CN104556236B - 一种电池级硫酸锰的制备方法 - Google Patents
一种电池级硫酸锰的制备方法 Download PDFInfo
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- CN104556236B CN104556236B CN201410808549.3A CN201410808549A CN104556236B CN 104556236 B CN104556236 B CN 104556236B CN 201410808549 A CN201410808549 A CN 201410808549A CN 104556236 B CN104556236 B CN 104556236B
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- Prior art keywords
- manganese
- sulfide
- lithium battery
- obtains
- solution
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- 229940099596 manganese sulfate Drugs 0.000 title claims abstract description 41
- 235000007079 manganese sulphate Nutrition 0.000 title claims abstract description 41
- 239000011702 manganese sulphate Substances 0.000 title claims abstract description 41
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 title claims abstract description 41
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 19
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000000243 solution Substances 0.000 claims abstract description 30
- CADICXFYUNYKGD-UHFFFAOYSA-N sulfanylidenemanganese Chemical compound [Mn]=S CADICXFYUNYKGD-UHFFFAOYSA-N 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 22
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- 239000012065 filter cake Substances 0.000 claims abstract description 16
- 150000002696 manganese Chemical class 0.000 claims abstract description 14
- 239000012266 salt solution Substances 0.000 claims abstract description 13
- 238000001914 filtration Methods 0.000 claims abstract description 11
- 239000002002 slurry Substances 0.000 claims abstract description 9
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 9
- 239000011734 sodium Substances 0.000 claims abstract description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000013078 crystal Substances 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 8
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 6
- 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 claims abstract description 6
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000010009 beating Methods 0.000 claims abstract description 5
- 239000008367 deionised water Substances 0.000 claims abstract description 5
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000002425 crystallisation Methods 0.000 claims abstract description 3
- 230000008025 crystallization Effects 0.000 claims abstract description 3
- 238000000926 separation method Methods 0.000 claims abstract description 3
- 229910052799 carbon Inorganic materials 0.000 claims abstract 2
- 229960004424 carbon dioxide Drugs 0.000 claims abstract 2
- 239000013049 sediment Substances 0.000 claims description 11
- 239000011656 manganese carbonate Substances 0.000 claims description 5
- 235000006748 manganese carbonate Nutrition 0.000 claims description 5
- 229940093474 manganese carbonate Drugs 0.000 claims description 5
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 claims description 5
- XMWCXZJXESXBBY-UHFFFAOYSA-L manganese(ii) carbonate Chemical compound [Mn+2].[O-]C([O-])=O XMWCXZJXESXBBY-UHFFFAOYSA-L 0.000 claims description 5
- 239000000376 reactant Substances 0.000 claims description 4
- 230000008030 elimination Effects 0.000 claims description 3
- 238000003379 elimination reaction Methods 0.000 claims description 3
- 239000012528 membrane Substances 0.000 claims description 2
- 238000005374 membrane filtration Methods 0.000 claims description 2
- DPLVEEXVKBWGHE-UHFFFAOYSA-N potassium sulfide Chemical compound [S-2].[K+].[K+] DPLVEEXVKBWGHE-UHFFFAOYSA-N 0.000 claims description 2
- 238000001223 reverse osmosis Methods 0.000 claims description 2
- 238000010792 warming Methods 0.000 claims description 2
- UYJXRRSPUVSSMN-UHFFFAOYSA-P ammonium sulfide Chemical compound [NH4+].[NH4+].[S-2] UYJXRRSPUVSSMN-UHFFFAOYSA-P 0.000 claims 1
- 230000007062 hydrolysis Effects 0.000 claims 1
- 238000006460 hydrolysis reaction Methods 0.000 claims 1
- 239000007788 liquid Substances 0.000 claims 1
- KNLQKHUBPCXPQD-UHFFFAOYSA-N manganese;sulfuric acid Chemical compound [Mn].OS(O)(=O)=O KNLQKHUBPCXPQD-UHFFFAOYSA-N 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 238000004062 sedimentation Methods 0.000 claims 1
- 238000005987 sulfurization reaction Methods 0.000 claims 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 18
- 229910052748 manganese Inorganic materials 0.000 abstract description 16
- 239000011572 manganese Substances 0.000 abstract description 16
- 229910052742 iron Inorganic materials 0.000 abstract description 11
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 abstract description 8
- 229910052791 calcium Inorganic materials 0.000 abstract description 7
- 239000011575 calcium Substances 0.000 abstract description 7
- 229910052749 magnesium Inorganic materials 0.000 abstract description 7
- 239000011777 magnesium Substances 0.000 abstract description 7
- 229910052725 zinc Inorganic materials 0.000 abstract description 7
- 239000011701 zinc Substances 0.000 abstract description 7
- 229910052700 potassium Inorganic materials 0.000 abstract description 5
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 abstract description 4
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 abstract description 4
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052793 cadmium Inorganic materials 0.000 abstract description 4
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052759 nickel Inorganic materials 0.000 abstract description 4
- 238000005406 washing Methods 0.000 abstract description 4
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052785 arsenic Inorganic materials 0.000 abstract description 3
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052804 chromium Inorganic materials 0.000 abstract description 3
- 239000011651 chromium Substances 0.000 abstract description 3
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052802 copper Inorganic materials 0.000 abstract description 2
- 239000010949 copper Substances 0.000 abstract description 2
- 239000011591 potassium Substances 0.000 abstract description 2
- 150000002641 lithium Chemical class 0.000 abstract 1
- 229910052979 sodium sulfide Inorganic materials 0.000 description 9
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 description 9
- 239000000047 product Substances 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 238000005903 acid hydrolysis reaction Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 229910021380 Manganese Chloride Inorganic materials 0.000 description 1
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 description 1
- WAEMQWOKJMHJLA-UHFFFAOYSA-N Manganese(2+) Chemical compound [Mn+2] WAEMQWOKJMHJLA-UHFFFAOYSA-N 0.000 description 1
- NPYPAHLBTDXSSS-UHFFFAOYSA-N Potassium ion Chemical compound [K+] NPYPAHLBTDXSSS-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- KLARSDUHONHPRF-UHFFFAOYSA-N [Li].[Mn] Chemical compound [Li].[Mn] KLARSDUHONHPRF-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- CJDPJFRMHVXWPT-UHFFFAOYSA-N barium sulfide Chemical compound [S-2].[Ba+2] CJDPJFRMHVXWPT-UHFFFAOYSA-N 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- -1 iron ion Chemical class 0.000 description 1
- 235000002867 manganese chloride Nutrition 0.000 description 1
- 239000011565 manganese chloride Substances 0.000 description 1
- 229940099607 manganese chloride Drugs 0.000 description 1
- 229910001437 manganese ion Inorganic materials 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 229910001414 potassium ion Inorganic materials 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
- C01G45/10—Sulfates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
Description
项目名称 | 实测结果 |
钙 | 1.63 |
镁 | 5.59 |
铬 | 1.283 --> |
镍 | 5.77 |
铜 | ND |
镉 | ND |
砷 | ND |
锌 | 1.49 |
铁 | 3.42 |
项目名称 | 实测结果 |
钙 | 21.06 |
镁 | 15.32 |
铅 | 6.19 |
镍 | 9.18 |
铜 | ND |
镉 | 3.13 |
锌 | 3.77 |
铁 | 5.74 |
Claims (2)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
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CN201410808549.3A CN104556236B (zh) | 2014-12-23 | 2014-12-23 | 一种电池级硫酸锰的制备方法 |
Applications Claiming Priority (1)
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CN201410808549.3A CN104556236B (zh) | 2014-12-23 | 2014-12-23 | 一种电池级硫酸锰的制备方法 |
Publications (2)
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CN104556236A CN104556236A (zh) | 2015-04-29 |
CN104556236B true CN104556236B (zh) | 2016-05-04 |
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Families Citing this family (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105565395B (zh) * | 2015-11-20 | 2017-07-28 | 厦门紫金矿冶技术有限公司 | 一种铜矿山萃余液的处理方法 |
CN105645475B (zh) * | 2016-03-31 | 2017-11-17 | 湖北浩元材料科技有限公司 | 一种应用于锂电正极材料的高纯锰源制备方法 |
CN107311853B (zh) * | 2017-06-22 | 2020-05-19 | 赤峰开瑞科技有限公司 | 一种电池级草酸锰铁的合成方法 |
CN110396599B (zh) * | 2019-07-24 | 2021-03-23 | 南京博驰新能源股份有限公司 | 一种锂电池回收再利用方法 |
CN112062159A (zh) * | 2020-08-04 | 2020-12-11 | 福建省连城锰矿有限责任公司 | 一种免除钾钠钙镁法制备电子级硫酸锰的工艺 |
CN115044773A (zh) * | 2022-06-17 | 2022-09-13 | 中伟新材料股份有限公司 | 从含金属渣中回收锰、锌的方法 |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101798119A (zh) * | 2010-03-29 | 2010-08-11 | 贵州红星发展股份有限公司 | 一种制备一水合硫酸锰的方法 |
CN102115204A (zh) * | 2010-12-31 | 2011-07-06 | 谢善情 | 一种用锰尾矿制备硫酸锰、硫酸亚铁和硫酸钙的方法 |
CN102583563A (zh) * | 2011-01-10 | 2012-07-18 | 常开军 | 一种用于电池材料的超高纯电池级氯化锰制造方法 |
CN103011297A (zh) * | 2012-12-07 | 2013-04-03 | 中信大锰矿业有限责任公司 | 软锰矿为原料采用碳火法生产高纯硫酸锰的方法 |
JP2013209267A (ja) * | 2012-03-30 | 2013-10-10 | Jx Nippon Mining & Metals Corp | 硫酸マンガンの製造方法 |
-
2014
- 2014-12-23 CN CN201410808549.3A patent/CN104556236B/zh active Active
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101798119A (zh) * | 2010-03-29 | 2010-08-11 | 贵州红星发展股份有限公司 | 一种制备一水合硫酸锰的方法 |
CN102115204A (zh) * | 2010-12-31 | 2011-07-06 | 谢善情 | 一种用锰尾矿制备硫酸锰、硫酸亚铁和硫酸钙的方法 |
CN102583563A (zh) * | 2011-01-10 | 2012-07-18 | 常开军 | 一种用于电池材料的超高纯电池级氯化锰制造方法 |
JP2013209267A (ja) * | 2012-03-30 | 2013-10-10 | Jx Nippon Mining & Metals Corp | 硫酸マンガンの製造方法 |
CN103011297A (zh) * | 2012-12-07 | 2013-04-03 | 中信大锰矿业有限责任公司 | 软锰矿为原料采用碳火法生产高纯硫酸锰的方法 |
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Denomination of invention: A preparation method of battery grade manganese sulfate Effective date of registration: 20220214 Granted publication date: 20160504 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 preparation method of battery grade manganese sulfate Effective date of registration: 20230228 Granted publication date: 20160504 Pledgee: Agricultural Bank of China Limited Zhijiang sub branch Pledgor: HUBEI HAOYUAN MATERIAL TECHNOLOGY Co.,Ltd. Registration number: Y2023110000082 |
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Granted publication date: 20160504 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 preparation method for battery grade manganese sulfate Granted publication date: 20160504 Pledgee: Agricultural Bank of China Limited Zhijiang sub branch Pledgor: HUBEI HAOYUAN MATERIAL TECHNOLOGY Co.,Ltd. Registration number: Y2024980006205 |
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