JP7258000B2 - 樹脂多孔質体の製造方法 - Google Patents
樹脂多孔質体の製造方法 Download PDFInfo
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- JP7258000B2 JP7258000B2 JP2020173668A JP2020173668A JP7258000B2 JP 7258000 B2 JP7258000 B2 JP 7258000B2 JP 2020173668 A JP2020173668 A JP 2020173668A JP 2020173668 A JP2020173668 A JP 2020173668A JP 7258000 B2 JP7258000 B2 JP 7258000B2
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Description
Ra2=4(δD1-δD2)2+(δP1-δP2)2+(δH1-δH2)2
エチレン-ビニルアルコール共重合体(EVOH)は、モノマー単位として、エチレン単位およびビニルアルコール単位を含有する共重合体である。EVOH中のエチレン単位の含有量は、特に制限はないが、好ましくは10モル%以上であり、より好ましくは15モル%以上であり、さらに好ましくは20モル%以上であり、特に好ましくは25モル%以上である。また、EVOH中のエチレン単位の含有量は、好ましくは60モル%以下であり、より好ましくは50モル%以下であり、さらに好ましくは45モル%以下である。EVOHのけん化度は、特に制限はないが、好ましくは80モル%以上であり、より好ましくは90モル%以上であり、さらに好ましくは95モル%以上である。けん化度の上限は、けん化に関する技術的限界により定まり、例えば、99.99モル%である。なお、EVOHのエチレン単位の含有量およびけん化度は、公知方法(例、1H-NMR測定等)により求めることができる。
酢酸セルロースの好適な良溶媒としては、N,N-ジメチルホルムアミド、N,N-ジメチルアセトアミド、N-メチルピロリドン等の含窒素極性溶媒(特に含窒素非プロトン性極性溶媒);蟻酸メチル、酢酸メチル等のエステル類;アセトン、シクロヘキサノン等のケトン類;テトラヒドロフラン、ジオキサン、ジオキソラン等の環状エーテル類;メチルグリコール、メチルグリコールアセテート等のグリコール誘導体;塩化メチレン、クロロホルム、テトラクロロエタン等のハロゲン化炭化水素;炭酸プロピレン等の環状カーボネート類;DMSO等の含硫黄極性溶媒(特に含硫黄非プロトン性極性溶媒)などが挙げられる。なかでも、含硫黄非プロトン性極性溶媒が好ましく、DMSOがより好ましい。
ポリフッ化ビニリデンの好適な良溶媒としては、N,N-ジメチルホルムアミド、N,N-ジメチルアセトアミド、N-メチルピロリドン等の含窒素極性溶媒(特に含窒素非プロトン性極性溶媒);DMSO等の含硫黄極性溶媒(特に含硫黄非プロトン性極性溶媒)などが挙げられる。なかでも、含窒素非プロトン性極性溶媒が好ましく、N,N-ジメチルホルムアミドがより好ましい。
フッ化ビニリデン-ヘキサフルオロプロピレン共重合体(P(VDF-HFP))は、モノマー単位として、フッ化ビニリデン単位およびヘキサフルオロプロピレン単位を含有する共重合体である。これらの単位の共重合割合は特に制限はなく、セパレータの特性に応じて適宜決定すればよい。フッ化ビニリデン-ヘキサフルオロプロピレン共重合体は、公知方法に従い合成して入手することができ、市販品(例、アルケマ社製Kynar FLEX 2850-00、2800-00、2800-20、2750-01、2500-20、3120-50、2851-00、2801-00、2821-00、2751-00、2501-00等)としても入手可能である。
サンプル瓶に酢酸セルロース(Aldrich社製、平均分子量50,000)2.1質量部を秤量した。このサンプル瓶に、良溶媒としてのアセトン10質量部を添加した。サンプル瓶を40℃~50℃に加熱して、酢酸セルロースをアセトンに完全に溶解させた。その後、サンプル瓶に、貧溶媒としての水1.5質量部を添加し、撹拌した。このようにして、溶媒をアセトン/水の混合溶媒とする酢酸セルロース溶液を得た。
乾燥炉内の温度を200℃に変更した以外は、実施例1と同様にして、酢酸セルロースの多孔質膜を作製した。
実施例1で作製した酢酸セルロース溶液を、基材としてのアルミニウム箔上にキャスティングにより塗布した。このとき、塗布厚みは200μmであった。酢酸セルロース溶液が塗布されたアルミニウム箔を、30℃に設定した熱風乾燥機内に入れて、60秒間乾燥を行って、アセトン/水の混合溶媒を除去した。このようにして、アルミニウム箔上に酢酸セルロースの多孔質膜を得た。
実施例1で作製した酢酸セルロース溶液を、基材としてのアルミニウム箔上にキャスティングにより塗布した。このとき、塗布厚みは200μmであった。酢酸セルロース溶液が塗布されたアルミニウム箔を、60℃に設定した熱風乾燥機内に入れて、60秒間乾燥を行って、アセトン/水の混合溶媒を除去した。このようにして、アルミニウム箔上に酢酸セルロースの多孔質膜を得た。
実施例1で作製した酢酸セルロース溶液を、基材としてのアルミニウム箔上にキャスティングにより塗布した。このとき、塗布厚みは200μmであった。酢酸セルロース溶液が塗布されたアルミニウム箔を、表面温度50℃に設定したホットプレート上に置いて、60秒間乾燥を行って、アセトン/水の混合溶媒を除去した。このようにして、アルミニウム箔上に酢酸セルロースの多孔質膜を得た。
サンプル瓶にフッ化ビニリデン-ヘキサフルオロプロピレン共重合体(アルケマ社製「Kynar-FLEX 2821-00」、グレード:パウダータイプ、以下「P(VDF-HFP)」と記す)1.0質量部を秤量した。このサンプル瓶に、良溶媒としてのメチルエチルケトン(MEK)3.2質量部を添加した。サンプル瓶を40℃~50℃に加熱して、P(VDF-HFP)をMEKに完全に溶解させた。その後、サンプル瓶に、貧溶媒としての1,2-プロパンジオール0.4質量部を添加し、撹拌した。このようにして、溶媒をMEK/プロパンジオールの混合溶媒とするP(VDF-HFP)溶液を得た。
乾燥炉内の温度を200℃に設定した以外は、実施例3と同様にして、アルミニウム箔上にP(VDF-HFP)の多孔質膜を得た。
実施例3で作製したP(VDF-HFP)溶液を、基材としてのアルミニウム箔上にキャスティングにより塗布した。このとき、塗布厚みは200μmであった。P(VDF-HFP)溶液が塗布されたアルミニウム箔を、100℃に設定した熱風乾燥機内に導入して、60秒間乾燥を行って、MEK/プロパンジオールの混合溶媒を除去した。このようにして、アルミニウム箔上にP(VDF-HFP)の多孔質膜を得た。
実施例3で作製したP(VDF-HFP)溶液を、基材としてのアルミニウム箔上にキャスティングにより塗布した。このとき、塗布厚みは200μmであった。P(VDF-HFP)溶液が塗布されたアルミニウム箔を、表面温度80℃に設定したホットプレート上に置いて、60秒間乾燥を行って、MEK/プロパンジオールの混合溶媒を除去した。このようにして、アルミニウム箔上にP(VDF-HFP)の多孔質膜を得た。
各実施例および各比較例で得られた多孔質膜の表面にエタノールを滴下して、エタノールが多孔質膜の裏面まで浸透したか否かを目視で評価した。結果を表1に示す。エタノールが多孔質膜の裏面まで浸透する場合には、スキン層がなく全体が多孔質化されていると判断できる。一方、エタノールが浸透しない場合は、多孔質膜の表層部にスキン層が形成されていると判断できる。
比較例1および実施例1,3で得られた多孔質膜の表面を、走査型電子顕微鏡(SEM)にて観察した。比較例1および実施例1,3で得られた多孔質膜の表面のSEM写真を、それぞれ図3~5に示す。
20 過熱水蒸気導入管
30 第1バルブ
40 熱交換器
50 制御盤
60 水蒸気導入管
70 第2バルブ
80 ボイラー
Claims (5)
- 非水溶性高分子の良溶媒および前記非水溶性高分子の貧溶媒を含有する混合溶媒に、前記非水溶性高分子が溶解した溶液を調製する工程と、
前記溶液を乾燥して前記混合溶媒を除去する工程と、
を包含し、
前記貧溶媒の沸点が、前記良溶媒の沸点よりも高く、
前記溶液の乾燥を、過熱水蒸気を用いて行う、
樹脂多孔質体の製造方法。 - 前記溶液を調製する工程の後であって前記溶液を乾燥する工程の前に、基材の表面上に前記調製した非水溶性高分子の溶液を薄膜状に塗工する工程をさらに包含する、請求項1に記載の製造方法。
- 前記基材が、二次電池の電極である、請求項2に記載の製造方法。
- 前記非水溶性高分子が、エチレン-ビニルアルコール共重合体、またはフッ化ビニリデン-ヘキサフルオロプロピレン共重合体である、請求項1~3のいずれか1項に記載の製造方法。
- 前記溶液の乾燥を、140℃以上の温度で過熱水蒸気を用いて行う、請求項1~4のいずれか1項に記載の製造方法。
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