JPWO2017038615A1 - ラミネート用接着剤、多層フィルム、及びこれを用いた二次電池 - Google Patents
ラミネート用接着剤、多層フィルム、及びこれを用いた二次電池 Download PDFInfo
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- JPWO2017038615A1 JPWO2017038615A1 JP2017508693A JP2017508693A JPWO2017038615A1 JP WO2017038615 A1 JPWO2017038615 A1 JP WO2017038615A1 JP 2017508693 A JP2017508693 A JP 2017508693A JP 2017508693 A JP2017508693 A JP 2017508693A JP WO2017038615 A1 JPWO2017038615 A1 JP WO2017038615A1
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- Prior art keywords
- adhesive
- film
- secondary battery
- resin
- styrene
- Prior art date
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Abstract
Description
次に、本発明のラミネート用接着剤に用いる酸基又は酸無水物基を有するオレフィン樹脂(A)は、オレフィン系モノマーと、エチレン性不飽和カルボン酸またはエチレン性不飽和カルボン酸無水物との共重合体、或いは、ポリオレフィンへエチレン性不飽和カルボン酸またはエチレン性不飽和カルボン酸無水物をグラフト変性した樹脂が挙げられる。
次に、硬化剤(B)は、酸基又は酸無水物基を有するオレフィン樹脂(A)と反応し架橋させて接着剤自体を硬化させる成分であり、多官能イソシアネート化合物、アジリジン基含有化合物、及びエポキシ化合物、メラミン樹脂などが挙げられる。
ここで使用し得る硬化促進剤は、例えば、リン系化合物、第3級アミン、イミダゾール、有機酸金属塩、ルイス酸、アミン錯塩等が挙げられる。これらのなかでも硬化促進効果に優れる点からイミダゾールが好ましい。
また、上記スチレン樹脂(C)は、融点80〜140℃の範囲にあるものが耐電解液性に優れる点から好ましい。また、その重量平均分子量が800〜3,000の範囲にあるものが金属フィルムへの濡れ性が改善され、フッ酸のブロック効果が一層優れたものとなる点から好ましい。なお、ここで、重量平均分子量は、下記の条件にて測定される値である。
カラム ;東ソー株式会社製 TSK−GUARDCOLUMN SuperHZ−L
+東ソー株式会社製 TSK−GEL SuperHZM−M×4
検出器 ;RI(示差屈折計)
データ処理;東ソー株式会社製 マルチステーションGPC−8020modelII
測定条件 ;カラム温度 40℃
溶媒 テトラヒドロフラン
流速 0.35ml/分
標準 ;単分散ポリスチレン
試料 ;樹脂固形分換算で0.2質量%のテトラヒドロフラン溶液をマイクロフィルターでろ過したもの(100μl)
脂環族系有機溶剤としては、シクロヘキサン、メチルシクロヘキサン等が好ましく、エステル系溶剤としては、酢酸エチル、酢酸ブチル等が好ましく、アルコール系溶剤としては、エタノール、メタノール、n−プロパノール、2−プロパノール(イソプロピルアルコール)、ブタノール、ヘキサノール等が好ましく、中でもブタノール、イソプロピルアルコールが好ましい。配合比率は特に限定はないが、脂環族系有機溶剤が混合溶媒全体量に対し50%を占める量であると、溶解性により優れ好ましい。
例えば、メチルシクロヘキサン/酢酸ブチル/ブタノールや、メチルシクロヘキサンと酢酸エチルとイソプロピルアルコールとの組み合わせが好ましい。
前記混合溶媒は、通常、スチレン系樹脂の他の熱可塑性樹脂は溶解し難いところ、本発明で用いるスチレン樹脂(C)は熱可塑性樹脂でありながら該混合溶媒に良好に溶解する。そのため、前記混合溶媒を使用する場合に、接着剤の塗工性、金属フィルムへの濡れ性が良好なものとなり、フッ酸ブロックの効果が一層良好なものとなる。
本発明のラミネート用接着剤を用い、無延伸ポリオレフィンフィルムと金属フィルムとを貼り合わせることにより、本発明の多層フィルムを得ることができる。
次に、本発明の多層フィルムを用いて二次電池を製造するにあたり、その二次電池の形態としては、多層フィルムをパウチ状に成形し二次電池としたもの、或いは、多層フィルムを深絞り成形又は張り出し成形により外装材を形成して二次電池としたものが挙げられる。
前記した通り、これらのリチウム塩が水分との加水分解反応によりフッ酸を発生し、金属面の腐食や多層フィルムの各層間のラミネート強度の低下を引き起こすことがあったが、本発明ではこのフッ酸を金属面から効果的にブロックさせることができる。
なお、各実施例及び比較例にて使用したスチレン樹脂の重量平均分子量(Mw)は下記の条件にて測定された値である。
カラム ;東ソー株式会社製 TSK−GUARDCOLUMN SuperHZ−L
+東ソー株式会社製 TSK−GEL SuperHZM−M×4
検出器 ;RI(示差屈折計)
データ処理;東ソー株式会社製 マルチステーションGPC−8020modelII
測定条件 ;カラム温度 40℃
溶媒 テトラヒドロフラン
流速 0.35ml/分
標準 ;単分散ポリスチレン
試料 ;樹脂固形分換算で0.2質量%のテトラヒドロフラン溶液をマイクロフィルターでろ過したもの(100μl)
酸基又は酸無水物基を有するオレフィン樹脂(A)として1−プロペンと1−ブテンを含む共重合体に無水マレイン酸をグラフト変性した酸基含有オレフィン樹脂の20質量部と混合溶媒(メチルシクロヘキサン/酢酸ブチル/ブタノール=72/7/1(質量比))の80質量部に溶解させた樹脂溶液(不揮発分20質量%、東洋紡社製「ハードレンNS-2002」)100質量部を主剤として用い、表1又は表2に示すエポキシ化合物の他の成分を混合し良く撹拌して主剤のプレミクスチャーを製造した。次いで、表1又は表2に示すエポキシ化合物を表1又は表2中の配合量で、前記プレミクスチャーに配合して接着剤を調整した後、未表面処理アルミフォイル(東洋アルミニウム社製アルミニウム箔「1N30H」:膜厚30μm)にバーコーターで塗布量5g/m2(dry)で塗布し、80℃−1分間乾燥させた後、未延伸ポリオレフィンフィルム(東レフィルム加工株式会社製「ZK−93KM」膜厚:70μm)と100℃で貼り合せて積層体を作製した。
その後、60℃−5日エージングさせた後に初期接着強度を測定した。
酸基又は酸無水物基を有するオレフィン樹脂(A)として1−プロペンと1−ブテンを含む共重合体にマレイン酸をグラフト変性した酸基含有オレフィン樹脂(GMP7550E)を20質量部と混合溶媒(メチルシクロヘキサン/酢酸エチル/イソプロピルアルコール=72/7/1の混合溶媒)の80質量部に溶解させた樹脂溶液(不揮発分20質量%)100質量部を主剤として用いた以外は実施例4と同様にして接着剤を調整し、該接着剤を用いて積層体を作製した。
(株)エー・アンド・ディー製テンシロン試験において、前記塗工物を15mm幅にカットし、180°剥離強度を測定した。
積層体を電解液「エチレンカーボネート:エチルメチルカーボネート:ジメチルカーボネート=1:1:1(wt%)+LiPF6:1mol+ビニレンカーボネート:1質量%」に85℃−7日間浸漬させ、浸漬前後の接着強度の保持率から以下のとおりに評価を実施した。
○:80%以上
△:60%以上80%未満、
×:60%未満
表1及び表2の配合に従い、主剤と硬化剤、溶剤を配合し良く攪拌して脱泡した後、B型粘度計にて粘度を測定した。サンプル瓶の蓋をしっかりと閉め、40℃の恒温槽に入れ、2時間後、4時間後、6時間後、それぞれの粘度を測定し、粘度の推移を下記の基準にて評価した。
○:初期に対する粘度上昇率が30%未満
△:初期に対する粘度上昇率が30%以上50%未満
×:初期に対する粘度上昇率が50%以上
(熱間強度試験)
(株)エー・アンド・ディー社製テンシロン試験において、前記塗工物を15mm幅にカットし、80℃の恒温槽内で剥離強度を測定した。
GMP7550E:1−プロペンと1−ブテンを含む共重合体にマレイン酸をグラフト変性した酸基含有オレフィン樹脂(不揮発分100質量%)
キュアゾール2E4MZ:イミダゾール(四国化成工業株式会社製「キュアゾール2E4MZ」、不揮発分100%)
デナコールEX-321:エポキシ樹脂(トリメチロールプロパンポリグリシジルエーテル、ナガセケムテックス社製「デナコールEX-321」、不揮発分100質量%)
FTR6100:スチレン系モノマーと重合性脂肪族モノマーとの共重合体(三井化学社製スチレン系樹脂「FTR6100」、重量平均分子量1100、不揮発分100質量%)
FTR2140:スチレンとα−メチルスチレンとの共重合体(三井化学社製「FTR2140」重量平均分子量3200、不揮発分100質量%)
FMR0150:スチレン系モノマーと重合性芳香族モノマーとの共重合体(三井化学社製「FMR0150」、重量平均分子量2000、不揮発分100質量%)
FTR8120:スチレン系モノマーの単独重合体(三井化学社製「FTR8120」、重量平均分子量1500、不揮発分100質量%)
エピクロン860:ビスフェノールA型エポキシ樹脂(DIC株式会社製「エピクロン860」エポキシ当量240g/eq.、不揮発分100質量%)
B:本発明のラミネート用接着剤
C:金属フィルム
D:接着剤層
E:基材フィルム
a:タブリード
b:多層フィルム
c:ヒートシール部
d:電極端子
e:成形体
Claims (12)
- 酸基又は酸無水物基を有するオレフィン樹脂(A)、硬化剤(B)、及びスチレン樹脂(C)を必須成分とするラミネート用接着剤であって、前記スチレン樹脂(C)の配合割合が前記オレフィン樹脂(A)の100質量部に対して0.01〜1.5質量部の範囲であることを特徴とするラミネート用接着剤。
- 前記スチレン樹脂(C)が融点80〜140℃の範囲にある請求項1に記載のラミネート用接着剤。
- 前記スチレン系樹脂(C)が、重量平均分子量800〜3,000の範囲にあるものである請求項1または2に記載のラミネート用接着剤。
- 前記スチレン系樹脂(C)が、スチレン系モノマーの単独重合体、スチレンとα−メチルスチレンとの共重合体、スチレン系モノマーと重合性脂肪族モノマーとの共重合体、またはスチレン系モノマーと重合性芳香族モノマーとの共重合体である請求項1〜3のいずれかに記載のラミネート用接着剤。
- 前記硬化剤(B)が、エポキシ化合物である請求項1〜4のいずれかに記載のラミネート用接着剤。
- 前記酸基又は酸無水物基を有するオレフィン樹脂(A)が、炭素原子数3〜8のオレフィンの単独重合体又は炭素原子数3〜8のオレフィンの2種以上の共重合体に、エチレン性不飽和カルボン酸またはエチレン性不飽和カルボン酸無水物をグラフト変性したものである請求項1〜5のいずれかに記載のラミネート用接着剤。
- 脂環族系有機溶剤とエステル系溶剤とアルコール系溶剤との混合溶媒を含有する請求項1〜6のいずれかに記載のラミネート用接着剤。
- 無延伸ポリオレフィンフィルムと金属フィルムとを請求項1〜7のいずれかに記載の接着剤により接着した積層体を必須のフィルム構成とする多層フィルム。
- 前記金属フィルムの前記接着剤により接着した側とは反対側に更に接着層を介して基材フィルムがラミネートされている請求項8に記載の多層フィルム。
- 前記基材フィルムが二軸延伸ポリエステルフィルム又は二軸延伸ポリアミドフィルムである請求項9に記載の多層フィルム。
- 二次電池本体、該二次電池の正極及び負極にそれぞれ接合するタブリード、電解質溶液、及び前記タブリードを二次電池外部に露出する様に前記二次電池本体と電解質溶液とを封入する外装材とを必須の構成要素とする二次電池であって、
前記外装材が、請求項8〜10のいずれかに記載の多層フィルムを、前記無延伸ポリオレフィンフィルム側がヒートシール部を形成するようにパウチ状の包装袋を構成しているものであることを特徴とする二次電池。 - 請求項8〜10のいずれかに記載の多層フィルムが、深絞り成形又は張り出し成形により無延伸ポリオレフィンフィルム側がシーラント面を構成する様にエンボス状に賦型された形状を有し、2つの該多層フィルムのシーラント面同士が貼合され、かつ、この貼合により形成される内部空隙に二次電池本体と電極端子が配設され、該電極端子は電池外部へ露出されており、かつ、該内部空隙に電解質溶液が液密に充填されている構造を有することを特徴とする二次電池。
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TWI785173B (zh) * | 2017-12-26 | 2022-12-01 | 日商迪愛生股份有限公司 | 接著劑、積層體、電池用包裝材料及電池 |
WO2019171709A1 (ja) * | 2018-03-06 | 2019-09-12 | 東洋紡株式会社 | ポリオレフィン系接着剤組成物 |
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