CN104860285A - Drying method for lithium iron phosphate precursor slurry - Google Patents
Drying method for lithium iron phosphate precursor slurry Download PDFInfo
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- CN104860285A CN104860285A CN201510167416.7A CN201510167416A CN104860285A CN 104860285 A CN104860285 A CN 104860285A CN 201510167416 A CN201510167416 A CN 201510167416A CN 104860285 A CN104860285 A CN 104860285A
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- Prior art keywords
- slurry
- drying
- lithium phosphate
- drying means
- ferric lithium
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- 239000002002 slurry Substances 0.000 title claims abstract description 71
- 238000001035 drying Methods 0.000 title claims abstract description 63
- 239000002243 precursor Substances 0.000 title claims abstract description 26
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 title claims abstract description 5
- 238000000034 method Methods 0.000 claims abstract description 31
- 238000003756 stirring Methods 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims abstract description 9
- 239000006228 supernatant Substances 0.000 claims abstract description 3
- 239000007787 solid Substances 0.000 claims description 22
- 229910001386 lithium phosphate Inorganic materials 0.000 claims description 13
- TWQULNDIKKJZPH-UHFFFAOYSA-K trilithium;phosphate Chemical compound [Li+].[Li+].[Li+].[O-]P([O-])([O-])=O TWQULNDIKKJZPH-UHFFFAOYSA-K 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 12
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000003860 storage Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- LDHBWEYLDHLIBQ-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide;hydrate Chemical compound O.[OH-].[O-2].[Fe+3] LDHBWEYLDHLIBQ-UHFFFAOYSA-M 0.000 claims description 6
- 239000000839 emulsion Substances 0.000 claims description 5
- 229910000398 iron phosphate Inorganic materials 0.000 claims description 4
- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical group [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 claims description 4
- 238000004062 sedimentation Methods 0.000 claims description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 238000005245 sintering Methods 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 238000013517 stratification Methods 0.000 claims description 2
- 238000005265 energy consumption Methods 0.000 abstract description 12
- 238000004519 manufacturing process Methods 0.000 abstract description 10
- 238000009776 industrial production Methods 0.000 abstract 1
- 230000002708 enhancing effect Effects 0.000 description 5
- 229910010707 LiFePO 4 Inorganic materials 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
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- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a drying method for a lithium iron phosphate precursor slurry. The method is characterized by dividing a traditional drying process into four processes, wherein the steps the processes: 1, subjecting ground and mixed precursor slurry to settling and layering by standing and other means, and eliminating layered supernatant liquid; and 2, uniformly mixing the rest of the slurry under stirring, and carrying out drying by using a common drying device. The method provided by the invention does not require complicated equipment and process flow and has small investment; meanwhile, in the continuous operation of industrial production, the method can greatly decrease required time and energy consumption of drying, thereby improving production efficiency and reducing production cost.
Description
Technical field
The present invention relates to material technical field of drying, particularly relate to a kind of drying means of ferric lithium phosphate precursor slurry.
Background technology
LiFePO 4 material is one of the most promising positive electrode material in current field of lithium ion secondary, according to the development in current power battery and energy-storage battery market, estimates that the demand to LiFePO 4 material also can present the growth of blowout formula.The present stage industry preparation of iron lithium phosphate is based on solid phase method, and it has different preparation flows according to different technique, and some technique also needs to carry out secondary wet process ground and mixed to Preburning material.Comparatively conventional is Ferrox technique, tertiary iron phosphate technique, iron oxide red technique etc.Mixed solvent mostly is water or ethanol, methyl alcohol, acetone and other organic solvent.In order to prevent mixing step putty, the slurry solid content configured is lower, during follow-up dry consumption energy consumption.Steaming method under drying principles many employings constant-pressure and high-temperature, low-voltage high-temperature, low pressure normal temperature condition, equipment is as Bicone drying unit, rake drying plant, spraying type drying plant, track type drying plant.Wherein spray drying device can not the too high slurry of dry solid content, and energy consumption is high, and equipment price is expensive, and treatment capacity is less, and cost of equipment maintenance is high, does not meet the requirement of industrial green energy conservation low cost.Track type drying plant requires that solid content is more high better, but the slurry that general industryization is produced is difficult to reach higher solid content, therefore also can bring the problem that energy consumption is high, and this equipment price is expensive.Comparatively traditional bipyramid is dry and rake is dry, and drying efficiency is low, and energy consumption is high, and time of drying is long, but equipment price is cheap.
In sum, under existing dry technology, material produce is because drying section duration, and the features such as energy consumption is large, become the short slab of whole material producing line, directly affects whole piece and produces the production capacity of line and the cost of product.
Summary of the invention
Technical problem to be solved by this invention is the drying means providing a kind of ferric lithium phosphate precursor slurry.
Object of the present invention can be achieved through the following technical solutions:
A drying means for ferric lithium phosphate precursor slurry, specifically comprises following steps:
1), by the precursor pulp mixed 1. be transferred in storage tank and leave standstill, add emulsion splitter simultaneously, use ultrasonic, electric sedimentation or change the methods such as temperature to accelerate the sedimentation layering of slurry;
2), complete stratification after, directly pour out supernatant liquid or discharge clear liquid by valve on container; Thus the slurry obtaining lower floor's high solids content 2.;
3), by the slurry of lower floor's high solids content 2. stir for some time, mix;
4), by 2. dry for the slurry of lower floor's high solids content of mixing.
Preferably, described ferric lithium phosphate precursor refers to not through reaction raw materials or the Preburning material of the iron lithium phosphate of final sintering processes.
Preferably, 1. described precursor pulp can be Ferrox technique, iron oxide red technique, tertiary iron phosphate process slurry, or the one of the slurry of regrind batch mixing after pre-burning.
Preferably, described precursor pulp solvent 1. can be water, methyl alcohol, ethanol, acetone, Virahol one or both.
Preferably, described precursor pulp solid content is 1. 1%-60%.
Preferably, described precursor pulp 1. in powder body material granular size between 10 nanometers to 100 micron.
Preferably, described time of repose is 0.5-240 hour.
Beneficial effect of the present invention: 1, do not need large-scale expensive device, only need need to be equipped with multiple storage tank with agitator according to production technique can realize.
2, technique and simple to operate.
3, under continuous seepage condition, the method greatly can shorten time of drying and reduce energy consumption for drying, thus enhances productivity, and reduces production cost.
Embodiment
For the ease of the understanding of content of the present invention, below in conjunction with embodiment, the invention will be further described, and following examples are only a part of embodiment of the present invention.
Embodiment 1
With the slurry of tertiary iron phosphate technique water system mixing 1., have the solid content of 40%, the D50 of slurry granularity is in 500 nanometers.After standing 36h, slurry is layering 1..The water on upper strata is discharged and is reclaimed, and slurry 2 solid content of lower floor is increased to 70%.The stirring of storage tank is opened, slurry 2. dispersed with stirring 4 hours.2. utilize track type drying plant to carry out drying in scattered slurry, time of drying foreshortens to the 5h of slurry 2. needed for drying by the 10h of slurry 1. needed for convection drying.And because the continuity of producing, the time needed for leaving standstill can be ignored.Greatly save time of drying and reduce energy consumption for drying, thus enhancing productivity, reducing production cost.
Embodiment 2
With the slurry of iron oxide red technique water system mixing 1., have the solid content of 30%, the D50 of slurry granularity is at 2 microns.Add a small amount of ethanol as after emulsion splitter also standing 24h, slurry is layering 1..The clear liquid on upper strata is discharged and is reclaimed, and the slurry of lower floor 2. solid content is increased to 80%.The stirring of storage tank is opened, slurry 2. dispersed with stirring 24 hours.2. utilize bipyramid equipment to carry out drying in scattered slurry, time of drying foreshortens to the 4h of slurry 2. needed for drying by the 10h of slurry 1. needed for convection drying.And because the continuity of producing, the time needed for leaving standstill can be ignored.Greatly save time of drying and reduce energy consumption for drying, thus enhancing productivity, reducing production cost.
Embodiment 3
With the slurry of Ferrox technique ethanol system mixing 1., have the solid content of 20%, the D50 of slurry granularity is at 4 microns.Add a small amount of water as after emulsion splitter also standing 12h, slurry is layering 1..The clear liquid on upper strata is discharged and is reclaimed, and the slurry of lower floor 2. solid content is increased to 80%.The stirring of storage tank is opened, slurry 2. dispersed with stirring 12 hours.2. utilize rake drying plant to carry out drying in scattered slurry, time of drying foreshortens to the 4h of slurry 2. needed for drying by the 16h of slurry 1. needed for convection drying.And because the continuity of producing, the time needed for leaving standstill can be ignored.Greatly save time of drying and reduce energy consumption for drying, thus enhancing productivity, reducing production cost.
Embodiment 4
With the slurry of Ferrox process methanol system mixing 1., have the solid content of 20%, the D50 of slurry granularity is at 10 microns.Add a small amount of water as after emulsion splitter also standing 48h, slurry is layering 1..The clear liquid on upper strata is discharged and is reclaimed, and the slurry of lower floor 2. solid content is increased to 90%.The stirring of storage tank is opened, slurry 2. dispersed with stirring 48 hours.2. utilize track type drying plant to carry out drying in scattered slurry, time of drying foreshortens to the 2h of slurry 2. needed for drying by the 16h of slurry 1. needed for convection drying.And because the continuity of producing, the time needed for leaving standstill can be ignored.Greatly save time of drying and reduce energy consumption for drying, thus enhancing productivity, reducing production cost.
Embodiment 5
Carry out the slurry of regrind mixing 1. with the Preburning material ethanol system of Ferrox technique to Preburning material, have the solid content of 50%, the D50 of slurry granularity is at 5 microns.After slurry leaves standstill 12h, slurry is layering 1..The clear liquid on upper strata is discharged and is reclaimed, and the slurry of lower floor 2. solid content is increased to 90%.The stirring of storage tank is opened, slurry 2. dispersed with stirring 24 hours.Utilize track type drying plant to carry out drying in scattered slurry 2, time of drying foreshortens to the 2h of slurry 2. needed for drying by the 8h of slurry 1. needed for convection drying.And because the continuity of producing, the time needed for leaving standstill can be ignored.Greatly save time of drying and reduce energy consumption for drying, thus enhancing productivity, reducing production cost.
Above content is only citing made for the present invention and explanation; affiliated those skilled in the art make various amendment to described specific embodiment or supplement or adopt similar mode to substitute; only otherwise depart from the design of invention or surmount this scope as defined in the claims, protection scope of the present invention all should be belonged to.
Claims (7)
1. a drying means for ferric lithium phosphate precursor slurry, is characterized in that, specifically comprises following steps:
1), by the precursor pulp mixed 1. be transferred in storage tank and leave standstill, add emulsion splitter simultaneously, use ultrasonic, electric sedimentation or change the methods such as temperature to accelerate the sedimentation layering of slurry;
2), complete stratification after, directly pour out supernatant liquid or discharge clear liquid by valve on container; Thus the slurry obtaining lower floor's high solids content 2.;
3), by the slurry of lower floor's high solids content 2. stir for some time, mix;
4), by 2. dry for the slurry of lower floor's high solids content of mixing.
2. the drying means of a kind of ferric lithium phosphate precursor slurry according to claim 1, is characterized in that, described ferric lithium phosphate precursor refers to not through reaction raw materials or the Preburning material of the iron lithium phosphate of final sintering processes.
3. the drying means of a kind of ferric lithium phosphate precursor slurry according to claim 1, it is characterized in that, 1. described precursor pulp can be Ferrox technique, iron oxide red technique, tertiary iron phosphate process slurry, or the one of the slurry of regrind batch mixing after pre-burning.
4. the drying means of a kind of ferric lithium phosphate precursor slurry according to claim 1, is characterized in that, described precursor pulp solvent 1. can be water, methyl alcohol, ethanol, acetone, Virahol one or both.
5. the drying means of a kind of ferric lithium phosphate precursor slurry according to claim 1, is characterized in that, described precursor pulp solid content is 1. 1%-60%.
6. the drying means of a kind of ferric lithium phosphate precursor slurry according to claim 1, is characterized in that, described precursor pulp 1. in powder body material granular size between 10 nanometers to 100 micron.
7. the drying means of a kind of ferric lithium phosphate precursor slurry according to claim 1, it is characterized in that, described time of repose is 0.5-240 hour.
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| CN201510167416.7A CN104860285A (en) | 2015-04-10 | 2015-04-10 | Drying method for lithium iron phosphate precursor slurry |
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| CN201510167416.7A CN104860285A (en) | 2015-04-10 | 2015-04-10 | Drying method for lithium iron phosphate precursor slurry |
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101428782A (en) * | 2008-12-15 | 2009-05-13 | 中国海洋石油总公司 | Coprecipitation process for producing lithium cell anode material of lithium iron phosphate |
| CN101891181A (en) * | 2010-08-11 | 2010-11-24 | 河北工业大学 | Preparation method of pure-phase high-crystallinity lithium iron phosphate |
| CN101913588A (en) * | 2010-07-08 | 2010-12-15 | 中国科学院宁波材料技术与工程研究所 | Method for preparing lithium iron phosphate nano material |
| CN102295280A (en) * | 2011-06-15 | 2011-12-28 | 湖南红太阳光电科技有限公司 | Method for improving electrochemical performance of lithium ion battery cathode material lithium iron phosphate |
| CN102709557A (en) * | 2012-06-05 | 2012-10-03 | 无锡合志科技有限公司 | Preparation method for anode paste of lithium iron phosphate battery |
| CN102969502A (en) * | 2012-11-26 | 2013-03-13 | 厦门钨业股份有限公司 | Preparation method of high-vibration-compaction low-specific-surface-area lithium iron phosphate made by positive pole material |
| CN103825024A (en) * | 2014-02-24 | 2014-05-28 | 宁波工程学院 | Battery-grade ferric phosphate and preparation method |
| CN104425820A (en) * | 2013-09-09 | 2015-03-18 | 北京国能电池科技有限公司 | Lithium ferric manganese phosphate material and preparation method thereof and lithium ion battery cathode material |
-
2015
- 2015-04-10 CN CN201510167416.7A patent/CN104860285A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101428782A (en) * | 2008-12-15 | 2009-05-13 | 中国海洋石油总公司 | Coprecipitation process for producing lithium cell anode material of lithium iron phosphate |
| CN101913588A (en) * | 2010-07-08 | 2010-12-15 | 中国科学院宁波材料技术与工程研究所 | Method for preparing lithium iron phosphate nano material |
| CN101891181A (en) * | 2010-08-11 | 2010-11-24 | 河北工业大学 | Preparation method of pure-phase high-crystallinity lithium iron phosphate |
| CN102295280A (en) * | 2011-06-15 | 2011-12-28 | 湖南红太阳光电科技有限公司 | Method for improving electrochemical performance of lithium ion battery cathode material lithium iron phosphate |
| CN102709557A (en) * | 2012-06-05 | 2012-10-03 | 无锡合志科技有限公司 | Preparation method for anode paste of lithium iron phosphate battery |
| CN102969502A (en) * | 2012-11-26 | 2013-03-13 | 厦门钨业股份有限公司 | Preparation method of high-vibration-compaction low-specific-surface-area lithium iron phosphate made by positive pole material |
| CN104425820A (en) * | 2013-09-09 | 2015-03-18 | 北京国能电池科技有限公司 | Lithium ferric manganese phosphate material and preparation method thereof and lithium ion battery cathode material |
| 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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Address after: 230000 Yaohai Industrial Zone, Hefei New District, Anhui, No. D weft Road, No. 7 Applicant after: Gotion High-tech Co., Ltd. Address before: 230000 Yaohai Industrial Park, Anhui, Hefei No. D weft Road, No. 7 Applicant before: Hefei Guoxuan High-Tech Power Energy Co.,Ltd. |
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Application publication date: 20150826 |
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