CN102225890B - 一种用于磷酸铁锂材料生产的电池级草酸亚铁制造方法 - Google Patents
一种用于磷酸铁锂材料生产的电池级草酸亚铁制造方法 Download PDFInfo
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- CN102225890B CN102225890B CN2011101110594A CN201110111059A CN102225890B CN 102225890 B CN102225890 B CN 102225890B CN 2011101110594 A CN2011101110594 A CN 2011101110594A CN 201110111059 A CN201110111059 A CN 201110111059A CN 102225890 B CN102225890 B CN 102225890B
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- iron
- oxalate
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 28
- 239000000463 material Substances 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title claims abstract description 16
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 title abstract description 4
- 229940062993 ferrous oxalate Drugs 0.000 title abstract 4
- OWZIYWAUNZMLRT-UHFFFAOYSA-L iron(2+);oxalate Chemical compound [Fe+2].[O-]C(=O)C([O-])=O OWZIYWAUNZMLRT-UHFFFAOYSA-L 0.000 title abstract 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 102
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims abstract description 101
- 229910052742 iron Inorganic materials 0.000 claims abstract description 50
- 239000000047 product Substances 0.000 claims abstract description 36
- 235000006408 oxalic acid Nutrition 0.000 claims abstract description 29
- 238000006243 chemical reaction Methods 0.000 claims abstract description 26
- 150000002505 iron Chemical class 0.000 claims abstract description 20
- 239000012266 salt solution Substances 0.000 claims abstract description 20
- 239000000243 solution Substances 0.000 claims abstract description 16
- 238000003756 stirring Methods 0.000 claims abstract description 16
- 238000001914 filtration Methods 0.000 claims abstract description 13
- 239000002253 acid Substances 0.000 claims abstract description 11
- 239000000706 filtrate Substances 0.000 claims abstract description 8
- 239000012065 filter cake Substances 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims abstract description 4
- VEPSWGHMGZQCIN-UHFFFAOYSA-H ferric oxalate Chemical compound [Fe+3].[Fe+3].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O VEPSWGHMGZQCIN-UHFFFAOYSA-H 0.000 claims description 31
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 13
- 229940039748 oxalate Drugs 0.000 claims description 13
- 229910010707 LiFePO 4 Inorganic materials 0.000 claims description 10
- 239000006227 byproduct Substances 0.000 claims description 10
- 150000001875 compounds Chemical class 0.000 claims description 10
- -1 ferric oxide compound Chemical class 0.000 claims description 9
- 239000000126 substance Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 150000003839 salts Chemical class 0.000 claims description 6
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 4
- 239000011790 ferrous sulphate Substances 0.000 claims description 4
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims description 4
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 4
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 claims description 4
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 4
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 claims description 3
- JVTAAEKCZFNVCJ-UHFFFAOYSA-M Lactate Chemical compound CC(O)C([O-])=O JVTAAEKCZFNVCJ-UHFFFAOYSA-M 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 3
- VBIXEXWLHSRNKB-UHFFFAOYSA-N ammonium oxalate Chemical compound [NH4+].[NH4+].[O-]C(=O)C([O-])=O VBIXEXWLHSRNKB-UHFFFAOYSA-N 0.000 claims description 3
- 238000009413 insulation Methods 0.000 claims description 3
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- ZNCPFRVNHGOPAG-UHFFFAOYSA-L sodium oxalate Chemical compound [Na+].[Na+].[O-]C(=O)C([O-])=O ZNCPFRVNHGOPAG-UHFFFAOYSA-L 0.000 claims description 3
- 229940039790 sodium oxalate Drugs 0.000 claims description 3
- 238000000967 suction filtration Methods 0.000 claims description 3
- 229910021653 sulphate ion Inorganic materials 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- 229910052745 lead Inorganic materials 0.000 abstract description 8
- 229910052759 nickel Inorganic materials 0.000 abstract description 8
- FFRBMBIXVSCUFS-UHFFFAOYSA-N 2,4-dinitro-1-naphthol Chemical compound C1=CC=C2C(O)=C([N+]([O-])=O)C=C([N+]([O-])=O)C2=C1 FFRBMBIXVSCUFS-UHFFFAOYSA-N 0.000 abstract description 7
- 229910052793 cadmium Inorganic materials 0.000 abstract description 4
- 229910052804 chromium Inorganic materials 0.000 abstract description 4
- 229910052791 calcium Inorganic materials 0.000 abstract description 3
- 229910052802 copper Inorganic materials 0.000 abstract description 3
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 3
- 229910052749 magnesium Inorganic materials 0.000 abstract description 3
- 238000001035 drying Methods 0.000 abstract 1
- 230000010287 polarization Effects 0.000 abstract 1
- 238000005086 pumping Methods 0.000 abstract 1
- LDHBWEYLDHLIBQ-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide;hydrate Chemical compound O.[OH-].[O-2].[Fe+3] LDHBWEYLDHLIBQ-UHFFFAOYSA-M 0.000 description 18
- 239000011734 sodium Substances 0.000 description 12
- 238000009826 distribution Methods 0.000 description 10
- 239000012535 impurity Substances 0.000 description 9
- 238000011049 filling Methods 0.000 description 8
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 6
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 6
- 238000007599 discharging Methods 0.000 description 6
- 229910052700 potassium Inorganic materials 0.000 description 6
- 239000011591 potassium Substances 0.000 description 6
- 229910052708 sodium Inorganic materials 0.000 description 6
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 4
- 239000012295 chemical reaction liquid Substances 0.000 description 4
- 229910001448 ferrous ion Inorganic materials 0.000 description 4
- 235000011194 food seasoning agent Nutrition 0.000 description 4
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 4
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 4
- 238000005649 metathesis reaction Methods 0.000 description 4
- 238000000643 oven drying Methods 0.000 description 4
- 238000010792 warming Methods 0.000 description 4
- 238000012423 maintenance Methods 0.000 description 3
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 3
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical compound [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 description 2
- 238000006479 redox reaction Methods 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 239000005955 Ferric phosphate Substances 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 229940032958 ferric phosphate Drugs 0.000 description 1
- 229910000398 iron phosphate Inorganic materials 0.000 description 1
- 229910000399 iron(III) phosphate Inorganic materials 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
Images
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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- Battery Electrode And Active Subsutance (AREA)
- Compounds Of Iron (AREA)
Abstract
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CN102225890B true CN102225890B (zh) | 2013-11-20 |
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Families Citing this family (5)
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CN102557916B (zh) * | 2011-12-02 | 2014-11-05 | 江西赣锋锂业股份有限公司 | 一种磷酸铁锂专用电池级草酸亚铁的制备方法 |
CN103922920B (zh) * | 2014-04-16 | 2015-06-24 | 安徽中医药大学 | 一维草酸亚铁纳米线的制备方法 |
CN104030915B (zh) * | 2014-06-11 | 2016-04-27 | 湖南海利株洲精细化工有限公司 | 一种高纯超微细草酸亚铁的清洁制备方法 |
US20210269310A1 (en) * | 2018-06-30 | 2021-09-02 | Mai Attia | Process for removing cadmium and other metals and impurities in phosphate-contaning materials |
CN109881026B (zh) * | 2019-02-19 | 2021-06-15 | 北京中科康仑环境科技研究院有限公司 | 一种从铁、镍浸出液中分离和提取铁和镍的方法 |
Citations (5)
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US20020182497A1 (en) * | 2001-05-15 | 2002-12-05 | Kabushiki Kaisha Toyota Chuo Kenkyusho | Carbon-containing lithium-iron composite phosphorus oxide for lithium secondary battery positive electrode active material and process for producing the same |
CN1948259A (zh) * | 2006-10-28 | 2007-04-18 | 李传友 | 磷酸(亚)铁锂专用草酸亚铁的生产方法 |
CN101058536A (zh) * | 2007-01-24 | 2007-10-24 | 湖南化工研究院 | 超微细草酸亚铁的制备方法 |
CN101200422A (zh) * | 2006-12-15 | 2008-06-18 | 比亚迪股份有限公司 | 用于制备磷酸亚铁锂的草酸亚铁的制备方法 |
CN101462942A (zh) * | 2008-12-29 | 2009-06-24 | 刘世琦 | 利用酸洗废液生产高纯电池级草酸亚铁的方法 |
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Publication number | Priority date | Publication date | Assignee | Title |
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US20020182497A1 (en) * | 2001-05-15 | 2002-12-05 | Kabushiki Kaisha Toyota Chuo Kenkyusho | Carbon-containing lithium-iron composite phosphorus oxide for lithium secondary battery positive electrode active material and process for producing the same |
CN1948259A (zh) * | 2006-10-28 | 2007-04-18 | 李传友 | 磷酸(亚)铁锂专用草酸亚铁的生产方法 |
CN101200422A (zh) * | 2006-12-15 | 2008-06-18 | 比亚迪股份有限公司 | 用于制备磷酸亚铁锂的草酸亚铁的制备方法 |
CN101058536A (zh) * | 2007-01-24 | 2007-10-24 | 湖南化工研究院 | 超微细草酸亚铁的制备方法 |
CN101462942A (zh) * | 2008-12-29 | 2009-06-24 | 刘世琦 | 利用酸洗废液生产高纯电池级草酸亚铁的方法 |
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Denomination of invention: A manufacturing method of battery grade ferrous oxalate for the production of lithium iron phosphate material Effective date of registration: 20220214 Granted publication date: 20131120 Pledgee: Agricultural Bank of China Limited Zhijiang sub branch Pledgor: HUBEI HAOYUAN MATERIAL TECHNOLOGY Co.,Ltd. Registration number: Y2022980001539 |
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Denomination of invention: A manufacturing method of battery grade ferrous oxalate used for the production of lithium iron phosphate material Effective date of registration: 20230228 Granted publication date: 20131120 Pledgee: Agricultural Bank of China Limited Zhijiang sub branch Pledgor: HUBEI HAOYUAN MATERIAL TECHNOLOGY Co.,Ltd. Registration number: Y2023110000082 |
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Denomination of invention: A battery grade ferrous oxalate manufacturing method for the production of lithium iron phosphate materials Granted publication date: 20131120 Pledgee: Agricultural Bank of China Limited Zhijiang sub branch Pledgor: HUBEI HAOYUAN MATERIAL TECHNOLOGY Co.,Ltd. Registration number: Y2024980006205 |
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