CN102694169B - FePO4/高分子裂解碳复合材料及其制备方法以及NH4Fe2(OH)(PO4)2·2H2O/高分子复合材料及其制备方法 - Google Patents
FePO4/高分子裂解碳复合材料及其制备方法以及NH4Fe2(OH)(PO4)2·2H2O/高分子复合材料及其制备方法 Download PDFInfo
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- CN102694169B CN102694169B CN201210057607.4A CN201210057607A CN102694169B CN 102694169 B CN102694169 B CN 102694169B CN 201210057607 A CN201210057607 A CN 201210057607A CN 102694169 B CN102694169 B CN 102694169B
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- 239000002131 composite material Substances 0.000 title claims abstract description 103
- 229920000642 polymer Polymers 0.000 title claims abstract description 71
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 64
- 238000002360 preparation method Methods 0.000 title claims abstract description 59
- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical compound [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 title abstract description 30
- 229910000399 iron(III) phosphate Inorganic materials 0.000 title abstract description 15
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 title abstract 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 126
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 63
- 235000003891 ferrous sulphate Nutrition 0.000 claims abstract description 61
- 239000011790 ferrous sulphate Substances 0.000 claims abstract description 61
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims abstract description 61
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims abstract description 61
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 59
- 150000001875 compounds Chemical class 0.000 claims abstract description 38
- 239000007788 liquid Substances 0.000 claims abstract description 37
- 239000000178 monomer Substances 0.000 claims abstract description 37
- 238000005406 washing Methods 0.000 claims abstract description 37
- 239000000839 emulsion Substances 0.000 claims abstract description 36
- 238000000926 separation method Methods 0.000 claims abstract description 32
- 239000000463 material Substances 0.000 claims abstract description 30
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 26
- 238000003756 stirring Methods 0.000 claims abstract description 25
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 20
- 239000003999 initiator Substances 0.000 claims abstract description 16
- 239000007800 oxidant agent Substances 0.000 claims abstract description 15
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims abstract description 12
- 239000012298 atmosphere Substances 0.000 claims abstract description 11
- 238000011065 in-situ storage Methods 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 238000000975 co-precipitation Methods 0.000 claims abstract description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 92
- 229920002521 macromolecule Polymers 0.000 claims description 85
- 239000000243 solution Substances 0.000 claims description 84
- 239000007864 aqueous solution Substances 0.000 claims description 58
- 230000001276 controlling effect Effects 0.000 claims description 50
- 229910021529 ammonia Inorganic materials 0.000 claims description 42
- 239000000376 reactant Substances 0.000 claims description 42
- 238000005336 cracking Methods 0.000 claims description 40
- 239000007787 solid Substances 0.000 claims description 31
- 230000032683 aging Effects 0.000 claims description 29
- 239000000843 powder Substances 0.000 claims description 24
- 239000004793 Polystyrene Substances 0.000 claims description 20
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 20
- 229920002223 polystyrene Polymers 0.000 claims description 20
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 20
- 238000002425 crystallisation Methods 0.000 claims description 19
- 230000008025 crystallization Effects 0.000 claims description 19
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 18
- 230000001105 regulatory effect Effects 0.000 claims description 18
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Chemical compound [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 18
- 238000004227 thermal cracking Methods 0.000 claims description 18
- 239000002202 Polyethylene glycol Substances 0.000 claims description 17
- 229920001223 polyethylene glycol Polymers 0.000 claims description 17
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 16
- YTPLMLYBLZKORZ-UHFFFAOYSA-N Thiophene Chemical compound C=1C=CSC=1 YTPLMLYBLZKORZ-UHFFFAOYSA-N 0.000 claims description 16
- 238000006243 chemical reaction Methods 0.000 claims description 16
- 238000000354 decomposition reaction Methods 0.000 claims description 15
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 15
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 15
- 230000001590 oxidative effect Effects 0.000 claims description 14
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 14
- 239000000047 product Substances 0.000 claims description 14
- 239000002994 raw material Substances 0.000 claims description 14
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 13
- 238000007689 inspection Methods 0.000 claims description 13
- 239000012265 solid product Substances 0.000 claims description 13
- QNRATNLHPGXHMA-XZHTYLCXSA-N (r)-(6-ethoxyquinolin-4-yl)-[(2s,4s,5r)-5-ethyl-1-azabicyclo[2.2.2]octan-2-yl]methanol;hydrochloride Chemical group Cl.C([C@H]([C@H](C1)CC)C2)CN1[C@@H]2[C@H](O)C1=CC=NC2=CC=C(OCC)C=C21 QNRATNLHPGXHMA-XZHTYLCXSA-N 0.000 claims description 12
- 229920002125 Sokalan® Polymers 0.000 claims description 11
- 239000004584 polyacrylic acid Substances 0.000 claims description 11
- 229920000767 polyaniline Polymers 0.000 claims description 11
- 229920000128 polypyrrole Polymers 0.000 claims description 11
- 229920000123 polythiophene Polymers 0.000 claims description 11
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 239000011261 inert gas Substances 0.000 claims description 9
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 8
- 229930192474 thiophene Natural products 0.000 claims description 8
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 5
- 230000003647 oxidation Effects 0.000 claims description 5
- 238000007254 oxidation reaction Methods 0.000 claims description 5
- 150000003233 pyrroles Chemical class 0.000 claims description 5
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims description 5
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 abstract description 16
- 238000000034 method Methods 0.000 abstract description 15
- 229910019142 PO4 Inorganic materials 0.000 abstract description 6
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 239000002243 precursor Substances 0.000 abstract 2
- 238000001035 drying Methods 0.000 abstract 1
- 230000002708 enhancing effect Effects 0.000 abstract 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 16
- 239000003643 water by type Substances 0.000 description 16
- 229910000398 iron phosphate Inorganic materials 0.000 description 15
- 229940068984 polyvinyl alcohol Drugs 0.000 description 15
- 235000019422 polyvinyl alcohol Nutrition 0.000 description 15
- 239000005955 Ferric phosphate Substances 0.000 description 9
- 229940032958 ferric phosphate Drugs 0.000 description 9
- 238000013019 agitation Methods 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 8
- 239000012299 nitrogen atmosphere Substances 0.000 description 8
- 230000002441 reversible effect Effects 0.000 description 8
- 239000000377 silicon dioxide Substances 0.000 description 8
- 229910052493 LiFePO4 Inorganic materials 0.000 description 6
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 description 6
- 239000002482 conductive additive Substances 0.000 description 6
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 5
- 229910001416 lithium ion Inorganic materials 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000010405 anode material Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000011268 mixed slurry Substances 0.000 description 4
- -1 polyethylene ketopyrrolidine Polymers 0.000 description 4
- 229910010707 LiFePO 4 Inorganic materials 0.000 description 3
- 150000002505 iron Chemical class 0.000 description 3
- 229920000151 polyglycol Polymers 0.000 description 3
- 239000010695 polyglycol Substances 0.000 description 3
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 2
- 229930006000 Sucrose Natural products 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000005720 sucrose Substances 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- 239000003513 alkali Substances 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000003750 conditioning effect Effects 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Catalysts (AREA)
- Carbon And Carbon Compounds (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
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CN201210057607.4A CN102694169B (zh) | 2012-03-07 | 2012-03-07 | FePO4/高分子裂解碳复合材料及其制备方法以及NH4Fe2(OH)(PO4)2·2H2O/高分子复合材料及其制备方法 |
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CN201210057607.4A CN102694169B (zh) | 2012-03-07 | 2012-03-07 | FePO4/高分子裂解碳复合材料及其制备方法以及NH4Fe2(OH)(PO4)2·2H2O/高分子复合材料及其制备方法 |
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CN102694169B true CN102694169B (zh) | 2014-11-12 |
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Families Citing this family (6)
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CN104362317A (zh) * | 2014-11-05 | 2015-02-18 | 上海纳米技术及应用国家工程研究中心有限公司 | 锂离子电池用磷酸铁/导电聚合物复合正极材料及制备方法 |
CN106099104B (zh) * | 2016-08-26 | 2019-07-26 | 常开军 | 一种用于二次电池制造的无锂正极材料及其制造方法 |
CN107785558B (zh) * | 2017-10-27 | 2020-07-03 | 重庆特瑞新能源材料有限公司 | 一种磷酸铁锂/炭复合正极材料的制备方法 |
CN108336352A (zh) * | 2017-12-29 | 2018-07-27 | 贵州唯特高新能源科技有限公司 | 一种高电导率高振实密度磷酸铁锂的制备方法 |
CN109305663A (zh) * | 2018-08-15 | 2019-02-05 | 湖南鸿跃电池材料有限公司 | 电池级无水磷酸铁及其制备方法 |
CN109449431B (zh) * | 2018-12-16 | 2020-12-11 | 江西华昊新能源有限公司 | 一种制备锂电池用粒径可控磷酸钴锂复合正极材料的方法 |
Citations (4)
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CN1559889A (zh) * | 2004-02-20 | 2005-01-05 | 北大先行科技产业有限公司 | 锂离子电池正极材料磷酸亚铁锂的制备方法 |
CN101244813A (zh) * | 2007-02-15 | 2008-08-20 | 比亚迪股份有限公司 | 碱式磷酸铁铵及制备方法、磷酸铁的制备方法及磷酸亚铁锂的制备方法 |
CN101279726A (zh) * | 2008-04-11 | 2008-10-08 | 赵兵 | 一种磷酸亚铁锂的制备方法 |
CN102013468A (zh) * | 2009-09-07 | 2011-04-13 | 深圳市贝特瑞新能源材料股份有限公司 | 一种高导电性磷酸铁锂正极材料的制备方法 |
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US20110300442A1 (en) * | 2010-06-02 | 2011-12-08 | Infinity Energy (Hong Kong) Co., Limited | Novel nanoscale solution method for synthesizing lithium cathode active materials |
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Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN1559889A (zh) * | 2004-02-20 | 2005-01-05 | 北大先行科技产业有限公司 | 锂离子电池正极材料磷酸亚铁锂的制备方法 |
CN101244813A (zh) * | 2007-02-15 | 2008-08-20 | 比亚迪股份有限公司 | 碱式磷酸铁铵及制备方法、磷酸铁的制备方法及磷酸亚铁锂的制备方法 |
CN101279726A (zh) * | 2008-04-11 | 2008-10-08 | 赵兵 | 一种磷酸亚铁锂的制备方法 |
CN102013468A (zh) * | 2009-09-07 | 2011-04-13 | 深圳市贝特瑞新能源材料股份有限公司 | 一种高导电性磷酸铁锂正极材料的制备方法 |
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