JP2011032445A - 多孔質フィルム、電池用セパレータ及び電池 - Google Patents
多孔質フィルム、電池用セパレータ及び電池 Download PDFInfo
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- JP2011032445A JP2011032445A JP2009183164A JP2009183164A JP2011032445A JP 2011032445 A JP2011032445 A JP 2011032445A JP 2009183164 A JP2009183164 A JP 2009183164A JP 2009183164 A JP2009183164 A JP 2009183164A JP 2011032445 A JP2011032445 A JP 2011032445A
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- porous film
- heat
- molecular weight
- battery
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- LXEJRKJRKIFVNY-UHFFFAOYSA-N terephthaloyl chloride Chemical compound ClC(=O)C1=CC=C(C(Cl)=O)C=C1 LXEJRKJRKIFVNY-UHFFFAOYSA-N 0.000 description 1
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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
Landscapes
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
- Laminated Bodies (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Cell Separators (AREA)
Abstract
【解決手段】超高分子量ポリオレフィンと重量平均分子量3000以下のポリオレフィンワックスとを含む樹脂組成物を用いて得られる多孔質フィルムであって、60℃以下で溶融する成分を実質的に含まない多孔質フィルム。前記多孔質フィルムの少なくとも片面に、多孔質の耐熱層が積層されている積層多孔質フィルム。電池用セパレータである前記多孔質フィルムまたは積層多孔質フィルム。
【選択図】なし
Description
[1]超高分子量ポリオレフィンと重量平均分子量3000以下のポリオレフィンワックスとを含む樹脂組成物を用いて得られる多孔質フィルムであって、60℃以下で溶融する成分を実質的に含まない多孔質フィルム。
[2]上記[1]における樹脂組成物が、ポリオレフィンワックスを5〜50重量%含む多孔質フィルム(ただし樹脂組成物の重量を100%とする)。
[3]上記[1]または[2]に記載の多孔質フィルムの少なくとも片面に、多孔質の耐熱層が積層されている積層多孔質フィルム。
[4]電池用セパレータである上記[1]または[2]に記載の多孔質フィルム、あるいは上記[3]に記載の積層多孔質フィルム。
[5]上記[4]に記載の電池用セパレータを含む電池。
多孔質フィルムに60℃で溶融する成分が含まれるかどうかは、示差走査熱量測定(DSC)によって確認することができる。
塗工性の観点から耐熱樹脂は、固有粘度1.0〜2.8dl/gの耐熱樹脂であることが好ましく、固有粘度1.7〜2.5dl/gの耐熱樹脂であることがより好ましい。ここでの固有粘度は、一度析出させた耐熱樹脂を溶解し、耐熱樹脂硫酸溶液にして測定された値である。塗工性の観点から塗工液中の耐熱樹脂濃度は0.5〜10重量%であることが好ましい。
がより好ましい。塩化物が0.5モル以上であると、生成するパラアラミドの溶解性が十分となり、6.0モル以下であると塩化物が溶媒に溶け残ることがなくなるため好ましい。一般には、アルカリ金属、またはアルカリ土類金属の塩化物が2重量%以上でパラアラミドの溶解性が十分となる場合が多く、10重量%以下でアルカリ金属、またはアルカリ土類金属の塩化物が極性アミド系溶媒または極性尿素系溶媒などの極性有機溶媒に溶け残ることなく完全に溶解する場合が多い。
該無機微粒子の含有量は多孔質フィルム中1重量%〜95重量%以下であることが好ましく、5重量%〜50重量%であることがより好ましい。1重量%以上であると、十分な多孔性が得られるためイオン透過性に優れ、95重量%以下であると十分な膜強度が得られるためハンドリングに優れる。使用する無機微粒子の形状は、特に限定はなく、球状でもランダムな形状でも使用できる。
(a)耐熱樹脂100重量部を含む極性有機溶媒溶液に、耐熱樹脂100重量部に対しセラミックス粉末を1〜500重量部分散したスラリー状塗工液を調整する
(b)該塗工液を多孔質フィルムの少なくとも片面に塗工し、塗工膜を形成する。
(c)加湿、溶媒除去、あるいは耐熱樹脂を溶解しない溶媒への浸漬などの手段で、前記塗工膜から耐熱樹脂を析出させた後、必要に応じて乾燥する。
塗工液は、特開2001−316006号公報に記載の塗工装置及び特開2001−23602号公報に記載の方法により連続的に塗工することが好ましい。
セイコーインスツル株式会社製のSSC/5200を用いて、昇温速度10℃/分で測定した。
パラアラミド(ポリ(パラフェニレンテレフタルアミド))の合成
攪拌翼、温度計、窒素流入管及び粉体添加口を有する、3リットルのセパラブルフラスコを使用して、ポリ(パラフェニレンテレフタルアミド)の製造を行った。フラスコを十分乾燥し、N−メチル−2−ピロリドン(NMP)2200gを仕込み、200℃で2時間真空乾燥した塩化カルシウム粉末151.07gを添加し、100℃に昇温して完全に溶解させた。室温に戻して、パラフェニレンジアミン、68.23gを添加し完全に溶解させた。この溶液を20℃±2℃に保ったまま、テレフタル酸ジクロライド、124.97gを10分割して約5分おきに添加した。その後も攪拌しながら、溶液を20℃±2℃に保ったまま1時間熟成した。1500メッシュのステンレス金網でろ過した。得られた溶液は、パラアラミド濃度6%であった。
塗工液の調整
先に重合したパラアラミド溶液100gをフラスコに秤取し、300gのNMPを添加し、パラアラミド濃度が1.5重量%の溶液に調製して60分間攪拌した。上記のパラアラミド濃度が1.5重量%の溶液に、アルミナC(日本アエロジル社製)を6g、アドバンスドアルミナAA−03(住友化学社製)を6g混合し、240分間攪拌した。得られた溶液を1000メッシュの金網でろ過し、その後酸化カルシウム0.73gを添加して240分間攪拌して中和を行い、減圧下で脱泡してスラリー上の塗工液を得た。
接着強度の測定
得られた塗工液を多孔質フィルム上に130μm厚となるようにバーコーターで塗布した後、50℃70%RHのオーブンに15秒間入れ、多孔質フィルム上にアラミドを析出させた。1.5Rの突起を1つ有する2cm角のSUS板の上に錘を載せて、突起部を析出させたアラミド層の上に滑らせ、アラミド層が剥がれない最大の錘の重さを測定した。錘の重さが大きいほど、アラミド層と多孔質フィルムの接着強度が高い。
超高分子量ポリエチレン粉末(340M、三井化学社製)を70重量%、重量平均分子量1000のポリエチレンワックス(FNP−0115、日本精鑞社製)30重量%、この超高分子量ポリエチレンとポリエチレンワックスの100重量部に対して、酸化防止剤(Irg1010、チバ・スペシャリティ・ケミカルズ社製)0.4重量%、(P168、チバ・スペシャリティ・ケミカルズ社製)0.1重量%、ステアリン酸ナトリウム1.3重量%を加え、更に全体積に対して38体積%となるように平均孔径0.1μmの炭酸カルシウム(丸尾カルシウム社製)を加え、これらを粉末のままヘンシェルミキサーで混合した後、二軸混練機で溶融混練してポリオレフィン樹脂組成物とした。該ポリオレフィン樹脂組成物を表面温度が150℃一対のロールにて圧延し、膜厚約60μmのシートを作成した。このシートを塩酸水溶液(塩酸4mol/L、非イオン系界面活性剤0.5重量%)に浸漬させることで炭酸カルシウムを除去し、続いて105℃で5.8倍に延伸して多孔質フィルム(A)を得た。
多孔質フィルム(A)のDSC測定を行なったところ、60℃で溶融する成分が存在しないことが確かめられた。
前記(2)の「接着強度測定」に記載した方法に従い、多孔質フィルム(A)にアラミド層を積層してその接着強度を測定したところ、9gであった。
ポリエチレンワックスとして、三井化学社製の重量平均分子量1000のハイワックス110Pを用いた以外は実施例1と同様にして、多孔質フィルム(B)を得た。
多孔質フィルム(B)のDSC測定を行なったところ、60℃以下で溶融する成分が存在することが確かめられた。
多孔質フィルム(B)に、実施例1と同様にしてアラミド層を積層してその接着強度を測定したところ、5gであった。
Claims (6)
- 超高分子量ポリオレフィンと重量平均分子量3000以下のポリオレフィンワックスとを含む樹脂組成物を用いて得られる多孔質フィルムであって、60℃以下で溶融する成分を実質的に含まない多孔質フィルム。
- 前記樹脂組成物が、ポリオレフィンワックスを5〜50重量%含む請求項1に記載の多孔質フィルム(ただし樹脂組成物の重量を100%とする)。
- 請求項1または2に記載の多孔質フィルムの少なくとも片面に、多孔質の耐熱層が積層されている積層多孔質フィルム。
- 電池用セパレータである請求項1または2に記載の多孔質フィルム。
- 電池用セパレータである請求項3に記載の積層多孔質フィルム。
- 請求項5または6に記載の電池用セパレータを含む電池。
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CN201080034814.7A CN102471518B (zh) | 2009-08-06 | 2010-08-02 | 多孔膜、电池用隔膜和电池 |
KR1020127003023A KR101679451B1 (ko) | 2009-08-06 | 2010-08-02 | 다공질 필름, 전지용 세퍼레이터 및 전지 |
US13/388,874 US9259900B2 (en) | 2009-08-06 | 2010-08-02 | Porous film, battery separator, and battery |
EP10806570.7A EP2463331A4 (en) | 2009-08-06 | 2010-08-02 | POROUS FILM, SEPARATOR FOR BATTERIES AND BATTERY |
KR1020167032188A KR101791376B1 (ko) | 2009-08-06 | 2010-08-02 | 다공질 필름, 전지용 세퍼레이터 및 전지 |
PCT/JP2010/063437 WO2011016571A1 (ja) | 2009-08-06 | 2010-08-02 | 多孔質フィルム、電池用セパレータ及び電池 |
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JP2022016067A (ja) | 2020-07-10 | 2022-01-21 | 住友化学株式会社 | 非水電解液二次電池用セパレータの検査方法、製造方法、検査装置および製造装置、並びに非水電解液二次電池用セパレータ |
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US20220069414A1 (en) | 2020-09-03 | 2022-03-03 | Sumitomo Chemical Company, Limited | Porous layer for nonaqueous electrolyte secondary battery |
US20220069418A1 (en) | 2020-09-03 | 2022-03-03 | Sumitomo Chemical Company, Limited | Porous layer for nonaqueous electrolyte secondary battery |
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WO2000020493A1 (en) * | 1998-10-01 | 2000-04-13 | Tonen Chemical Corporation | Microporous polyolefin film and process for producing the same |
JP2002069221A (ja) * | 2000-06-14 | 2002-03-08 | Sumitomo Chem Co Ltd | 多孔質フィルムおよびそれを用いた電池用セパレータ |
JP2002128943A (ja) * | 2000-10-26 | 2002-05-09 | Tonen Chem Corp | ポリオレフィン微多孔膜及びその製造方法 |
JP2006307163A (ja) * | 2005-03-31 | 2006-11-09 | Sumitomo Chemical Co Ltd | ポリオレフィン系樹脂組成物からなるシート、多孔性フィルムおよび電池用セパレータ |
Cited By (3)
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KR20150046127A (ko) * | 2012-08-23 | 2015-04-29 | 제이엔씨 주식회사 | 우수한 내열성을 갖는 복합 다공성막 |
KR101698370B1 (ko) * | 2012-08-23 | 2017-01-20 | 제이엔씨 주식회사 | 우수한 내열성을 갖는 복합 다공성막 |
US9748542B2 (en) | 2012-08-23 | 2017-08-29 | Jnc Corporation | Composite porous film having excellent heat resistance |
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