JP2020182930A - 架橋ポリオレフィン分離膜およびその製造方法 - Google Patents
架橋ポリオレフィン分離膜およびその製造方法 Download PDFInfo
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- JP2020182930A JP2020182930A JP2019232633A JP2019232633A JP2020182930A JP 2020182930 A JP2020182930 A JP 2020182930A JP 2019232633 A JP2019232633 A JP 2019232633A JP 2019232633 A JP2019232633 A JP 2019232633A JP 2020182930 A JP2020182930 A JP 2020182930A
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- separation membrane
- polyolefin
- weight
- photoreactive substance
- porous
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- Granted
Links
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- 125000003187 heptyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
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- 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
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- 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
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- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
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- Polymers & Plastics (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Cell Separators (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
Description
(i)メルトダウン温度170℃以上、(ii)縦方向(MD)引張強度700〜3,000kgf/cm2、(iii)横方向(TD)引張強度700〜3,000kgf/cm2、(iv)縦方向(MD)引張伸率30〜150%、および(v)横方向(TD)引張伸率30〜150%。
重量平均分子量Mwが350,000であり、分子量分布Mw/Mnが5である高密度ポリエチレン(HDPE)30重量部および40℃での動粘度が70cStであるパラフィンオイル70重量部を混合して、2軸押出機(内径58mm,L/D=56)に投入した。スクリュー回転速度40rpm、200℃の条件で前記2軸押出機で幅が300mmのT−ダイ(T−Die)で吐出させた後、温度が40℃のキャストロール(casting roll)を通過させて、厚みが800μmのベースシートを製造した。
溶融指数3.0g/10minのポリプロピレン100重量部に光開始剤であるベンゾフェノン0.05重量部、連結剤であるジビニルベンゼン2重量部を2軸押出機を利用して混練し、ペレットを製粒し、T−ダイが付着した1軸押出機で押出して、前駆体フィルムを製造し、155℃のコンベクションオーブン(convection oven)で熱処理後、これを縦方向(MD)1軸延伸機で常温で20%、150℃で100%延伸し、150℃で20%弛緩して熱固定した。これを通じて得られた多孔性フィルムに6,000Wの紫外線ランプ(lmax〜250nm)で10秒間露光して、多孔性分離膜を製造した。
ポリプロピレンを溶融指数1g/10minの高密度ポリエチレンに代え、コンベクションオーブンで熱処理を125℃で、延伸および熱固定温度を120℃で実施したことを除いて、前記比較例2と同じ方法で多孔性分離膜を製造した。
ベンゾフェノンをベンジルジメチルケタル(benzildimethylketal)に代え、ジビニルベンゼンをビスフェノール−Aエポキシジアクリレート(bisphenol−A epoxydiacrylate)に代えたことを除いて、前記比較例2と同じ方法で多孔性分離膜を製造した。
高密度ポリエチレンを溶融指数3.0g/10minのポリプロピレンに代え、連結剤を使用せず、コンベクションオーブンで熱処理を155℃で、延伸および熱固定温度を150℃で実施したことを除いて、前記比較例3と同じ方法で多孔性分離膜を製造した。
重量平均分子量Mwが350,000であり、分子量分布Mw/Mnが5である高密度ポリエチレン29.5重量部、シラン変性高密度ポリエチレン0.5重量部、および40℃での動粘度が70cStであるパラフィンオイル70重量部を混合して、2軸押出機(内径58mm,L/D=56)に投入した。架橋触媒であるジブチルスズジラウレートを前記パラフィンオイルのうち一部に予め分散させ、前記2軸押出機を通過する物質の総重量を基準として0.5重量%になるように前記2軸押出機のサイドインジェクターを通じて投入した。スクリュー回転速度40rpm、200℃の条件で前記2軸押出機で幅が300mmのT−ダイで吐出させた後、温度が40℃のキャストロールを通過させて、厚みが800μmのベースシートを製造した。
含浸槽に担持されたジクロロメタン溶液のうちベンゾフェノンの濃度を0.005重量%に変更したことを除いて、前記実施例1と同じ方法で多孔性分離膜を製造した。
溶融温度が135℃であり、重量平均分子量が350,000である高密度ポリエチレン35重量部、40℃での動粘度が70cStであるパラフィンオイル65重量部、トリメトキシビニルシラン2重量部、ジブチルスズジラウレート2重量部および2,5−ジメチル−2,5−ジ(tert−ブチルペルオキシ)ヘキサン(2,5−dimethyl−2,5−di(tert−butylperoxy)hexane)0.04重量部を混合して、2軸押出機(内径58mm、L/D=56)に投入した。200℃、スクリュー回転速度30rpmの条件で前記2軸押出機で反応押出させて、シラン変性ポリオレフィン組成物を製造し、幅が300mmのTダイで吐出後、温度が40℃のキャストロールを通過させて、厚みが800μmのベースシートを製造した。前記ベースシートを108℃のロール延伸機で縦方向(MD)5.5倍延伸し、123℃のテンター延伸機で横方向(TD)に5.5倍延伸して、延伸フィルムを製造した。前記延伸フィルムを25℃のジクロロメタン浸出槽に含浸して、10分間パラフィンオイルを抽出、除去した。パラフィンオイルが除去されたフィルムを127℃に熱固定して、多孔性分離膜を製造した。前記分離膜を80℃、湿度90%の恒温恒湿槽で24時間の間架橋させて、多孔性分離膜を製造した。
本発明で測定した物性それぞれに対する試験方法は、下記の通りである。温度に対する別途の言及がない場合、常温(25℃)で測定した。
−気孔率(%):ASTM F316−03に基づいて、PMI社のCapillary Porometerを使用して半径が25mmの分離膜試験片の気孔率を測定した。
−引張強度(kgf/cm2):引張強度測定機を利用してサイズが20×200mmの分離膜試験片に応力を加えて試験片の破断が発生するまで加えられた応力を測定した。
−引張伸率(%):引張強度測定機を利用してサイズが20×200mmの分離膜試験片に応力を加えて試験片の破断が発生するまで伸びた最大長さを測定し、下記計算式を使用して引張伸率を計算した。
引張伸率(%)=(l1−l2)/l1*100
(前記計算式で、l1は、伸長前の試験片の横または縦方向の長さであり、l2は、破断直前の試験片の横または縦方向の長さである。)
−穿孔強度(gf):KATO TECH社の穿孔強度測定機KES−G5モデルを利用してサイズが100×50mmの分離膜試験片に直径0.5mmのスティック(Stick)で0.05cm/secの速度で力を加えて前記試験片が穿孔される時点に加えられた力を測定した。
−メルトダウン温度(℃):熱機械分析装置(Thermomechanical analysis,TMA)を利用して分離膜試験片に0.01Nの力を加えた後、5℃/分の速度で昇温させて、前記試験片の変形程度を測定した。前記試験片が破断される温度をメルトダウン温度とした。
−熱収縮率(%):120℃のオーブンで1時間の間サイズが200×200mmの分離膜試験片をA4紙の間に入れて放置した後、常温冷却させて、試験片の横および縦方向の収縮した長さを測定し、下記計算式を使用して熱収縮率を計算した。
熱収縮率(%)=(l3−l4)/l3*100
(前記計算式で、l3は、収縮前の試験片の横または縦方向の長さであり、l4は、収縮後の試験片の横または縦方向の長さである。)
フレーム(外郭:15cm×15cm、内径:10cm×10cm)に実施例1、比較例1および比較例6で製造された分離膜をポリイミドテープで固定させた後、80℃から始まって3℃/分の昇温速度でコンベクションオーブン(convection oven)に露出させた。
本発明の範囲は、後述する請求範囲によって示され、請求範囲の意味および範囲そしてその均等概念から導き出されるすべての変更または変形された形態が本発明の範囲に含まれるものと解すべきである。
Claims (10)
- ポリオレフィンを含むフィブリル(fibril)と、光反応性物質により前記フィブリルの表面に形成された第1ラジカル、および前記光反応性物質に形成された第2ラジカルのうち少なくとも一部が反応して生成された結合構造とを含む分離膜。
- 前記ポリオレフィンの重量平均分子量Mwが250,000〜800,000であり、分子量分布Mw/Mnが3〜7である、請求項1に記載の分離膜。
- 前記ポリオレフィンは、ポリエチレン、ポリプロピレン、ポリブチレン、ポリメチルペンテン、エチレンビニルアセテート、エチレンブチルアクリレート、エチレンエチルアクリレートおよびこれらのうち2以上の組合せまたは共重合体よりなる群から選ばれる一つである、請求項1に記載の分離膜。
- 前記光反応性物質は、水素置換型光開始剤である、請求項1に記載の分離膜。
- 前記水素置換型光開始剤は、ベンゾフェノン(Benzophenone)系、カンファーキノン(camphorquinone)系、アントラキノン(anthraquinone)系、チオキサントン(thiozanthone)系、アルファヒドロキシケトン(α−hydroxyketone)系、ビスアシルホスフィンオキシド系、アルファアミノケトン(α−aminoketone)系、フェニルグリオキシラート(phenylglyoxylate)系、モノアシルホスフィンオキシド(monoacylphosphinoxide)系、ベンジルジメチルケタル(benzildimethylketal)系またはこれらの置換体や誘導体およびこれらのうち2以上の組合せよりなる群から選ばれる一つである、請求項4に記載の分離膜。
- 前記結合構造は、ジビニルベンゼン、ビスフェノール−Aジメタクリレート、ビスフェノール−Aエポキシジアクリレート、トリアリルシアヌレート、トリアリルイソシアヌレート、ペンタエリスリトールトリアリルエーテル、ブタンジオールジアクリレート、エチレングリコールジアクリレートおよびこれらのうち2以上の組合せよりなる群から選ばれる一つの連結剤をさらに含む、請求項1に記載の分離膜。
- 前記分離膜のうち前記結合構造の含量は、0.001〜10重量%である、請求項1に記載の分離膜。
- 前記分離膜は、下記(i)〜(v)の条件のうち一つ以上を満たす、請求項1に記載の分離膜。
(i)メルトダウン温度170〜350℃
(ii)縦方向(MD)引張強度700〜3,000kgf/cm2
(iii)横方向(TD)引張強度700〜3,000kgf/cm2
(iv)縦方向(MD)引張伸率30〜150%
(v)横方向(TD)引張伸率30〜150% - 請求項1〜8のいずれかに記載の分離膜を含む電気化学素子。
- (a)ポリオレフィンおよび気孔形成剤を含む組成物を押出機に投入し、シート形態に成形および延伸する段階、
(b)前記延伸したシートから気孔形成剤を抽出して、多孔膜を製造する段階、
(c)前記多孔膜に光反応性物質を含む溶液を塗布したり含浸させる段階、および
(d)前記多孔膜に光を照射して、前記光反応性物質により形成された第1ラジカルおよび前記光反応性物質に形成された第2ラジカルのうち少なくとも一部を反応させて結合構造を生成させる段階、を含む分離膜の製造方法。
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CN103421208A (zh) * | 2013-05-23 | 2013-12-04 | 浙江大学 | 一种辐照交联锂离子电池隔膜及其制备方法 |
WO2018095094A1 (zh) * | 2016-11-25 | 2018-05-31 | 上海恩捷新材料科技股份有限公司 | 一种电池隔离膜的制备方法 |
CN108192116A (zh) * | 2017-12-29 | 2018-06-22 | 上海恩捷新材料科技股份有限公司 | 一种光引发交联聚合物隔离膜及其制备方法 |
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CN111864159A (zh) | 2020-10-30 |
US11557814B2 (en) | 2023-01-17 |
US20200343506A1 (en) | 2020-10-29 |
EP3731305A1 (en) | 2020-10-28 |
JP7398728B2 (ja) | 2023-12-15 |
KR102181119B1 (ko) | 2020-11-23 |
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