JP2023530820A - 複合材剥離方法 - Google Patents
複合材剥離方法 Download PDFInfo
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- JP2023530820A JP2023530820A JP2022568795A JP2022568795A JP2023530820A JP 2023530820 A JP2023530820 A JP 2023530820A JP 2022568795 A JP2022568795 A JP 2022568795A JP 2022568795 A JP2022568795 A JP 2022568795A JP 2023530820 A JP2023530820 A JP 2023530820A
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Abstract
Description
一態様において、本明細書で提供されるのは、複合体を剥離液に浸漬することによって複合体を剥離する方法であって;複合体が、基材と、基材の片面または両面に塗布された、ポリマーバインダーを含むコーティングとを含み;ポリマーバインダーが、酸基含有モノマーから誘導される構造単位を含むコポリマーを含む方法である。
処理した電極剥離液混合物のpH値を、電極式pH計(ION2700、Eutech Instruments)で測定した。
パウチ型フルリチウムイオン電池の組み立て
A)ポリマーバインダーの調製
蒸留水380gを含む丸底フラスコに、水酸化ナトリウム(NaOH)16gを添加した。混合物を80rpmで30分間撹拌し、第1の懸濁液を得た。
導電剤(Super P(登録商標);Timcal Ltd、ボーディオ、スイスより入手)12gと、ポリマーバインダー100g(固形分9.00重量%)とをオーバーヘッドスターラー(R20、IKA)を用いて撹拌しながら脱イオン水74g中に分散させることによって、第1の混合物を調製した。添加後、25℃で約30分間、1,200rpmの速度で第1の混合物をさらに攪拌した。
黒鉛(BTR New Energy Materials Inc.、Shenzhen、広東、中国)93重量%を、1重量%カルボキシメチルセルロース(CMC、BSH-12、DKS Co. Ltd.、日本)およびバインダーである3重量%SBR(AL-2001、NIPPON A&L INC.、日本)、および導電助剤である3重量%カーボンブラックと、脱イオン水中で混合して負極スラリーを調製した。アノードスラリーの固形分は51.5重量%であった。スラリーを8μmの厚さを有する銅箔の両面にドクターブレードを用いて約120μmのギャップ幅で塗布した。銅箔上に塗布したスラリーを熱風乾燥機により約50℃で2.4分間乾燥させ、負極を得た。次いで、電極をプレスしてアノード電極層の厚さを60μmに減少させ、アノード電極層の表面密度を10mg/cm2とした。
乾燥後、得られたカソードコーティングおよびアノードコーティングを用いて、5.2cm×8.5cmおよび5.4cm×8.7cmの大きさの長方形の片に切断することで、カソードシートおよびアノードシートをそれぞれ作製した。カソードシートおよびアノードシートを交互に重ね、25μmの厚さを有する多孔質ポリエチレンセパレータ(Celgard,LLC、米国)で仕切って、パウチ型電池を調製した。電解液は、LiPF6(1M)を、体積比1:1:1のエチレンカルボナート(EC)、エチルメチルカルボナート(EMC)およびジメチルカルボナート(DMC)の混合液に溶解させたものを用いた。水分および酸素の含有量が<1ppmの高純度アルゴン雰囲気中で、セルを組み立てた。電解液を充填した後、パウチセルを真空封止し、次いで、標準形状のパンチ器具を使用して機械的にプレスした。
A)パウチ型電池の放電および分解
使用したリチウムイオン電池(0.5kg)を、6%NaCl溶液に12時間浸漬することによって、完全に放電させた。放電後、リチウムイオン電池を機械的に分解し、電極を回収した。電極を、約2cm~約4cmの平均長さを有する小片に切断した。
無水クエン酸(Sigma-Aldrich、米国)9.8gをDI水990.2gに添加し、0.98重量%のクエン酸濃度の剥離液を調製した。
カソード5.07gを、50℃で、40分間、1000gの剥離液が入った容器に入れた。カソード層をアルミニウム箔から剥離した。処理した電極-剥離液混合液は、pH値が2.05である。浸漬後、メッシュ幅4mmの篩を通過させることにより、クエン酸およびDI水を含む剥離液を除去し、カソード層およびアルミニウム箔を回収した。剥離液は、さらに電極の剥離に再利用することが可能であった。回収したカソード層とアルミ箔とを大気圧下、80℃、5時間、オーブンで乾燥させ、96.8%の回収率を得た。剥離成功率および剥離後のカソード成分の回収率を測定し、以下の表1に示す。
実施例1に記載の方法により、パウチ型リチウムイオン電池を作製した。次いで、組み立てたパウチ型電池を、実施例1と同様の方法で繰り返しサイクルに供した。
A)パウチ型電池の放電および分解
使用したリチウムイオン電池(0.5kg)を、6%NaCl溶液に12時間浸漬することによって、完全に放電させた。放電後、リチウムイオン電池を機械的に分解し、電極を回収した。電極を、約2cm~約4cmの平均長さを有する小片に切断した。
995gのDI水に5gの無水クエン酸(Sigma-Aldrich、米国)を添加し、クエン酸濃度0.50重量%の剥離液を調製した。
カソード5.08gを、50℃で、50分間、剥離液1000gの入った容器に入れた。アルミニウム箔からカソード層を剥離した。処理した電極-剥離液混合液のpH値は2.30である。浸漬後、メッシュ幅4mmの篩を通過させることにより、クエン酸およびDI水を含む剥離液を除去し、カソード層およびアルミニウム箔を回収した。剥離液は、さらに電極の剥離に再利用することが可能であった。回収したカソード層およびアルミ箔を大気圧下、80℃、5時間、オーブンで乾燥し、99.4%の回収率を得た。
A)パウチ型電池の放電および分解
使用したリチウムイオン電池(0.5kg)を、6%NaCl水溶液に12時間浸漬することによって、完全に放電させた。放電後、リチウムイオン電池を機械的に分解し、電極を回収した。電極を、約2cm~約4cmの平均長さを有する小片に切断した。
DI水997.5gに無水クエン酸2.5g(Sigma-Aldrich、米国)を添加し、クエン酸濃度0.25重量%の剥離液を調製した。
カソード5.08gを、50℃で、60分間、剥離液1000gの入った容器に入れた。カソード層をアルミニウム箔から剥離した。処理した電極-剥離液混合液のpH値は2.46である。浸漬後、メッシュ幅4mmの篩を通過させることにより、クエン酸およびDI水を含む剥離液を除去し、カソード層およびアルミニウム箔を回収した。剥離液は、さらに電極の剥離に再利用することが可能であった。回収したカソード層およびアルミニウム箔を大気圧下、80℃で5時間、オーブンで乾燥させ、96.5%の回収率を得た。
A)パウチ型電池の放電および分解
使用したリチウムイオン電池(0.5kg)を、6%NaCl溶液に12時間浸漬することによって、完全に放電させた。放電後、リチウムイオン電池を機械的に分解し、電極を回収した。電極を、約2cm~約4cmの平均長さを有する小片に切断した。
DI水999gに無水クエン酸1g(Sigma-Aldrich、米国)を添加し、クエン酸濃度0.01重量%の剥離液を調製した。
カソード5.07gを、50℃で、70分間、剥離液1000gの入った容器に入れた。カソード層をアルミニウム箔から剥離した。処理した電極-剥離液混合液のpH値は2.62である。浸漬後、メッシュ幅4mmの篩を通過させることにより、クエン酸およびDI水を含む剥離液を除去し、カソード層およびアルミニウム箔を回収した。剥離液は、さらに電極の剥離に再利用することが可能であった。回収したカソード層およびアルミニウム箔を大気圧下、80℃で5時間、オーブンで乾燥させ、96.6%の回収率を得た。
実施例2に記載の方法により、パウチ型リチウムイオン二次電池を作製した。次いで、組み立てたパウチ型電池を、実施例2と同様の方法で繰り返しサイクルに供した。
カソードを剥離液に90℃で50分間浸漬した以外は、実施例2と同様の方法で電池のリサイクルを行った。
カソードを剥離液に70℃で50分間浸漬した以外は、実施例2と同様の方法で電池のリサイクルを行った。
カソードを剥離液に25℃、50分間浸漬した以外は、実施例2と同様の方法で電池のリサイクルを行った。
カソードを剥離液に50℃、30分間浸漬した以外は、実施例2と同様の方法で電池のリサイクルを行った。
カソードを剥離液に50℃、60分間浸漬した以外は、実施例2と同様の方法で電池のリサイクルを行った。
カソードを剥離液に50℃、80分間浸漬した以外は、実施例2と同様の方法で電池のリサイクルを行った。
剥離液の調製において、無水クエン酸5gを同重量のブタン二酸に置き換えた以外は、実施例2と同様の方法で電池のリサイクルを行った。
剥離液の調製において、無水クエン酸5gを同重量のフマル酸に置き換えた以外は、実施例2と同様の方法で電池のリサイクルを行った。
剥離液の調製において、無水クエン酸5gを同重量のソルビン酸に置き換えた以外は、実施例2と同様の方法で電池のリサイクルを行った。
剥離液の調製において、無水クエン酸5gを同重量の安息香酸に置き換えた以外は、実施例2と同様の方法で電池のリサイクルを行った。
276gのNMC532を同重量のLCOに置き換えた以外は、実施例2に記載の方法により、パウチ型リチウムイオン電池を作製した。次いで、組み立てたパウチ型電池を、実施例2と同様の方法で繰り返しサイクルに供した。
276gのNMC532を同重量のNMC622(Shandong Tianjiao New Energy Co.,Ltd、中国より入手)に置き換えた以外は、実施例2に記載の方法により、パウチ型リチウムイオン電池を作製した。次いで、組み立てたパウチ型電池を、実施例2と同様の方法で繰り返しサイクルに供した。
276gのNMC532を同重量のNMC811(Shandong Tianjiao New Energy Co.,Ltd、中国より入手)に置き換えた以外は、実施例2に記載の方法により、パウチ型リチウムイオン電池を作製した。次いで、組み立てたパウチ型電池を、実施例2と同様の方法で繰り返しサイクルに供した。
276gのNMC532を同重量のLFPに置き換えた以外は、実施例2に記載の方法により、パウチ型リチウムイオン電池を作製した。次いで、組み立てたパウチ型電池を、実施例2と同様の方法で繰り返しサイクルに供した。
実施例15~18の電池のリサイクルを、実施例2と同様の方法で行った。実施例15の剥離後のカソード成分(すなわち、カソード電極層および集電体)および剥離液のICP質量分析データを、以下の表2に示す。
ポリマーバインダーの調製において、第2の懸濁液の調製で57.80gのAAを添加し、第3の懸濁液の調製でAMを添加せず、第4の懸濁液の調製で10.20gのANを添加した以外は、実施例3に記載の方法でパウチ型リチウムイオン電池を作製した。次いで、組み立てたパウチ型電池を、実施例3と同様の方法で繰り返しサイクルに供した。
カソードを剥離液に50℃で50分間浸漬したこと以外は、実施例3と同様の方法で電池のリサイクルを行った。
パウチ型フルリチウムイオン電池の組み立て
A)ポリマーバインダーの調製
水酸化リチウム5.13gをDI水3.85gに溶解させた。その後、蒸留水289.17gを含む500mL丸底フラスコに、水酸化リチウム溶液8.98gを添加した。混合物を200rpmで30分間撹拌し、第1の懸濁液を得た。
導電剤(Super P(登録商標);Timcal Ltd、ボーディオ、スイスより入手)12gおよびポリマーバインダー100g(固形分14.93重量%)をオーバーヘッドスターラー(R20、IKA)で撹拌しながら脱イオン水74gに分散させて、第1の混合物を調製した。添加後、第1の混合物を、25℃で約30分間、1,200rpmの速度でさらに攪拌した。
黒鉛(BTR New Energy Materials Inc.、Shenzhen、広東、中国)93重量%と、カルボキシメチルセルロース(CMC、BSH-12、DKS Co. Ltd.、日本)1重量%およびバインダーであるSBR(AL-2001、NIPPON A&L INC.、日本)3重量%、および導電助剤であるカーボンブラック3重量%を、脱イオン水中で混合して、負極スラリーを調製した。アノードスラリーの固形分は51.5重量%であった。スラリーを、厚さ8μmの銅箔の両面にドクターブレードを用いてギャップ幅約120μmで塗布した。この銅箔に塗布したスラリーを熱風乾燥機により約50℃で2.4分間乾燥させ、負極を得た。次いで、電極をプレスしてアノード電極層の厚さを60μmに減少させ、アノード電極層の表面密度を10mg/cm2とした。
乾燥後、得られたカソードコーティングおよびアノードコーティングを用いて、5.2cm×8.5cmおよび5.4cm×8.7cmの大きさの長方形の片に切断して、カソードシートおよびアノードシートをそれぞれ作製した。カソードシートとアノードシートとを交互に重ね、厚さ25μmの多孔質ポリエチレンセパレータ(Celgard、LLC、米国)で仕切って、パウチ型電池を作製した。電解液は、LiPF6(1M)を、体積比1:1:1のエチレンカルボナート(EC)、エチルメチルカルボナート(EMC)、ジメチルカルボナート(DMC)の混合液に溶解したものであった。水分および酸素の含有量が<1ppmの高純度アルゴン雰囲気中で、セルを組み立てた。電解液充填後、パウチセルを真空封止し、標準形状のパンチ器具を使用して機械的にプレスした。
A)パウチ型電池の放電および分解
使用したリチウムイオン電池(0.5kg)を6%NaCl水溶液に12時間浸漬し、完全に放電させた。放電後、リチウムイオン電池を機械的に分解し、電極を回収した。電極を、約2cm~約4cmの平均長さを有する小片に切断した。
無水クエン酸(Sigma-Aldrich、米国)9.8gをDI水990.2gに添加し、クエン酸濃度0.98重量%の剥離液を調製した。
カソード5.07gを、50℃、50分間、剥離液1000gの入った容器に入れた。カソード層をアルミニウム箔から剥離した。浸漬後、メッシュ幅4mmの篩を通過させることにより、クエン酸およびDI水を含む剥離液を除去し、カソード層およびアルミニウム箔を回収した。剥離液は、さらに電極の剥離に再利用することが可能であった。回収したカソード層とアルミニウム箔とを大気圧下、80℃、5時間、オーブンで乾燥させ、96.8%の回収率を得た。剥離成功率および剥離後のカソード成分の回収率を測定し、以下の表1に示す。
実施例20に記載の方法により、パウチ型リチウムイオン電池を作製した。次いで、組み立てたパウチ型電池を、実施例20と同様の方法で繰り返しサイクルに供した。
クエン酸濃度0.50重量%の剥離液の調製において、DI水995gに無水クエン酸5gを添加した以外は、実施例20と同様の方法で電池のリサイクルを実施した。
クエン酸濃度0.01重量%の剥離液の調製において、DI水999gに無水クエン酸1gを加えた以外は、実施例20と同様の方法で電池のリサイクルを行った。
実施例21に記載の方法により、パウチ型リチウムイオン電池を作製した。次いで、組み立てたパウチ型電池を、実施例21と同様の方法で繰り返しサイクルに供した。
カソードを剥離液に90℃で50分間浸漬した以外は、実施例21と同様の方法で電池のリサイクルを行った。
カソードを剥離液に40℃、50分間浸漬した以外は、実施例21と同様の方法で電池のリサイクルを行った。
カソードを剥離液に50℃、30分間浸漬した以外は、実施例21と同様の方法で電池のリサイクルを行った。
カソードを剥離液に50℃、100分間浸漬した以外は、実施例21と同様の方法で電池のリサイクルを行った。
剥離液の調製において、無水クエン酸5gを同重量のブタン二酸に置き換えたこと以外は、実施例21と同様の方法で電池のリサイクルを行った。
剥離液の調製において、無水クエン酸5gを同重量のフマル酸に置き換えた以外は、実施例21と同様の方法で、電池のリサイクルを実施した。
剥離液の調製において、無水クエン酸5gを同重量のソルビン酸に置き換えた以外は、実施例21と同様の方法で、電池のリサイクルを実施した。
剥離液の調製において、無水クエン酸5gを同重量の安息香酸に置き換えた以外は、実施例21と同様の方法で、電池のリサイクルを実施した。
276gのNMC532を同重量のLCOに置き換えた以外は、実施例21に記載の方法により、パウチ型リチウムイオン電池を作製した。次いで、組み立てたパウチ型電池を、実施例21と同様の方法で繰り返しサイクルに供した。
282gのNMC532を同重量のNMC622に置き換えた以外は、実施例21に記載の方法により、パウチ型リチウムイオン電池を作製した。次いで、組み立てたパウチ型電池を、実施例21と同様の方法で繰り返しサイクルに供した。
282gのNMC532を同重量のNMC811に置き換えた以外は、実施例21に記載の方法により、パウチ型リチウムイオン電池を作製した。そして、組み立てたパウチ型電池を、実施例21と同様の方法で繰り返しサイクルに供した。
282gのNMC532を同重量のLFPに置き換えた以外は、実施例21に記載の方法により、パウチ型リチウムイオン電池を作製した。次いで、組み立てたパウチ型電池を、実施例21と同様の方法で繰り返しサイクルに供した。
実施例31~34の電池のリサイクルは、実施例21と同様の方法で行った。
ポリマーバインダーの調製において、第2の懸濁液の調製で22.53gのAAを添加し、第3の懸濁液の調製でAMを添加せず、第4の懸濁液の調製で90.13gのANを添加した以外は、実施例21に記載の方法でパウチ型リチウムイオン電池を作製した。次いで、組み立てたパウチ型電池を、実施例21と同様の方法で繰り返しサイクルに供した。
実施例21と同様の方法で、電池のリサイクルを行った。
ポリマーバインダーの調製において、第2の懸濁液の調製で36.04gのAAを同重量の2-エチルアクリル酸に置き換えた以外は、実施例2に記載の方法により、パウチ型リチウムイオン電池を作製した。次いで、組み立てたパウチ型電池を、実施例2と同様の方法で繰り返しサイクルに供した。
実施例2と同様の方法で、電池のリサイクルを行った。
ポリマーバインダーの調製において、第2の懸濁液の調製で36.04gのAAを同重量のビニルスルホン酸に置き換えた以外は、実施例2に記載の方法により、パウチ型リチウムイオン電池を作製した。次いで、組み立てたパウチ型電池を、実施例2と同様の方法で繰り返しサイクルに供した。
実施例2と同様にして、電池のリサイクルを行った。
ポリマーバインダーの調製において、第2の懸濁液の調製で31.54gのAAを同重量の2-エチルアクリル酸に置き換えた以外は、実施例21に記載の方法により、パウチ型リチウムイオン電池を作製した。次いで、組み立てたパウチ型電池を、実施例21と同様の方法で繰り返しサイクルに供した。
実施例21と同様の方法で、電池のリサイクルを行った。
ポリマーバインダーの調製において、第2の懸濁液の調製で31.54gのAAを同重量のビニルスルホン酸に置き換えた以外は、実施例21に記載の方法により、パウチ型リチウムイオン電池を作製した。次いで、組み立てたパウチ型電池を、実施例21と同様の方法で繰り返しサイクルに供した。
実施例21と同様の方法で、電池のリサイクルを行った。
A)ポリマーバインダーの調製
ポリフッ化ビニリデン、PVDF(Solef(登録商標)5130、Solvay S.A.、ベルギーから入手)10gを、N-メチル-2-ピロリドン、NMP(≧99%、Sigma-Aldrich、米国)100g中に500rpmで約3時間撹拌しながら分散させ、ポリマーバインダーを調製した。
オーバーヘッドスターラーで攪拌しながら、500mLの丸底フラスコ中で、上記ポリマーバインダー110gをNMP150gに分散させ、第1の懸濁液を調製した。添加後、第1の懸濁液を500rpmの速度で約10分間さらに攪拌した。
実施例2と同様の方法で、負極を作製した。
実施例2と同様の方法で、パウチ型電池を組み立てた。次いで、組み立てたパウチ型電池を、実施例2と同様の方法で繰り返しサイクルに供した。
実施例2と同様の方法で、電池のリサイクルを行った。
正極の作製において、ポリマーバインダーとしてポリアクリロニトリル(PAN)を用いた以外は、実施例21に記載の方法により、パウチ型リチウムイオン電池を作製した。次いで、組み立てたパウチ型電池を、実施例21と同様の方法で繰り返しサイクルに供した。
実施例21と同様の方法で、電池のリサイクルを行った。
実施例21に記載の方法により、パウチ型リチウムイオン電池を作製した。次いで、組み立てたパウチ型電池を、実施例21と同様の方法で繰り返しサイクルに供した。
硫酸濃度が3重量%の剥離液の調製において、DI水970gに硫酸30gを添加し、カソードを剥離液に50℃で10分間浸漬した以外は、実施例21と同様の方法で電池のリサイクルを実施した。
硫酸濃度が0.50重量%の剥離液の調製において、DI水995gに硫酸5gを添加し、カソードを剥離液に50℃で10分間浸漬した以外は、実施例21と同様の方法で電池のリサイクルを実施した。
硫酸濃度が3重量%の剥離液の調製において、DI水970gに硫酸30gを添加した以外は、実施例21と同様の方法で電池のリサイクルを実施した。
硫酸濃度が0.50重量%の剥離液の調製において、DI水995gに硫酸5gを添加した以外は、実施例21と同様の方法で電池のリサイクルを実施した。
パウチ型リチウムイオン電池を実施例2に記載の方法により作製した。組み立てたパウチ型電池を実施例2と同様の方法で繰り返しサイクルに供した。
硫酸濃度が3重量%の剥離液の調製において、DI水970gに硫酸30gを添加し、カソードを剥離液に50℃で10分間浸漬した以外は、実施例2と同様の方法で電池のリサイクルを実施した。
硫酸濃度が0.50重量%の剥離液の調製において、DI水995gに硫酸5gを添加し、カソードを剥離液に50℃で10分間浸漬した以外は、実施例2と同様の方法で電池のリサイクルを実施した。剥離後のカソード成分(すなわち、カソード電極層および集電体)および比較例8の剥離液のICP質量分析データを以下の表2に示す。
硫酸濃度が3重量%の剥離液の調製において、DI水970gに硫酸30gを添加した以外は、実施例2と同様の方法で電池のリサイクルを実施した。
硫酸濃度が0.50重量%の剥離液の調製において、DI水995gに硫酸5gを添加した以外は、実施例2と同様の方法で電池のリサイクルを実施した。
パウチ型リチウムイオン電池を実施例2に記載の方法により作製した。次いで、組み立てたパウチ型電池を実施例2と同様の方法で繰り返しサイクルに供した。
クエン酸濃度が2重量%の剥離液の調製において、DI水980gに無水クエン酸20gを添加した以外は、実施例2と同様の方法で電池のリサイクルを実施した。
パウチ型リチウムイオン電池を実施例21に記載の方法により作製した。次いで、組み立てたパウチ型電池を実施例21と同様の方法で繰り返しサイクルに供した。
クエン酸濃度が2重量%の剥離液の調製において、DI水980gに無水クエン酸20gを添加した以外は、実施例21と同様の方法で電池のリサイクルを実施した。
パウチ型リチウムイオン電池を実施例21に記載の方法により作製した。次いで、組み立てたパウチ型電池を実施例21と同様の方法で繰り返しサイクルに供した。
酸濃度が3重量%の剥離液の調製において、DI水970gに無水クエン酸15gと硫酸15gとを添加し、カソードを剥離液に50℃で10分間浸漬した以外は、実施例21と同様の方法で電池のリサイクルを実施した。
酸濃度が0.50重量%の剥離液の調製において、DI水995gに無水クエン酸2.5gと硫酸2.5gとを添加し、カソードを剥離液に50℃で10分間浸漬した以外は、実施例21と同様の方法で電池のリサイクルを実施した。
酸濃度が0.50重量%の剥離液の調製において、DI水995gに無水クエン酸2.5gと硫酸2.5gとを添加した以外は、実施例21と同様の方法で電池のリサイクルを実施した。
パウチ型リチウムイオン電池を実施例2に記載の方法により作製した。次いで、組み立てたパウチ型電池を実施例2と同様の方法で繰り返しサイクルに供した。
酸濃度が3重量%の剥離液の調製において、DI水970gに無水クエン酸15gと硫酸15gとを添加し、カソードを剥離液に50℃で10分間浸漬した以外は、実施例2と同様の方法で電池のリサイクルを実施した。
酸濃度が0.50重量%の剥離液の調製において、DI水995gに無水クエン酸2.5gと硫酸2.5gとを添加し、カソードを剥離液に50℃で10分間浸漬した以外は、実施例2と同様の方法で電池のリサイクルを実施した。
酸濃度が0.50重量%の剥離液の調製において、DI水995gに無水クエン酸2.5gと硫酸2.5gとを添加した以外は、実施例2と同様の方法で電池のリサイクルを実施した。
パウチ型リチウムイオン電池を実施例21に記載の方法により作製した。次いで、組み立てたパウチ型電池を実施例21と同様の方法で繰り返しサイクルに供した。
酸濃度が3重量%の剥離液の調製において、DI水970gに酢酸10gと無水クエン酸10gと硫酸10gとを添加し、カソードを剥離液に50℃で10分間浸漬した以外は、実施例21と同様の方法で電池のリサイクルを実施した。
酸濃度が0.50重量%の剥離液の調製において、DI水995gに酢酸1.67gと無水クエン酸1.67gと硫酸1.67gとを添加し、カソードを剥離液に50℃で10分間浸漬した以外は、実施例21と同様の方法で電池のリサイクルを実施した。
酸濃度が0.50重量%の剥離液の調製において、DI水995gに酢酸1.67gと無水クエン酸1.67gと硫酸1.67gとを添加した以外は、実施例21と同様の方法で電池のリサイクルを実施した。
パウチ型リチウムイオン電池を実施例2に記載の方法により作製した。次いで、組み立てたパウチ型電池を実施例2と同様の方法で繰り返しサイクルに供した。
酸濃度が3重量%の剥離液の調製において、DI水970gに酢酸10gと無水クエン酸10gと硫酸10gとを添加し、カソードを剥離液に50℃で10分間浸漬した以外は、実施例2と同様の方法で電池のリサイクルを実施した。
酸濃度が0.50重量%の剥離液の調製において、DI水995gに酢酸1.67gと無水クエン酸1.67gと硫酸1.67gとを添加し、カソードを剥離液に50℃で10分間浸漬した以外は、実施例2と同様の方法で電池のリサイクルを実施した。
酸濃度が0.50重量%の剥離液の調製において、DI水995gに酢酸1.67gと無水クエン酸1.67gと硫酸1.67gとを添加した以外は、実施例2と同様の方法で電池のリサイクルを実施した。
ポリマーバインダーの調製において、16.90gのAAを第2の懸濁液の調製時に添加し、AMを第3の懸濁液の調製時に添加せず、95.76gのANを第4の懸濁液の調製時に添加した以外は、パウチ型リチウムイオン電池を実施例21に記載の方法により作製した。次いで、組み立てたパウチ型電池を実施例21と同様の方法で繰り返しサイクルに供した。
実施例21と同様の方法で電池のリサイクルを実施した。
パウチ型リチウムイオン電池を実施例21に記載の方法により作製した。次いで、組み立てたパウチ型電池を実施例21と同様の方法で繰り返しサイクルに供した。
剥離液の調製において、剥離剤を添加せず、1000gのDI水のみを添加した以外は、実施例21と同様の方法で電池のリサイクルを実施した。
パウチ型リチウムイオン電池を実施例2に記載の方法により作製した。次いで、組み立てたパウチ型電池を実施例2と同様の方法で繰り返しサイクルに供した。
剥離液の調製において、剥離剤を添加せず、1000gのDI水のみを添加した以外は、実施例2と同様の方法で電池のリサイクルを実施した。
ポリマーバインダーの調製において、57.80gのAAを第2の懸濁液の調製時に添加し、AMを第3の懸濁液の調製時に添加せず、10.20gのANを第4の懸濁液の調製時に添加した以外は、パウチ型リチウムイオン電池を実施例2に記載の方法により作製した。次いで、組み立てたパウチ型電池を実施例2と同様の方法で繰り返しサイクルに供した。
剥離液の調製において、剥離剤を添加せず、1000gのDI水のみを添加した以外は、実施例2と同様の方法で電池のリサイクルを実施した。
Claims (20)
- 複合体を剥離液に浸漬することによって前記複合体を剥離する方法であって;
前記複合体が、基材と、前記基材の片面または両面に塗布された、ポリマーバインダーを含むコーティングとを含み;
前記ポリマーバインダーが、酸基含有モノマーから誘導される構造単位を含むコポリマーを含むことを特徴とする、前記方法。 - 前記コポリマーが、ニトリル基含有モノマー、アミド基含有モノマー、ヒドロキシル基含有モノマー、エステル基含有モノマー、エポキシ基含有モノマー、フッ素含有モノマーまたはそれらの組み合わせからなる群から選択される水素結合形成基含有モノマーから誘導される構造単位をさらに含む、請求項1に記載の方法。
- 水素結合形成基含有モノマーから誘導される構造単位の割合が、前記ポリマーバインダー中の前記コポリマー中のモノマー単位の総数モルに基づいて、約5モル%~約85モル%である、請求項2に記載の方法。
- 前記基材が、箔、シート、フィルムまたはそれらの組み合わせの形態であり;
前記基材が、ステンレス鋼、チタン、ニッケル、アルミニウム、銅、白金、金、銀、クロム、ジルコニウム、タングステン、モリブデン、ケイ素、スズ、バナジウム、亜鉛、カドミウム、若しくはそれらの合金、導電性樹脂またはそれらの組み合わせからなる群から選択され;
前記基材が外層および内層を含む2層構造を有し、前記外層が導電性材料を含み、および前記内層が絶縁材料または他の導電性材料を含む、請求項1に記載の方法。 - 前記導電性材料が、ステンレス鋼、チタン、ニッケル、アルミニウム、銅、白金、金、銀、クロム、ジルコニウム、タングステン、モリブデン、ケイ素、スズ、バナジウム、亜鉛、カドミウム、若しくははそれらの合金、導電性樹脂またはこれらの組み合わせからなる群から選択され;
前記絶縁材料が、ポリカルボナート、ポリアクリラート、ポリアクリロニトリル、ポリエステル、ポリアミド、ポリスチレン、ポリウレタン、ポリエポキシ、ポリ(アクリロニトリルブタジエンスチレン)、ポリイミド、ポリオレフィン、ポリエチレン、ポリプロピレン、ポリフェニレンスルフィド、ポリ(ビニルエステル)、ポリ塩化ビニル、ポリエーテル、ポリフェニレンオキシド、セルロースポリマーおよびそれらの組み合わせからなる群から選択されるポリマー材料であることを特徴とする、請求項4に記載の方法。 - 前記酸基含有モノマーが、カルボン酸基含有モノマー、スルホン酸基含有モノマー、ホスホン酸基含有モノマーまたはそれらの組み合わせからなる群から選択される、請求項1に記載の方法。
- 前記カルボン酸基含有モノマーが、アクリル酸、メタクリル酸、クロトン酸、2-ブチルクロトン酸、ケイ皮酸、マレイン酸、マレイン酸無水物、フマル酸、イタコン酸、イタコン酸無水物、テトラコン酸(tetraconic acid)、2-エチルアクリル酸、イソクロトン酸、cis-2-ペンテン酸、trans-2-ペンテン酸、アンゲリカ酸、チグリン酸、3,3-ジメチルアクリル酸、3-プロピルアクリル酸、trans-2-メチル-3-エチルアクリル酸、cis-2-メチル-3-エチルアクリル酸、3-イソプロピルアクリル酸、trans-3-メチル-3-エチルアクリル酸、cis-3-メチル-3-エチルアクリル酸、2-イソプロピルアクリル酸、トリメチルアクリル酸、2-メチル-3,3-ジエチルアクリル酸、3-ブチルアクリル酸、2-ブチルアクリル酸、2-ペンチルアクリル酸、2-メチル-2-ヘキセン酸、trans-3-メチル-2-ヘキセン酸、3-メチル-3-プロピルアクリル酸、2-エチル-3-プロピルアクリル酸、2,3-ジエチルアクリル酸、3,3-ジエチルアクリル酸、3-メチル-3-へキシルアクリル酸、3-メチル-3-tert-ブチルアクリル酸、2-メチル-3-ペンチルアクリル酸、3-メチル-3-ペンチルアクリル酸、4-メチル-2-ヘキセン酸、4-エチル-2-ヘキセン酸、3-メチル-2-エチル-2-ヘキセン酸、3-tert-ブチルアクリル酸、2,3-ジメチル-3-エチルアクリル酸、3,3-ジメチル-2-エチルアクリル酸、3-メチル-3-イソプロピルアクリル酸、2-メチル-3-イソプロピルアクリル酸、trans-2-オクテン酸、cis-2-オクテン酸、trans-2-デセン酸、α-アセトキシアクリル酸、β-trans-アリールオキシアクリル酸、α-クロロ-β-E-メトキシアクリル酸、メチルマレイン酸、ジメチルマレイン酸、フェニルマレイン酸、ブロモマレイン酸、クロロマレイン酸、ジクロロマレイン酸、フルオロマレイン酸、ジフルオロマレイン酸、ノニル水素マレアート、デシル水素マレアート、ドデシル水素マレアート、オクタデシル水素マレアート、フルオロアルキル水素マレアート、マレイン酸無水物、メチルマレイン酸無水物、ジメチルマレイン酸無水物、アクリル酸無水物、メタクリル酸無水物、メタクロレイン、塩化メタクリロイル、フッ化メタクリロイル、臭化メタクリロイル、およびそれらの組合せからなる群から選択される、請求項6に記載の方法。
- 前記スルホン酸基含有モノマーが、ビニルスルホン酸、メチルビニルスルホン酸、アリルビニルスルホン酸、アリルスルホン酸、メタリルスルホン酸、スチレンスルホン酸、2-スルホエチルメタクリル酸、2-メチルプロパ-2-エン-1-スルホン酸、2-アクリルアミド-2-メチル-1-プロパンスルホン酸、3-アリルオキシ-2-ヒドロキシ-1-プロパンスルホン酸およびそれらの組合せからなる群から選択される、請求項6に記載の方法。
- 前記ホスホン酸基含有モノマーが、ビニルホスホン酸、アリルホスホン酸、ビニルベンジルホスホン酸、アクリルアミドアルキルホスホン酸、メタクリルアミドアルキルホスホン酸、アクリルアミドアルキルジホスホン酸、アクリロイルホスホン酸、2-メタクリロイルオキシエチルホスホン酸、ビス(2-メタクリロイルオキシエチル)ホスホン酸、エチレン2-メタクリロイルオキシエチルホスホン酸、エチル-メタクリロイルオキシエチルホスホン酸およびそれらの組み合わせからなる群から選択される、請求項6に記載の方法。
- 酸基含有モノマーから誘導される構造単位の割合が、前記ポリマーバインダー中の前記コポリマー中のモノマー単位の総数モルに基づいて、約15モル%~約85モル%である、請求項1に記載の方法。
- 前記コポリマーが、ニトリル基含有モノマーから誘導される構造単位およびアミド基含有モノマーから誘導される構造単位をさらに含む、請求項1に記載の方法。
- 前記ニトリル基含有モノマーが、アクリロニトリル、α-ハロゲノアクリロニトリル、α-アルキルアクリロニトリル、α-クロロアクリロニトリル、α-ブロモアクリロニトリル、α-フルオロアクリロニトリル、メタクリロニトリル、α-エチルアクリロニトリル、α-イソプロピルアクリロニトリル、α-n-ヘキシルアクリロニトリル、α-メトキシアクリロニトリル、3-メトキシアクリロニトリル、3-エトキシアクリロニトリル、α-アセトキシアクリロニトリル、α-フェニルアクリロニトリル、α-トリルアクリロニトリル、α-(メトキシフェニル)アクリロニトリル、α-(クロロフェニル)アクリロニトリル、α-(シアノフェニル)アクリロニトリル、ビニリデンシアニドおよびそれらの組合せからなる群から選択され;
ニトリル基含有モノマーから誘導される構造単位の割合が、ポリマーバインダー中のコポリマー中のモノマー単位の総数モルに基づいて、約15モル%~約85モル%である、請求項11に記載の方法。 - 前記アミド基含有モノマーが、アクリルアミド、メタクリルアミド、N-メチルメタクリルアミド、N-エチルメタクリルアミド、N-n-プロピルメタクリルアミド、N-イソプロピルメタクリルアミド、イソプロピルアクリルアミド、N-n-ブチルメタクリルアミド、N-イソブチルメタクリルアミド、N,N-ジメチルアクリルアミド、N,N-ジメチルメタクリルアミド、N,N-ジエチルアクリルアミド、N,N-ジエチルメタクリルアミド、N-メチロールメタクリルアミド、N-(メトキシメチル)メタクリルアミド、N-(エトキシメチル)メタクリルアミド、N-(プロポキシメチル)メタクリルアミド、N-(ブトキシメチル)メタクリルアミド、N,N-ジメチルメタクリルアミド、N,N-ジメチルアミノプロピルメタクリルアミド、N,N-ジメチルアミノエチルメタクリルアミド、N,N-ジメチロールメタクリルアミド、ジアセトンメタクリルアミド、ジアセトンアクリルアミド、メタクリロイルモルホリン、N-ヒドロキシルメタクリルアミド、N-メトキシメチルアクリルアミド、N-メトキシメチルメタクリルアミド、N,N’-メチレン-ビス-アクリルアミド(MBA)、N-ヒドロキシメチルアクリルアミド、およびそれらの組合せからなる群から選択され;
アミド基含有モノマーから誘導される構造単位の割合が、ポリマーバインダー中のコポリマー中のモノマー単位のモルの総数に基づいて、約0モル%~約35モル%である、請求項11に記載の方法。 - 前記剥離液が、剥離剤と水性溶媒とを含む、請求項1に記載の方法。
- 前記剥離剤が、ギ酸、酢酸、グリコール酸、グリオキシル酸、シュウ酸、プロピオン酸、アクリル酸、プロピオル酸、乳酸、3-ヒドロキシプロピオン酸、グリセリン酸、ピルビン酸、3-オキソプロピオン酸、2,3-ジオキソプロピオン酸、マロン酸、タルトロン酸、ジヒドロキシマロン酸、メソシュウ酸、グリシド酸、酪酸、イソ酪酸、クロトン酸、イソクロトン酸、メタクリル酸、ビニル酢酸、テトロル酸、2-ヒドロキシ酪酸、3-ヒドロキシ酪酸、4-ヒドロキシ酪酸、2-オキソブタン酸、アセト酢酸、4-オキソブタン酸、ブタン二酸、メチルマロン酸、フマル酸、マレイン酸、2-ヒドロキシブタン二酸、酒石酸、オキサロ酢酸、ジオキソコハク酸、吉草酸、イソ吉草酸、2-メチルブチル酸(2-methylbutiric acid)、ピバル酸、3-ヒドロキシ吉草酸、4-ヒドロキシペンタン酸、3-ヒドロキシイソ吉草酸、グルタル酸、2-オキソグルタル酸、3-オキソグルタル酸、2-フロ酸、テトラヒドロフロ酸、ヘキサン酸、ヘキサン二酸、クエン酸、アコニット酸、イソクエン酸、ソルビン酸、ピメリン酸、安息香酸、サリチル酸、4-カルボキシ安息香酸、トリメシン酸、メリト酸、リンゴ酸、およびそれらの組合せからなる群から選択され;
前記水性溶媒が水、または水を主成分として含み微量成分を含む溶液である、請求項14に記載の方法。 - 前記水性溶媒中の水の割合が約51重量%~約100重量%であり;
前記微量成分がメタノール、エタノール、イソプロパノール、n-プロパノール、tert-ブタノール、n-ブタノール、アセトン、ジメチルケトン、メチルエチルケトン、エチルアセタート、イソプロピルアセタート、プロピルアセタート、ブチルアセタート、およびこれらの組み合わせからなる群から選択される、請求項15に記載の方法。 - 前記剥離液に対する前記複合体の重量比が約0.01%~約5%である、請求項1に記載の方法。
- 前記剥離液中の前記剥離剤の濃度が、前記剥離液の総重量に基づいて約0.01重量%~約1重量%である、請求項14に記載の方法。
- 前記複合体を約15分~約120分の時間、前記剥離液に浸漬し;
前記複合体を約25℃~約95℃の温度で前記剥離液に浸漬する、請求項1に記載の方法。 - 前記複合体-剥離液混合物を約10rpm~約3000rpmの速度で撹拌し;
前記複合体-剥離液混合物を約1分~約120分の時間撹拌する、請求項1に記載の方法。
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PCT/CN2020/110065 WO2021253615A1 (en) | 2020-06-17 | 2020-08-19 | Binder composition for secondary battery |
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