JP5714708B2 - リチウム二次電池の正極活物質前駆体製造用オールインワンタイプ連続式反応器およびこれを備える結晶分離装置 - Google Patents
リチウム二次電池の正極活物質前駆体製造用オールインワンタイプ連続式反応器およびこれを備える結晶分離装置 Download PDFInfo
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- 239000002243 precursor Substances 0.000 title claims description 40
- 239000007774 positive electrode material Substances 0.000 title claims description 35
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims description 15
- 229910052744 lithium Inorganic materials 0.000 title claims description 15
- 238000004519 manufacturing process Methods 0.000 title claims description 8
- 239000000376 reactant Substances 0.000 claims description 84
- 238000006243 chemical reaction Methods 0.000 claims description 60
- 238000002347 injection Methods 0.000 claims description 40
- 239000007924 injection Substances 0.000 claims description 40
- 239000007795 chemical reaction product Substances 0.000 claims description 30
- 239000002245 particle Substances 0.000 claims description 25
- 238000003756 stirring Methods 0.000 claims description 23
- 239000003507 refrigerant Substances 0.000 claims description 19
- 239000013078 crystal Substances 0.000 claims description 18
- 238000000926 separation method Methods 0.000 claims description 17
- 230000002093 peripheral effect Effects 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 238000013019 agitation Methods 0.000 claims description 9
- 238000003860 storage Methods 0.000 claims description 8
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 7
- 239000000047 product Substances 0.000 claims description 7
- 239000000243 solution Substances 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 5
- 239000006182 cathode active material Substances 0.000 claims description 4
- 239000000706 filtrate Substances 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 239000002002 slurry Substances 0.000 claims description 3
- 238000009826 distribution Methods 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- -1 NH 4 OH Substances 0.000 claims 1
- 238000001514 detection method Methods 0.000 claims 1
- 238000001802 infusion Methods 0.000 claims 1
- 239000000523 sample Substances 0.000 description 5
- 239000007788 liquid Substances 0.000 description 4
- 239000012530 fluid Substances 0.000 description 3
- 230000014509 gene expression Effects 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 238000010298 pulverizing process Methods 0.000 description 3
- 238000005096 rolling process Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 230000000903 blocking effect Effects 0.000 description 2
- 239000002826 coolant Substances 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000011790 ferrous sulphate Substances 0.000 description 1
- 235000003891 ferrous sulphate Nutrition 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 238000011027 product recovery Methods 0.000 description 1
- 230000010349 pulsation Effects 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 230000002123 temporal effect Effects 0.000 description 1
- CYRMSUTZVYGINF-UHFFFAOYSA-N trichlorofluoromethane Chemical compound FC(Cl)(Cl)Cl CYRMSUTZVYGINF-UHFFFAOYSA-N 0.000 description 1
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Description
rapid formation and collapse of microscopic bubbles in a liquid」)と呼び、このとき、約1000barの圧力、約5000Kの瞬間温度を有する高温高圧の瞬間的な衝撃波が発生するため、これが非常に高いエネルギー源として働いて試料粒子を粉砕する作用をする。
11:反応チャンバー
12:フランジ部
13:反応物注入ポート
14:反応結果物排出ポート
15:余剰のポート
20:攪拌モーター
30:攪拌棒
40:温度調節部
41:冷媒チャンバー
42:冷媒
50:粒子粉砕部
60:流量感知センサー
70:流量制御部
80:第1サポーター
80a:第2サポーター
81:サポートパネル
82:転がりローラー
100:反応物貯留タンク
200:供給ポンプ
300:正極活物質前駆体分離器
400:乾燥器
500:粒度分析器
600:走査電子顕微鏡
Claims (12)
- 内部に反応チャンバー(11)を有する非回転体としてのシリンダー(10)と、前記シリンダー(10)の一方の側に配設される攪拌モーター(20)と、前記攪拌モーター(20)のモーター軸(21)と結合されたままで、前記反応チャンバー(11)の内部に内蔵されるが、前記反応チャンバー(11)の壁面から離れて内蔵される攪拌棒(30)と、を有する連続式反応器であって、
前記シリンダー(10)の一方の側に形成されたフランジ部(12)と、
前記フランジ部の上に反応チャンバー(11)と連通するように形成されて反応物が注入される1以上の反応物注入ポート(13)と、
前記シリンダー(10)の他方の側に反応チャンバー(11)と連通するように形成されて反応結果物が排出される反応結果物排出ポート(14)と、
前記シリンダー(10)の反応物注入ポート(13)と反応結果物排出ポート(14)との間に反応チャンバー(11)と連通するように形成される多数の余剰のポート(15)と、
前記シリンダー(10)の外周面と内周面との間に配設される温度調節部(40)と、
前記反応物注入ポート(13)の流路の上に設けられて反応物注入ポートを介して注入される反応物の粒子を粉砕する粒子粉砕部(50)と、
前記反応物注入ポート(13)と、反応結果物排出ポート(14)および余剰のポート(15)のうちの少なくともいずれかに設けられて反応物の流量を感知する流量感知センサー(60)と、
前記流量感知センサー(60)によって帰還された流量感知データーによって反応物注入ポート(13)を介して流入する反応物の流量、反応チャンバー11の内部を通過する反 応物の流量、または反応結果物排出ポート14を介して排出される反応結果物の流量を加 減制御する流量制御部(70)と、
を備えるが、
前記温度調節部(40)は、環状の冷媒チャンバー(41)と、前記冷媒チャンバーの内部に充填される冷媒(42)と、を有することを特徴とするリチウム二次電池の正極活物質前駆体製造用オールインワンタイプ連続式反応器。 - 前記攪拌モーター(20)は、10〜2000rpmの範囲内で回転速度が調節可能な変速型攪拌モーターであることを特徴とする請求項1に記載のリチウム二次電池の正極活物質前駆体製造用オールインワンタイプ連続式反応器。
- 前記反応物は、メタル溶液、NH4OHおよびNaOHを含むことを特徴とする請求項1に記載のリチウム二次電池の正極活物質前駆体製造用オールインワンタイプ連続式反応器。
- 前記メタル溶液は、Ni、MnおよびCoを含む混合溶液であることを特徴とする請求項3に記載のリチウム二次電池の正極活物質前駆体製造用オールインワンタイプ連続式反応器。
- 前記反応物は、LiOH、FeSO4およびH3PO4を含むことを特徴とする請求項1に記載のリチウム二次電池の正極活物質前駆体製造用オールインワンタイプ連続式反応器。
- 前記反応チャンバー(11)の内周面と攪拌棒(30)の外周面との間の間隔(g)/攪拌棒の半径(d)は、1.0以下であることを特徴とする請求項1に記載のリチウム二次電池の正極活物質前駆体製造用オールインワンタイプ連続式反応器。
- 内部に反応チャンバー(11)を有する非回転体としてのシリンダー(10)と、前記シリンダー(10)の一方の側に配設される攪拌モーター(20)と、前記攪拌モーター(20)のモーター軸(21)と結合されたままで、前記反応チャンバー(11)の内部に内蔵されるが、前記反応チャンバー(11)の壁面から離れて内蔵される攪拌棒(30)と、を有する連続式反応器であって、
前記シリンダー(10)の上に隔設された多数のフランジ部(12)と、
前記各フランジ部(12)の上に反応チャンバー(11)と連通するように形成されて反応物が注入される1以上の反応物注入ポート(13)と、
前記シリンダー(10)の他方の側に反応チャンバー(11)と連通するように形成されて反応結果物が排出される反応結果物排出ポート(14)と、
前記シリンダー(10)の反応物注入ポート(13)と反応結果物排出ポート(14)との間に反応チャンバー(11)と連通するように形成される多数の余剰のポート(15)と、
前記シリンダー(10)の外周面と内周面との間に配設される温度調節部(40)と、
前記反応物注入ポート(13)の流路の上に設けられて反応物注入ポートを介して注入される反応物の粒子を粉砕する粒子粉砕部(50)と、
前記反応物注入ポート(13)と、反応結果物排出ポート(14)および余剰のポート(15)のうちの少なくともいずれかに設けられて反応物の流量を感知する流量感知センサー(60)と、
前記流量感知センサー(60)によって帰還された流量感知データーによって反応物注入ポート(13)を介して流入する反応物の流量、反応チャンバー(11)の内部を通過す る反応物の流量、または反応結果物排出ポート(14)を介して排出される反応結果物の 流量を加減制御する流量制御部(70)と、
を備えるが、
前記温度調節部(40)は、環状の冷媒チャンバー(41)と、前記冷媒チャンバーの内部に充填される冷媒(42)と、を有することを特徴とするリチウム二次電池の正極活物質前駆体製造用オールインワンタイプ連続式反応器。 - 請求項1から請求項6のいずれかに記載のオールインワンタイプ連続式反応器と、
前記オールインワンタイプ連続式反応器のフランジ部(12)に形成された多数の反応物注入ポート(13)および各連結ライン(L1、L2、L3)を介して連結される多数の反応物貯留タンク(100)と、
前記各連結ライン(L1、L2、L3)の上に設けられて各反応物貯留タンク(100)内の反応物をポンピングして前記オールインワンタイプ連続式反応器の反応チャンバー(11)に注入するためのそれぞれの供給ポンプ(200)と、
前記オールインワンタイプ連続式反応器の反応結果物排出ポート(14)と連結されて、反応結果物排出ポート(14)を介して排出される反応済みスラーリー状の物質から正極活物質前駆体およびろ液を分離する正極活物質前駆体分離器(300)と、
前記正極活物質前駆体分離器(300)と連結されて、正極活物質前駆体分離器(300)において分離された正極活物質前駆体を乾燥する乾燥器(400)と、
を備えることを特徴とする結晶分離装置。 - 前記正極活物質前駆体分離器(300)は、遠心分離器または脱水器であることを特徴とする請求項8に記載の結晶分離装置。
- 前記乾燥器(400)に連設されて、乾燥された正極活物質前駆体の粒度分布および大きさを分析する粒度分析器(500)をさらに備えることを特徴とする請求項8に記載の結晶分離装置。
- 前記粒度分析器(500)に連設されて、正極活物質前駆体の粒子形状および粒径の均一度を分析する走査電子顕微鏡(600)をさらに備えることを特徴とする請求項10に記載の結晶分離装置。
- 前記走査電子顕微鏡(600)に連設されて、正極活物質前駆体の密度を測定する密度測定器(700)をさらに備えることを特徴とする請求項11に記載の結晶分離装置。
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