分校 | A method of lithium iron phosphate positive material is prepared with acid washing iron red for raw material |
| CN111573739A (en) * | 2020-06-09 | 2020-08-25 | 首钢集团有限公司 | Method for producing iron oxide red from high manganese steel waste acid liquid |
| CN112897594A (en) * | 2021-04-01 | 2021-06-04 | 安徽工业大学 | Method for synchronously preparing iron oxide red and sodium disilicate by utilizing desiliconized sludge |
| CN115286045A (en) * | 2022-07-13 | 2022-11-04 | 首钢京唐钢铁联合有限责任公司 | Method for preparing high-purity iron oxide red from cold rolling waste pickling liquor |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105399143A (en) * | 2015-12-15 | 2016-03-16 | 上海宝钢磁业有限公司 | Iron oxide red for lithium iron phosphate and preparation method and application thereof |
| CN105399143B (en) * | 2015-12-15 | 2018-05-11 | 上海宝钢磁业有限公司 | A kind of LiFePO4 iron oxide red and preparation method and application |
| CN108046230A (en) * | 2017-12-16 | 2018-05-18 | 蒋央芳 | A kind of method that one-step method prepares nanometer anhydrous iron phosphate |
| CN108046230B (en) * | 2017-12-16 | 2021-01-29 | 蒋央芳 | Method for preparing nano anhydrous iron phosphate by one-step method |
| CN109019547A (en) * | 2018-08-29 | 2018-12-18 | 郑忆依 | A kind of utilization method of waste battery grade ferric phosphate |
| CN109576511A (en) * | 2018-12-05 | 2019-04-05 | 核工业北京化工冶金研究院 | A kind of In Pregnant Solution From In-situ Leaching method for removing iron |
| CN110021747A (en) * | 2019-04-25 | 2019-07-16 | 东北大学秦皇岛分校 | A method of lithium iron phosphate positive material is prepared with acid washing iron red for raw material |
| CN111573739A (en) * | 2020-06-09 | 2020-08-25 | 首钢集团有限公司 | Method for producing iron oxide red from high manganese steel waste acid liquid |
| CN112897594A (en) * | 2021-04-01 | 2021-06-04 | 安徽工业大学 | Method for synchronously preparing iron oxide red and sodium disilicate by utilizing desiliconized sludge |
| CN115286045A (en) * | 2022-07-13 | 2022-11-04 | 首钢京唐钢铁联合有限责任公司 | Method for preparing high-purity iron oxide red from cold rolling waste pickling liquor |
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Application publication date: 20121121 |