JP7018077B6 - 反応装置及び方法 - Google Patents
反応装置及び方法 Download PDFInfo
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- JP7018077B6 JP7018077B6 JP2019565541A JP2019565541A JP7018077B6 JP 7018077 B6 JP7018077 B6 JP 7018077B6 JP 2019565541 A JP2019565541 A JP 2019565541A JP 2019565541 A JP2019565541 A JP 2019565541A JP 7018077 B6 JP7018077 B6 JP 7018077B6
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- 238000000034 method Methods 0.000 title claims description 24
- 239000000243 solution Substances 0.000 claims description 173
- 238000006243 chemical reaction Methods 0.000 claims description 142
- 229910052751 metal Inorganic materials 0.000 claims description 54
- 239000002184 metal Substances 0.000 claims description 54
- 239000002994 raw material Substances 0.000 claims description 44
- 239000002243 precursor Substances 0.000 claims description 43
- 238000002347 injection Methods 0.000 claims description 38
- 239000007924 injection Substances 0.000 claims description 38
- 238000003756 stirring Methods 0.000 claims description 32
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- 239000011572 manganese Substances 0.000 claims description 23
- 239000007774 positive electrode material Substances 0.000 claims description 23
- 238000000975 co-precipitation Methods 0.000 claims description 21
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 20
- 229910052744 lithium Inorganic materials 0.000 claims description 20
- 238000002156 mixing Methods 0.000 claims description 18
- KFDQGLPGKXUTMZ-UHFFFAOYSA-N [Mn].[Co].[Ni] Chemical compound [Mn].[Co].[Ni] KFDQGLPGKXUTMZ-UHFFFAOYSA-N 0.000 claims description 17
- 239000000203 mixture Substances 0.000 claims description 5
- 238000003780 insertion Methods 0.000 claims description 4
- 230000037431 insertion Effects 0.000 claims description 4
- -1 nickel-cobalt-aluminum Chemical compound 0.000 claims description 4
- 239000011148 porous material Substances 0.000 claims description 4
- 229910052748 manganese Inorganic materials 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 2
- 238000004088 simulation Methods 0.000 description 15
- 238000010586 diagram Methods 0.000 description 12
- 238000004519 manufacturing process Methods 0.000 description 12
- 230000000694 effects Effects 0.000 description 10
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 10
- 239000002245 particle Substances 0.000 description 9
- 230000001965 increasing effect Effects 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 230000035484 reaction time Effects 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 4
- 238000007796 conventional method Methods 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 238000010926 purge Methods 0.000 description 2
- 238000003746 solid phase reaction Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910012851 LiCoO 2 Inorganic materials 0.000 description 1
- 229910015643 LiMn 2 O 4 Inorganic materials 0.000 description 1
- 229910014689 LiMnO Inorganic materials 0.000 description 1
- 229910013290 LiNiO 2 Inorganic materials 0.000 description 1
- 229910013100 LiNix Inorganic materials 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 230000001154 acute effect Effects 0.000 description 1
- BLJNPOIVYYWHMA-UHFFFAOYSA-N alumane;cobalt Chemical compound [AlH3].[Co] BLJNPOIVYYWHMA-UHFFFAOYSA-N 0.000 description 1
- 239000003637 basic solution Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000002738 chelating agent Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 229910000428 cobalt oxide Inorganic materials 0.000 description 1
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- AMWRITDGCCNYAT-UHFFFAOYSA-L manganese oxide Inorganic materials [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 1
- PPNAOCWZXJOHFK-UHFFFAOYSA-N manganese(2+);oxygen(2-) Chemical class [O-2].[Mn+2] PPNAOCWZXJOHFK-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910000480 nickel oxide Inorganic materials 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical class [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000010671 solid-state reaction Methods 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
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Description
Claims (15)
- 反応容器と、
前記反応容器の内部に提供され、多段のインペラーを備えた撹拌手段と、
前記反応容器に連携され、少なくとも前記インペラー間の空間に原料を投入する少なくとも一つ以上の投入ノズルを含む原料投入手段と、
を含み、
前記原料は金属溶液(metal solution)と第1及び第2溶液とを含み、
前記原料投入手段は、
前記反応容器の外部に配置される金属溶液混合手段と連携され、前記金属溶液を前記インペラー間の空間に投入する第1原料投入手段と、
前記インペラー間の空間に前記第1及び第2溶液を投入する第2及び第3原料投入手段と、
を含み、
前記第1~第3原料投入手段は、前記インペラー間の空間に加えて、前記反応容器の底及び最下段のインペラー間の空間に原料を投入する投入ノズルをさらに含み、
前記反応容器の外側に提供される容器重量感知手段をさらに含むことで、少なくともインペラー間の空間に投入される金属溶液と第1及び第2溶液は反応容器内の溶液レベルが高くなるほど、最下段の投入ノズルから順に上に位置された投入ノズルを介して反応容器の内部に投入される、反応装置。 - 前記原料投入手段の投入ノズルは混合手段と連結される金属溶液供給管と、前記第1及び第2溶液を供給する溶液供給管の端部に一体に提供されるか、または分解可能に組み立てられる、請求項1に記載の反応装置。
- 前記供給管の下端部が折り曲げられて前記投入ノズルを形成する、請求項2に記載の反応装置。
- 前記投入ノズルは複数の原料投入孔を含む、請求項1に記載の反応装置。
- 前記投入ノズルはコイル型投入ノズルとして提供される、請求項1に記載の反応装置。
- 前記下端部に投入ノズルが提供される供給管は、前記反応容器を通過して上下移動可能な移動型供給管として提供される、請求項3に記載の反応装置。
- 前記反応容器の内部に提供される少なくとも一つ以上の多孔性バッフルをさらに含む、請求項1に記載の反応装置。
- 前記多孔性バッフルに備えられる孔は、円状、楕円状、及び多角形のうち少なくとも一つで提供される、請求項7に記載の反応装置。
- 前記多孔性バッフルに提供された少なくとも一つ以上の開口部に挿入され、孔が形成された挿入固定体をさらに含む、請求項7に記載の反応装置。
- 前記多孔性バッフルに備えられた孔は、断面上、入口よりも出口が狭くなる傾斜孔として提供される、請求項7に記載の反応装置。
- 前記多孔性バッフルは、反応容器に備えられた撹拌手段の最下段のインペラーに近接して伸張する、請求項7に記載の反応装置。
- 前記混合手段は、
混合タンクと、
前記混合タンクに連結される供給管、ならびに前記供給管に備えられた流量調整器と、を含む、請求項1に記載の反応装置。 - 請求項1から12のいずれかの1項に記載の反応装置を用いる反応方法であって、
金属溶液(metal solution)を反応容器に設定された流量で投入する金属溶液投入段階と、
他の溶液を設定された流量で反応容器に投入する溶液投入段階と、
前記反応容器に投入された金属溶液と他の溶液とを攪拌して、リチウム二次電池用正極活物質を製造する共沈反応段階と、
を含み、前記金属溶液と他の溶液は、反応容器内の溶液レベルが高くなるほど、最下段の投入ノズルから順に上に位置された投入ノズルを介して反応容器の内部に投入される、反応方法。 - 前記金属溶液と他の溶液は、前記反応容器に備えられた撹拌手段のインペラー間の空間、前記反応容器の底及びインペラー間の空間のうち少なくとも一つの空間に投入される、請求項13に記載の反応方法。
- 前記共沈反応段階において、Ni:Co:MnまたはNi:Co:Alの組成を有する前記金属溶液とNaOH及びNH4OHの前記他の溶液とを反応させて、少なくとも中心距離に応じた濃度勾配(Gradient)を有するニッケル-コバルト-マンガン前駆体(NixCoyMn1-x-y(OH)2)またはニッケル-コバルト-アルミニウム前駆体(NixCoyAl 1-x-y (OH)2)を製造する、請求項13に記載の反応方法。
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