JP6773630B2 - 二軸配向細孔性膜、合成物、ならびに製造および使用の方法 - Google Patents
二軸配向細孔性膜、合成物、ならびに製造および使用の方法 Download PDFInfo
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- JP6773630B2 JP6773630B2 JP2017225491A JP2017225491A JP6773630B2 JP 6773630 B2 JP6773630 B2 JP 6773630B2 JP 2017225491 A JP2017225491 A JP 2017225491A JP 2017225491 A JP2017225491 A JP 2017225491A JP 6773630 B2 JP6773630 B2 JP 6773630B2
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- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
- 229920002397 thermoplastic olefin Polymers 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 150000004684 trihydrates Chemical class 0.000 description 1
- 238000010407 vacuum cleaning Methods 0.000 description 1
- PXXNTAGJWPJAGM-UHFFFAOYSA-N vertaline Natural products C1C2C=3C=C(OC)C(OC)=CC=3OC(C=C3)=CC=C3CCC(=O)OC1CC1N2CCCC1 PXXNTAGJWPJAGM-UHFFFAOYSA-N 0.000 description 1
- 230000002747 voluntary effect Effects 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
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- B29C55/02—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets
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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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Landscapes
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- Health & Medical Sciences (AREA)
- Polymers & Plastics (AREA)
- Medicinal Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Dispersion Chemistry (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Materials Engineering (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
- Laminated Bodies (AREA)
- Cell Separators (AREA)
- Shaping By String And By Release Of Stress In Plastics And The Like (AREA)
- Molding Of Porous Articles (AREA)
Description
本出願は、2011年3月10日に出願された係属中の米国特許出願通し番号第13/044,708号の恩恵およびそれに対する優先権を主張し、かつ、2010年3月12日に出願された米国仮特許出願通し番号第61/313,152号の恩恵およびそれに対する優先権を主張する。
本発明は、二軸配向細孔性膜、二軸配向細孔性膜を含む合成物、二軸配向微細孔性膜、二軸配向大細孔性膜、電池分離体、濾過媒体、湿度制御媒体、平薄板膜、液体保持媒体、および同様のもの、関連する方法、製造方法、使用方法、および同様のものを対象にする。
微細孔性重合体膜が既知であり、様々な工程により作ることができ、それにより膜が作られる工程は、膜の物理的特質に重大な影響を及ぼすことがある。例えば、ケスティング,ロバート・E.、合成重合膜、構造上の視点、第2版、ジョン・ワイリー&サンズ、ニューヨーク州、ニューヨーク、(1985年)(Kesting, Robert E., Synthetic Polymeric Membranes, A Structural Perspective, Second Edition, John Wiley & Sons, New York, NY, (1985))を参照されたい。微細孔性重合体膜を作るための3つの異なる既知の工程としては、乾燥伸長工程(CELGARD工程としても知られている)、湿潤工程、および粒子伸長工程が挙げられる。
本発明の少なくとも選択されている細孔性の材料、薄膜、層、膜、積層物、共押出成形、または合成物の実施形態に従い、いくつかの改良領域は、スリット以外の細孔形状、丸形状の細孔、増加した横方向の引張強さ、MDおよびTDの物理的特性の平衡、例えば、湿気輸送および水頭圧に関連する高性能、低減したガーリー、平衡した物理的特性を伴う高細孔性、細孔径および細孔径分布を含む細孔構造の均一性、増強された耐久性、他の細孔性材料とのそのような膜の合成物、そのような膜の合成物または積層物、細孔性不織材を有する薄膜または層、被覆膜、共押出成形膜、積層膜、所望の湿気輸送(または湿蒸気輸送)、水頭性能、および物理的強さの特性を有する膜、望ましい膜特長の損失を伴わないより物理的に有害な環境内における有用性、巨視物理的特性と組み合わされる膜湿気輸送性能の組み合わせ、疎水性で、非常に透過性があり、化学的および力学的に安定していること、高い引張強さを有すること、それらの組み合わせ、および/または同様のものを含むことがある。
1.HVAC:
a.液体乾燥剤(LD)空気調節(温度および湿度の制御)
b.水系空気調節(温度および湿度の制御)
c.エネルギー回収換気(ERV)
2.脱塩:蒸気脱塩用途
3.燃料電池:加湿ユニット
4.液体および/または空気の濾過:濾過器
典型:
0.75乃至1.50の範囲内のMD/TD縦横比
好適:
0.75乃至1.25の範囲内のMD/TD縦横比
最好適:
0.85乃至1.25の範囲内のMD/TD縦横比
機械方向MD(長さ)および横方向TD(幅)の縦横比範囲に対する典型的な数:
0.75乃至1.50の範囲内のMD/TD縦横比
例えば:
典型:
0.75乃至1.50の範囲内のMD/TD縦横比
0.50乃至7.50の範囲内のMD/ND寸法比
0.50乃至5.00の範囲内のTD/ND寸法比
好適:
0.75乃至1.25の範囲内のMD/TD縦横比
1.0乃至2.5の範囲内のMD/ND寸法比
1.0乃至2.5の範囲内のTD/ND寸法比
最好適:
0.85乃至1.25の範囲内のMD/TD縦横比
1.0乃至2.0の範囲内のMD/ND寸法比
1.0乃至2.0の範囲内のTD/ND寸法比
機械方向MD(長さ)、横方向TD(幅)、および厚さ方向ND(垂直高さ)の球形度の因数または比の範囲に対する典型的な数:
0.75乃至1.50の範囲内のMD/TD縦横比
0.50乃至7.50の範囲内のMD/ND寸法比
0.50乃至5.00の範囲内のTD/ND寸法比
本発明の様々な態様または実施形態を例解する目的のために、目下例示的である形態が図面内に示されているが、本発明が、示されている実施形態、正確な配列または手段に限定されないことが理解される。
本発明の少なくとも選択されている実施形態に従い、微細孔性膜は好適な修正された乾燥伸長工程(二軸配向工程)により作られ、かつ、実質的に丸形状の細孔と、0.5乃至6.0、好ましくは0.5乃至5.0、最も好ましくは0.5乃至4.0の範囲内にある横方向の引張強さに対する機械方向の引張強さの比と、を有する。微細孔性膜等の細孔性膜は、そこを通じて複数の細孔を有する、薄く、しなやかで、重合体の薄板、箔、または薄膜である。そのような膜は、単一重ねまたは多重ね、単一または多重の層、合成物、積層物、および同様のものであってよく、かつ、質量転移膜、圧力調整器、濾過膜、医療機器、電気化学的貯蔵機器用の分離体、燃料電池における使用のための膜、および/または同様のものを含むが、それらに限定されない多種多様な用途において用いることができる。
他に記載されていない限り、本明細書で報告されている試験値、厚さ、細孔性、引張強さ、および縦横比を、以下のように決定した:厚さ−Emveco Microgage 210−Aのマイクロメータを用いるASTM−D374、細孔性−ASTM D−2873、引張強さ−Instron Model 4201を用いるASTM D−882、および縦横比−SEM顕微鏡写真から得た測定値。
−単層PPの空気濾過膜に対して、≦2.5乃至〜25の好適なJISガーリー。
−単層PPのHEPA/ULPA膜に対して、≦0.5乃至〜5の好適なJISガーリー。
−膜の全域にわたる好適な丸い細孔構造および非常に均一の細孔構造。
乾燥工程により作られ、全く油/溶媒が添加されない。
高い細孔率:40−90%
非常に疎水性。
>140psiの水頭圧、>80psiの水侵入圧。
毛細管流動の細孔測定法/アクアポア試験/SEMを特徴とするような独特の細孔構造:少なくとも約0.04の毛細管流動により測定される平均流動細孔径、狭い範囲の細孔径を有する、均一で、丸く、または非スリット型の細孔構造。少なくとも約0.07ミクロンのアクアポアサイズ。高い気体/空気/湿気の透過性:1.0乃至100のJISガーリー、毛細管流動細孔測定法を特徴とするような高い流速、≧8,000g/m2−日のWVTR。
平衡したMD/TD強度:TD強度(>300kg/cm2)。
低いTD収縮率:≦2%の90℃におけるTD収縮率。
好適なPP重合体:MFI=0.1乃至10.0、>45%の重合体の結晶度。
好適なPE重合体:MFI=0.01乃至5.0、>50%の結晶度。
ASTM D−1238法で試験されるMFI。
試験条件:95%の頂部セルの湿度、5%の底部セルの湿度、90%の湿気勾配。
周囲温度。
JISガーリーを、OHKENの透過性試験器を用いることにより、気体透過性試験で測定する。
JISガーリーを、100ccの空気が4.8インチ(12.2cm)の水の低圧にて1平方インチ(6.45cm2)の薄膜を通過するのに必要とされる、秒における時間と定義する。
細孔率を、ASTM D2873という方法により測定する。
穿刺強さを、ASTM D3763に基づいてInstron Model 4442を用いて測定する。その測定を、その膜の幅の全域にわたり行って、平均化した穿刺エネルギー(穿刺強さ)を、試験試料を穿刺するのに必要とされる力と定義する。
引張特性を、Instron Model 4201を用いるASTM−882基準を用いて試験する。
収縮率を、修正したASTM−2732−96の手順を用いて、90℃にて60分にわたり測定する。
水頭圧を、ASTM D3393−91に基づいて測定した。
水侵入を、ASTM F316−93(湿潤流体−水、68.8ダイン/cm。気体:空気。)により試験した。
1.HVAC:
2.液体乾燥剤(LD)空気調節
3.水系空気調節
4.エネルギー回収換気(ERV)
5.脱塩
6.RO脱塩
7.蒸気脱塩
8.燃料電池
9.液体および/または空気の濾過
液体および空気の濾過の場合には特に、独特の細孔構造は、いくつかの明確な恩恵を有することがある。
高効率の空気濾過、
HEPA/ULPA用途、
近零放出の塵除去用途(清浄室、真空袋、覆面、手術着、塵袋、カートリッジ)、
濾過用途:
○高効率のHVAC濾過器媒体
○HEPA/ULPA媒体
○濾過膜合成物
液体濾過、
防護衣服、
機能性衣服/演技スポーツ用着用物、
医療用布、
および同様のもの。
1.HVAC:
a.液体乾燥剤(LD)空気調節(温度および湿度の制御):膜に基づくLDシステムでは、細孔性膜を通じて水蒸気を吸収または放出する塩溶液により、温度および湿度を制御することができる。熱がそのシステム内における原動力である(ほとんどの空気調節システムでのように、圧力ではない)。そのシステムを機能させるためには、水蒸気を容易に通す(液体を引き留めるための)疎水性膜を有することが必要であることがある。
b.水系空気調節(温度および湿度の制御):蒸発式の冷却システムまたは冷却水システムは、LDシステムとはいくらか異なる原理で動作するが、その膜の同じ本質的な特性を用いることになるだろう。
c.エネルギー回収換気(ERV):最も単純なHVAC用途は、補給空気および排気の間における熱および湿気の交換の主要な構成部としてその膜を用いる。
2.脱塩:蒸気脱塩用途は、HVACと同じ膜の特性を用いる。その膜が液体塩水を引き留めるが水蒸気を通すので、塩水および真水を膜により分離させるシステムを構築することができる。より高温圧での塩水をもって、真水はその塩水から放出し、その膜を通じて移動し、凝縮して真水流を形成する。
3.燃料電池:燃料電池では、陽子交換膜(PEM)が継続的に加湿されたままでなければならない。これを、膜に基づく加湿ユニットの使用をもって達成することができる。
4.液体および/または空気の濾過:これらの実施形態では、細孔性膜は単純な濾過器として作用することがある。液体、蒸気、気体、または空気がその膜を通過する際に、細孔を通過するには大きすぎる粒子が膜表面にて遮断される。
典型:
0.75乃至1.50の範囲内のMD/TD縦横比
好適:
0.75乃至1.25の範囲内のMD/TD縦横比
最好適:
0.85乃至1.25の範囲内のMD/TD縦横比
ここに、機械方向MD(長さ)および横方向TD(幅)の縦横比範囲に対する典型的な数がある:
0.75乃至1.50の範囲内のMD/TD縦横比
例えば:
典型:
0.75乃至1.50の範囲内のMD/TD縦横比
0.50乃至7.50の範囲内のMD/ND寸法比
0.50乃至5.00の範囲内のTD/ND寸法比
好適:
0.75乃至1.25の範囲内のMD/TD縦横比
1.0乃至2.5の範囲内のMD/ND寸法比
1.0乃至2.5の範囲内のTD/ND寸法比
最好適:
0.85乃至1.25の範囲内のMD/TD縦横比
1.0乃至2.0の範囲内のMD/ND寸法比
1.0乃至2.0の範囲内のTD/ND寸法比
ここに、機械方向MD(長さ)、横方向TD(幅)、および厚さ方向ND(垂直高さ)の球形度の因数または比の範囲に対する典型的な数がある:
0.75乃至1.50の範囲内のMD/TD縦横比
0.50乃至7.50の範囲内のMD/ND寸法比
0.50乃至5.00の範囲内のTD/ND寸法比
重合体を少なくとも単一層の非細孔性前駆体に押出成形するステップと、
前記非細孔性前駆体を二軸伸長するステップであって、前記二軸伸長が機械方向の伸長および横方向の伸長を含み、前記横方向の伸長が同時制御される機械方向の弛緩を含む、ステップと、を含む乾燥伸長工程により作られ、
かつ、実質的に丸形状の細孔、約40%乃至90%の細孔率、約0.5乃至5.0の範囲内にある横方向の引張強さに対する機械方向の引張強さの比、約100未満のガーリー、少なくとも約0.04ミクロンの平均流動細孔径、少なくとも約0.07ミクロンのアクアポアサイズ、および約140psiよりも大きい水頭圧を有する、細孔性重合体薄膜の少なくとも1つの層、
を備える、膜。
前記二軸伸長より前に細孔性中間体を形成するための機械方向の伸長のステップ、
をさらに含む、上記の膜。
同時制御される機械方向の弛緩を伴う前記横方向の伸長、同時の機械方向の伸長を伴う第2の横方向の伸長、その後の横方向の弛緩を含む、機械方向の伸長その後の前記二軸伸長のステップ、
を含む、上記の膜。
重合体を少なくとも単一層の非細孔性前駆体に押出成形するステップと、
前記非細孔性前駆体を二軸伸長するステップであって、前記二軸伸長が機械方向の伸長および横方向の伸長を含み、前記横方向の伸長が同時制御される機械方向の弛緩を含む、ステップと、を含む乾燥伸長工程により作られ、
かつ、実質的に丸形状の細孔、約40%乃至70%の細孔率、約0.5乃至5.0の範囲内にある横方向の引張強さに対する機械方向の引張強さの比、約300未満のガーリー、少なくとも約0.01ミクロンの平均流動細孔径、および少なくとも約0.04ミクロンのアクアポアサイズを有する、細孔性重合体薄膜の少なくとも1つの層、
を備える、電池分離体。
重合体を少なくとも単一層の非細孔性前駆体に押出成形するステップと、
前記非細孔性前駆体を二軸伸長するステップであって、前記二軸伸長が機械方向の伸長および横方向の伸長を含み、前記横方向の伸長が同時制御される機械方向の弛緩を含む、ステップと、を含む乾燥伸長工程により作られ、
かつ、実質的に丸形状の細孔、少なくとも約40%の細孔率、約0.5乃至5.0の範囲内にある横方向の引張強さに対する機械方向の引張強さの比、約300未満のガーリー、少なくとも約0.01ミクロンの平均流動細孔径、および少なくとも約0.04ミクロンのアクアポアサイズを有する、細孔性重合体薄膜の少なくとも1つの層、
を備える、膜。
重合体を非細孔性前駆体に押出成形するステップと、
前記非細孔性前駆体を二軸伸長するステップであって、前記二軸伸長が機械方向の伸長および横方向の伸長を含み、前記横方向が同時制御される機械方向の弛緩を含む、ステップと、
を備える、方法。
をさらに備える、上記の方法。
機械方向の伸長のステップと、
その後、同時の機械方向の弛緩を含む横方向の伸長のステップと、
を備える、上記の方法。
乾燥伸長工程により作られ、かつ、実質的に丸形状の細孔および0.5乃至6.0の範囲内にある横方向の引張強さに対する機械方向の引張強さの比を有する微細孔性重合体薄膜、
を備える、膜。
Claims (12)
- 単層PPのHEPA/ULPA膜を調製するための方法であって、前記方法が、
乾燥伸長工程により作られる細孔性ポリオレフィン薄膜の1つの層を有する膜を提供するステップであって、前記乾燥伸長工程が、
ポリオレフィンを少なくとも単一層の非細孔性前駆体に押出成形するステップと、
前記非細孔性前駆体を二軸伸長するステップであって、前記二軸伸長が機械方向の伸長および横方向の伸長を含み、前記横方向の伸長が、細孔性の単層PPのHEPA/ULPA膜を形成する同時制御される機械方向の弛緩を含み、前記細孔性の単層PPのHEPA/ULPA膜が、丸形状の細孔、40%乃至90%の細孔率、0.5乃至5.0の範囲内にある横方向の引張強さに対する機械方向の引張強さの比、100秒未満のJISガーリー、少なくとも0.04ミクロンの平均流動細孔径、0.04−0.12ミクロンのアクアポアサイズ、140psiよりも大きい水頭圧、および0.25乃至8.0の範囲内の球形度因数を有し、前記アクアポアサイズがASTM F316−93に基づいており、前記水頭圧がASTM D3393−91に基づいているステップと、
を備えるステップ
を備える、方法。 - 前記二軸伸長が、同時の機械方向の伸長を伴う横方向の伸長のステップをさらに含み、かつ、前記二軸伸長が横方向の弛緩のステップをさらに含む、請求項1に記載の方法。
- 前記非細孔性前駆体の前記二軸伸長が、機械方向の伸長の追加的なステップをさらに含む、請求項2に記載の方法。
- 前記乾燥伸長工程が、
前記二軸伸長より前に細孔性中間体を形成するための機械方向の伸長のステップ、
をさらに含む、請求項1に記載の方法。 - 前記乾燥伸長工程が、
同時制御される機械方向の弛緩を伴う前記横方向の伸長、同時の機械方向の伸長を伴う第2の横方向の伸長、その後の横方向の弛緩を含む、機械方向の伸長その後の前記二軸伸長のステップ、
を含む、請求項1に記載の方法。 - 前記細孔性ポリオレフィン薄膜が、少なくとも8ミクロンの厚さ、少なくとも300kgf/cm2の横方向の引張強さ、0.025未満の平均流動細孔径の標準偏差、少なくとも80psiの水侵入圧、および少なくとも8,000g/m2−日のWVTRをさらに有する、請求項1に記載の方法。
- 前記細孔性ポリオレフィン薄膜が、90℃にて1.0%未満、105℃にて1.5%未満、および120℃にて3.0%未満のうち少なくとも1つの横方向の収縮率をさらに有する、請求項1に記載の方法。
- 前記細孔性ポリオレフィン薄膜が、8ミクロン乃至80ミクロンの範囲内の厚さをさらに有する、請求項1に記載の方法。
- 前記非細孔性前駆体が、
膨張薄膜、溝穴鋳型薄膜、単一層押出成形および多層押出成形のうち少なくとも1つにより形成される単一層前駆体、ならびに共押出成形および積層のうち少なくとも1つにより形成される多層前駆体、
のうち少なくとも1つである、請求項1に記載の方法。 - 前記膜が、前記細孔性ポリオレフィン薄膜の少なくとも片側に結合された少なくとも1つの不織層、織層、または接合層をさらに含む、請求項1に記載の方法。
- 前記細孔性ポリオレフィン薄膜が、65%乃至90%の細孔率、1.0乃至5.0の範囲内にある横方向の引張強さに対する機械方向の引張強さの比、20秒未満のJISガーリー、少なくとも0.05ミクロンの平均流動細孔径、0.08−0.12ミクロンのアクアポアサイズ、および145psiよりも大きい水頭圧をさらに有する、請求項1に記載の方法。
- 前記丸形状の細孔が、0.75乃至1.25の範囲内の縦横比を有する、請求項1に記載の方法。
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JP2013527260A (ja) | 2013-06-27 |
EP2544841A4 (en) | 2015-09-02 |
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