JP7102678B2 - フッ素系樹脂多孔性膜およびその製造方法 - Google Patents
フッ素系樹脂多孔性膜およびその製造方法 Download PDFInfo
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Description
本出願は、2018年10月18日付韓国特許出願第10-2018-0124560号および2019年10月17日付韓国特許出願第10-2019-0129384号に基づいた優先権の利益を主張し、当該韓国特許出願の文献に開示された全ての内容は本明細書の一部として組み含まれる。
複数個のフッ素系樹脂フィブリルを含み、
前記フッ素系樹脂多孔性膜表面から膜全体厚さの10%以内の表面領域を除いたフッ素系樹脂多孔性膜の内部領域に存在するフィブリルの平均太さに対する、前記フッ素系樹脂多孔性膜の表面領域に存在するフィブリルの平均太さの比(表面領域に存在するフィブリルの平均太さ/膜内部領域に存在するフィブリルの平均太さ)が1.8から3である。
[数式1]
気孔度(%)={1-(重量[g]/(厚さ[cm]×面積[cm2]×真密度[g/cm3]))}×100
[数式2]
PTFE樹脂(登録商標650J、MCF社製、SSG(JIS K6892で測定):2.163)100重量部に対して潤滑剤(登録商標Isopar H、Exxon社製)22重量部を混合してフッ素系樹脂包含組成物を製造した後、50℃で24時間熟成した。次に、2MPaの圧力を加えて予備成形体ブロック(preform block)を製造し、ダイが備えられたペースト(paste)押出装備を利用して1mm厚さのシート形態に押出した後、カレンダリング(Calendering)を通じて300μm厚さに圧延してPTFEフィルムを製造した。製造したPTFEフィルムを200℃の加熱オーブンでロールツーロール(Roll to Roll)工程で熱処理して前記潤滑剤を完全に除去した。
下記表1に開示された条件を行うことを除き、前記実施例1と同様な方法で行ってPTFE多孔性膜を製造した。
前記実施例1で押出時、ロッド(rod)形態に押出し、下記表1に開示された条件で熱固定工程を行うことを除き、前記実施例1と同様な方法で行ってPTFE多孔性膜を製造した。
フッ素系樹脂多孔性膜表面でのフィブリルの太さと膜内部領域に存在するフィブリルの太さ比が3を超える場合、効果比較のために、熱固定工程を400℃の高温で行い、フッ素系樹脂多孔性膜を製造しようとした。
前記実施例1および2で製造したPTFE多孔性膜の表面および内部をそれぞれ走査電子顕微鏡(SEM)で観察し、その結果を図1a~図2bに示した。
前記実施例および比較例で製造したPTFE多孔性膜を下記の方法で評価し、その結果を下記表2および図3~5に示した。
[数式1]
気孔度(%)={1-(重量[g]/(厚さ[cm]×面積[cm2]×真密度[g/cm3]))}×100
[数式2]
Claims (11)
- 複数個のフッ素系樹脂フィブリルを含むフッ素系樹脂多孔性膜であって、
前記フッ素系樹脂多孔性膜は厚さが20から50μmであり、
前記フッ素系樹脂多孔性膜の内部領域でのフィブリルの平均太さに対する、表面領域に存在するフィブリルの平均太さの比が1.8から3であり、
前記表面領域は、前記フッ素系樹脂多孔性膜の表面から膜全体厚さの10%以内の領域であり、前記内部領域は、前記表面領域を除いた領域であり、
前記フッ素系樹脂多孔性膜は、120℃で30分間熱処理した後に変化した横方向長さ値と、前記熱処理前の横方向長さ値とを利用して下記数式2により計算した熱収縮率が10%以下であり、
ASTM D 882により測定した縦方向の引張強度が60から100MPaであり、横方向の引張強度が70から120MPaである、フッ素系樹脂多孔性膜。
[数式2]
- 前記表面領域でのフィブリルの平均太さが50から140nmであり、前記内部領域でのフィブリルの平均太さが40から70nmである、請求項1に記載のフッ素系樹脂多孔性膜。
- 前記内部領域は、フッ素系樹脂多孔性膜のある一面から膜全体厚さの10%超過90%未満の領域に該当する、請求項1または2に記載のフッ素系樹脂多孔性膜。
- 前記フッ素系樹脂多孔性膜内に含まれる気孔の平均気孔直径が0.1から0.25μmであり、最大気孔直径が0.3から0.45μmである、請求項1から3のいずれか一項に記載のフッ素系樹脂多孔性膜。
- 前記フッ素系樹脂多孔性膜の気孔度が70から90%である、請求項1から4のいずれか一項に記載のフッ素系樹脂多孔性膜。
- 前記フッ素系樹脂多孔性膜は厚さが30から50μmである、請求項1から5のいずれか一項に記載のフッ素系樹脂多孔性膜。
- 前記フッ素系樹脂多孔性膜は、ポリテトラフルオロエチレン、テトラフルオロエチレン-ペルフルオロアルキルビニルエーテル共重合体、テトラフルオロエチレン-ヘキサフルオロプロピレン共重合体、エチレン-テトラフルオロエチレンコポリマー樹脂、テトラフルオロエチレン-クロロトリフルオロエチレン共重合体、またはエチレン-クロロトリフルオロエチレン樹脂を含む、請求項1から6のいずれか一項に記載のフッ素系樹脂多孔性膜。
- 前記フッ素系樹脂多孔性膜は、JIS K6892を利用して測定した標準比重が2.14から2.22であるポリテトラフルオロエチレンを含む、請求項1から7のいずれか一項に記載のフッ素系樹脂多孔性膜。
- フッ素系樹脂と潤滑剤を混合して製造したフッ素系樹脂組成物をシート状に押出してフッ素系樹脂シートを製造する段階;
前記フッ素系樹脂シートを200から340℃の温度で1から12倍縦方向延伸する段階;および
前記縦方向延伸されたシートを200から320℃で5から25倍横方向延伸した後、370から390℃の温度で5秒から20秒間熱固定する段階を含む、請求項1から8のいずれか一項に記載のフッ素系樹脂多孔性膜の製造方法。 - 前記フッ素系樹脂シートの製造は、JIS K6892を利用して測定した標準比重が2.14から2.22であるフッ素系樹脂および潤滑剤を混合して製造したフッ素系樹脂組成物を加圧して予備成形体を形成し、前記予備成形体をダイを利用してシート状に押出した後に圧延し、120から200℃で熱処理することによって行われる、請求項9に記載のフッ素系樹脂多孔性膜の製造方法。
- 請求項1から8のいずれか一項に記載のフッ素系樹脂多孔性膜を含むフィルター。
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