JP6022669B2 - スルホン化ブロック共重合体および粒状炭素のブレンドならびにこれを含む膜、フィルムおよび被膜 - Google Patents
スルホン化ブロック共重合体および粒状炭素のブレンドならびにこれを含む膜、フィルムおよび被膜 Download PDFInfo
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- JP6022669B2 JP6022669B2 JP2015500466A JP2015500466A JP6022669B2 JP 6022669 B2 JP6022669 B2 JP 6022669B2 JP 2015500466 A JP2015500466 A JP 2015500466A JP 2015500466 A JP2015500466 A JP 2015500466A JP 6022669 B2 JP6022669 B2 JP 6022669B2
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- 229910017604 nitric acid Inorganic materials 0.000 description 1
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- 238000012705 nitroxide-mediated radical polymerization Methods 0.000 description 1
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- RPQRDASANLAFCM-UHFFFAOYSA-N oxiran-2-ylmethyl prop-2-enoate Chemical compound C=CC(=O)OCC1CO1 RPQRDASANLAFCM-UHFFFAOYSA-N 0.000 description 1
- WYURNTSHIVDZCO-SVYQBANQSA-N oxolane-d8 Chemical compound [2H]C1([2H])OC([2H])([2H])C([2H])([2H])C1([2H])[2H] WYURNTSHIVDZCO-SVYQBANQSA-N 0.000 description 1
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- LYBIZMNPXTXVMV-UHFFFAOYSA-N propan-2-yl prop-2-enoate Chemical compound CC(C)OC(=O)C=C LYBIZMNPXTXVMV-UHFFFAOYSA-N 0.000 description 1
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- SJMYWORNLPSJQO-UHFFFAOYSA-N tert-butyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OC(C)(C)C SJMYWORNLPSJQO-UHFFFAOYSA-N 0.000 description 1
- ISXSCDLOGDJUNJ-UHFFFAOYSA-N tert-butyl prop-2-enoate Chemical compound CC(C)(C)OC(=O)C=C ISXSCDLOGDJUNJ-UHFFFAOYSA-N 0.000 description 1
- 150000003509 tertiary alcohols Chemical class 0.000 description 1
- 229920003046 tetrablock copolymer Polymers 0.000 description 1
- 125000000383 tetramethylene group Chemical group [H]C([H])([*:1])C([H])([H])C([H])([H])C([H])([H])[*:2] 0.000 description 1
- 238000009823 thermal lamination Methods 0.000 description 1
- 229920002803 thermoplastic polyurethane Polymers 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- DQWPFSLDHJDLRL-UHFFFAOYSA-N triethyl phosphate Chemical compound CCOP(=O)(OCC)OCC DQWPFSLDHJDLRL-UHFFFAOYSA-N 0.000 description 1
- VOITXYVAKOUIBA-UHFFFAOYSA-N triethylaluminium Chemical compound CC[Al](CC)CC VOITXYVAKOUIBA-UHFFFAOYSA-N 0.000 description 1
- AFFZTFNQQHNSEG-UHFFFAOYSA-N trifluoromethyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OC(F)(F)F AFFZTFNQQHNSEG-UHFFFAOYSA-N 0.000 description 1
- ZESXUEKAXSBANL-UHFFFAOYSA-N trifluoromethyl prop-2-enoate Chemical compound FC(F)(F)OC(=O)C=C ZESXUEKAXSBANL-UHFFFAOYSA-N 0.000 description 1
- PGQNYIRJCLTTOJ-UHFFFAOYSA-N trimethylsilyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)O[Si](C)(C)C PGQNYIRJCLTTOJ-UHFFFAOYSA-N 0.000 description 1
- OTYBJBJYBGWBHB-UHFFFAOYSA-N trimethylsilyl prop-2-enoate Chemical compound C[Si](C)(C)OC(=O)C=C OTYBJBJYBGWBHB-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- 239000002023 wood Substances 0.000 description 1
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Images
Classifications
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- A62B17/00—Protective clothing affording protection against heat or harmful chemical agents or for use at high altitudes
- A62B17/006—Protective clothing affording protection against heat or harmful chemical agents or for use at high altitudes against contamination from chemicals, toxic or hostile environments; ABC suits
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/66—Polymers having sulfur in the main chain, with or without nitrogen, oxygen or carbon only
- B01D71/68—Polysulfones; Polyethersulfones
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
- C08F8/34—Introducing sulfur atoms or sulfur-containing groups
- C08F8/36—Sulfonation; Sulfation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/76—Macromolecular material not specifically provided for in a single one of groups B01D71/08 - B01D71/74
- B01D71/80—Block polymers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F297/00—Macromolecular compounds obtained by successively polymerising different monomer systems using a catalyst of the ionic or coordination type without deactivating the intermediate polymer
- C08F297/02—Macromolecular compounds obtained by successively polymerising different monomer systems using a catalyst of the ionic or coordination type without deactivating the intermediate polymer using a catalyst of the anionic type
- C08F297/04—Macromolecular compounds obtained by successively polymerising different monomer systems using a catalyst of the ionic or coordination type without deactivating the intermediate polymer using a catalyst of the anionic type polymerising vinyl aromatic monomers and conjugated dienes
- C08F297/046—Macromolecular compounds obtained by successively polymerising different monomer systems using a catalyst of the ionic or coordination type without deactivating the intermediate polymer using a catalyst of the anionic type polymerising vinyl aromatic monomers and conjugated dienes polymerising vinyl aromatic monomers and isoprene, optionally with other conjugated dienes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L53/00—Compositions of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers
- C08L53/005—Modified block copolymers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L53/00—Compositions of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers
- C08L53/02—Compositions of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers of vinyl-aromatic monomers and conjugated dienes
- C08L53/025—Compositions of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers of vinyl-aromatic monomers and conjugated dienes modified
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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
- 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
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
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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
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T442/00—Fabric [woven, knitted, or nonwoven textile or cloth, etc.]
- Y10T442/20—Coated or impregnated woven, knit, or nonwoven fabric which is not [a] associated with another preformed layer or fiber layer or, [b] with respect to woven and knit, characterized, respectively, by a particular or differential weave or knit, wherein the coating or impregnation is neither a foamed material nor a free metal or alloy layer
- Y10T442/2762—Coated or impregnated natural fiber fabric [e.g., cotton, wool, silk, linen, etc.]
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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
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T442/00—Fabric [woven, knitted, or nonwoven textile or cloth, etc.]
- Y10T442/20—Coated or impregnated woven, knit, or nonwoven fabric which is not [a] associated with another preformed layer or fiber layer or, [b] with respect to woven and knit, characterized, respectively, by a particular or differential weave or knit, wherein the coating or impregnation is neither a foamed material nor a free metal or alloy layer
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Description
(a)少なくとも2つのポリマー末端ブロックAと、少なくとも1つのポリマー内部ブロックBとを含む、少なくとも1つのスルホン化ブロック共重合体であって、各Aブロックが、スルホン酸もしくはスルホネート官能基を本質的に含有せず、各Bブロックは、Bブロックのモノマー単位の数に基づいて約10から約100モルパーセントまでのスルホン酸もしくはスルホネート官能基を含有するポリマーブロックである、スルホン化ブロック共重合体;
(b)粒状炭素;および
(c)場合により液体成分
を提供する。
(a)各Aブロックが、スルホン酸もしくはスルホネート官能基を本質的に含有せず、各Bブロックが、Bブロックのモノマー単位の数に基づいて約10から約100モルパーセントまでのスルホン酸もしくはスルホネート官能基を含有するポリマーブロックである、少なくとも2つのポリマー末端ブロックAと、少なくとも1つのポリマー内部ブロックBとを含む、少なくとも1つのスルホン化ブロック共重合体;
(b)粒状炭素;および
(c)場合により液体成分
を含む組成物に関する。
i)(a)各Aブロックが、スルホン酸もしくはスルホネート官能基を本質的に含有せず、各Bブロックが、Bブロックのモノマー単位の数に基づいて約10から約100モルパーセントまでのスルホン酸もしくはスルホネート官能基を含有するポリマーブロックである、少なくとも2つのポリマー末端ブロックAと、少なくとも1つのポリマー内部ブロックBとを含む、少なくとも1つのスルホン化ブロック共重合体;
(b)粒状炭素;および
(c)液体成分として少なくとも1種類の有機溶媒;
を含む分散体を提供する工程;
ii)分散体をキャストする工程;
iii)1または複数の有機溶媒(c)を蒸発させて、膜、フィルムまたは被膜を得る工程;および
iv)場合により、(iii)で得た前記電極、膜、フィルムまたは被膜を水または水性媒体に浸漬する工程
を含む。
(a1)各Aブロックが、スルホン酸もしくはスルホネート官能基を本質的に含有せず、各Bブロックが、Bブロックのモノマー単位の数に基づいて約10から約100モルパーセントまでのスルホン酸もしくはスルホネート官能基を含有するポリマーブロックである、少なくとも2つのポリマー末端ブロックAと、少なくとも1つのポリマー内部ブロックBとを含む、少なくとも1つのスルホン化ブロック共重合体;および
(c)場合により液体成分を含み、
該基材のスルホン化ブロック共重合体(a1)および該被膜のスルホン化ブロック共重合体(a)は、同一であるかまたは異なり、該基材は粒状炭素を含まない。
別に指定される場合を除いて、本明細書において使用される表現「ブレンド」とは、スルホン化ブロック共重合体(a)および液体成分(c)を本質的に含まない粒状炭素(b)を含む固体分散体をさす。
本明細書に記載される組成物中で用いられるスルホン化ブロック共重合体の一態様は、スルホン化ブロック共重合体のポリマー構造に関する。スルホン化ブロック共重合体は、各Aブロックがスルホン化されにくいポリマーブロックであり、各Bブロックがスルホン化されやすいポリマーブロックである、少なくとも2つのポリマー端部もしくは外側のブロックAと、少なくとも1つのポリマー内部ブロックBを有する。
本開示に従って用いられる粒状炭素は、本質的に、ダイアモンドやガラス状炭素以外の炭素のあらゆる粒子形態であってよい。従って、粒状炭素は、いずれの非晶質炭素、例えば、コークス、カーボンブラックおよび活性炭であってもよいし、カーボンナノチューブであってもよいし、またはこれらの2以上の混合物であってもよい。一部の実施形態では、また膜の使用目的に応じて、粒状炭素は、場合により互いに組み合わせたか、またはカーボンナノチューブと組み合わせた、非晶質炭素、好ましくはカーボンブラックまたは活性炭である。さらなる実施形態では、粒状炭素は、カーボンブラックであるか、または活性炭であるか、またはカーボンナノチューブであるか、またはこの2以上の組合せである。特定の実施形態では、粒状炭素は、カーボンブラックであるか、または活性炭であるか、またはカーボンナノチューブである。
スルホン化ブロック共重合体および粒状炭素は、本質的に、スルホン化ブロック共重合体中の粒状炭素の均質な固体分散体を生じる任意の重量比でブレンドすることができる。当業者は、均質な固体分散体を得るためにスルホン化ブロック共重合体とブレンドすることのできる粒状炭素の制限最大量が、ある程度まで、粒状炭素の平均粒度および粒度分布によって決まることを理解するであろう。一般に、平均粒度が増加するにつれて、均質な固体分散体を得るためにブレンドされ得る粒状炭素の最大量は減少し、粒度分布が広くなるにつれて、均質な固体分散体を得るためにブレンドされ得る粒状炭素の最大量は増加する。これらの傾向を考慮して、当業者は、日常的なスクリーニングにより、例えば、1または複数の具体的な粒状炭素および特定のスルホン化ブロック共重合体を様々な重量比で含む分散液を調製することおよび分散体をキャストしてフィルム試料を得ることにより、特定のスルホン化ブロック共重合体とブレンドして均質な固体分散体を得ることのできる、具体的な粒状炭素の制限最大量または炭素類の組合せを容易に決定することができるであろう。
好都合なことに、スルホン化ブロック共重合体および粒状炭素の分散液は、
(a)適した溶媒もしくは分散剤中の少なくとも1つのスルホン化ブロック共重合体の溶液もしくは分散体、および
(b)場合により適した分散剤中の分散体の形態の粒状炭素;
を提供すること、ならびに
(c)該溶液もしくは分散体(a)と(b)を混合すること
により得られる。
i)以下を含む上述の分散液を提供すること
(a)各Aブロックが、スルホン酸もしくはスルホネート官能基を本質的に含有せず、各Bブロックが、Bブロックのモノマー単位の数に基づいて約10から約100モルパーセントまでのスルホン酸もしくはスルホネート官能基を含有するポリマーブロックである、少なくとも2つのポリマー末端ブロックAと、少なくとも1つのポリマー内部ブロックBとを含む、少なくとも1つのスルホン化ブロック共重合体;
(b)粒状炭素;および
(c)液体成分として少なくとも1種類の有機溶媒;
ii)分散液をキャストすること;
iii)1または複数の有機溶媒(c)を蒸発させて、膜、フィルムまたは被膜の非水和もしくは乾燥形態を得ること;ならびに
iv)場合により、(iii)で得られる電極、膜、フィルムまたは被膜を水または水性媒体に浸漬して、電極、膜、フィルムまたは被膜を部分的にまたは完全に水和した形態で得ること
によって得ることができる。
幾つかの実施形態によれば、スルホン化ブロック共重合体と粒状炭素をブレンドすることは、材料の性能に驚くべき影響を及ぼすことが見出された。例えば、一部の実施形態では、ブレンドを含む膜の吸水は、粒状炭素を含まない対応するスルホン化ブロック共重合体を含む膜の吸水よりも著しく低い。本開示に従うブレンドを含む膜が水を吸収する傾向の低下は、粒状炭素を含まないスルホン化ブロック共重合体を含む膜と比較して、湿潤環境および水性環境での膜の明らかに改善された寸法安定性をもたらす。一部の実施形態では、本開示に従うブレンドを含む膜は、非常に高レベルのイオン伝導率を示す。特定の実施形態では、膜を通過するイオン輸送は、ブレンドが水を吸収する傾向が低いにもかかわらず高い。一部の実施形態では、膜は、高い比導電率、カチオン輸送に対する高い選択性および浸水時の低い膨潤を示す。一部の実施形態では、本開示に従うブレンドは、対応するスルホン化ブロック共重合体よりも明らかに低易燃性である。
選択透過性(%)=膜間の電位低下/0.0158
当然、他の溶液および濃度を用いることもできる。しかし、異なる濃度ならびに溶液中のイオン移動度の差に関して補正を行うことが必要である。
−試験片は、3.0mmから13mmの厚さを有する試験片の75mmの標線間距離で40mm/分を超える燃焼速度を有さないか
−試験片は、3.0mm未満の厚さを有する試験片の75mmの標線間距離で75mm/分を超える燃焼速度を有さないか、または
−試験片は、炎が100mm標線に到達する前に燃焼を停止する。
本明細書に記載されるブレンドは、多様な用途および最終用途において膜、フィルムおよび被膜として用いることができ、これらの性質プロフィールにより、これらのブレンドは、水に浸漬されるかまたは湿潤環境に曝露された場合の寸法安定性、良好な湿潤強度、良好な寸法安定性、良好な水およびイオン輸送特性、良好なメタノール抵抗性、容易なフィルムもしくは膜形成、良好なバリア性、制御された柔軟性および弾性、調節可能な硬度、熱/酸化安定性および低い易燃性を必要とする用途での膜用材料として特に適したものとなる。
(a1)各Aブロックが、スルホン酸もしくはスルホネート官能基を本質的に含有せず、各Bブロックが、Bブロックのモノマー単位の数に基づいて約10から約100モルパーセントまでのスルホン酸もしくはスルホネート官能基を含有するポリマーブロックである、少なくとも2つのポリマー末端ブロックAと、少なくとも1つのポリマー内部ブロックBとを含む、少なくとも1つのスルホン化ブロック共重合体;および
(c)場合により液体成分、例えば水
を含み、プロトン交換膜基材のスルホン化ブロック共重合体(a1)およびブレンドのスルホン化ブロック共重合体(a)は、同一であっても異なっていてもよく、プロトン交換膜基材は粒状炭素を含まない。かかるMEA中の適したプロトン交換膜には、特に、概しておよび特に、例えば、US8,012,539、US7,737,224、US5,516,831、US5,239,010およびUS2010/0048817に記載されるスルホン化ブロック共重合体から作成された膜が含まれる。
以下の実施例は例証だけを目的とし、決して本発明の範囲を制限することを目的とするものでも、また制限すると解釈されるべきでもない。
本明細書に記載されるWVTR(逆カップ)は、ASTM E96/E96Mと同様に測定された。このASTM法は、より小さいバイアルを使用し、10mlの水を用い、露出膜面積を(ASTM法に従う1000mm2に対して)160mm2とすることにより修正した。水を添加し、バイアルを膜試験種で密封した後、バイアルを反転させ、25℃の温度および50%の相対湿度を有する空気を膜全体に吹き付けた。重量損失を時間に対して測定し、試験した膜厚について標準化した時の測定値に基づいてg/m2として、またはg×ミル/m2として水輸送速度を計算した。
スルホン化ブロック共重合体の調製:
構成A−D−B−D−Aを有するペンタブロック共重合体を、順次アニオン重合により調製した。ここで、Aブロックはパラ−tertブチルスチレン(ptBS)のポリマーブロックであり、Dブロックは水素化イソプレン(非水素化:Ip;水素化:E/P)のポリマーブロックで構成され、Bブロックは非置換スチレン(S)のポリマーブロックで構成された。シクロヘキサン中のt−ブチルスチレンのアニオン重合をsec−ブチルリチウムを用いて開始させ、15,000g/モルの分子量を有するAブロックを得た。次に、イソプレンモノマーを添加して2番目のブロックを分子量9,000g/モルで得た(ptBS−Ip−Li)。その後、スチレンモノマーをリビング(ptBS−Ip−Li)ジブロック共重合体溶液に添加し、重合してリビングトリブロック共重合体(ptBS−Ip−S−Li)を得た。このポリマースチレンブロックは、28,000g/モルの分子量を有するポリスチレンだけで構成された。この溶液に、イソプレンモノマーの別のアリコートを添加して、11,000g/モルの分子量を有するイソプレンブロックを得た。従って、これはリビングテトラブロック共重合体構造(ptBS−Ip−S−Ip−Li)をもたらした。パラ−tertブチルスチレンモノマーの第2のアリコートを添加し、メタノールを添加することによりこの重合を終わらせて、約14,000g/モルの分子量を有するptBSブロックを得た。次に、標準的なCO2+/トリエチルアルミニウム法を用いてptBS−Ip−S−Ip−ptBSを水素化して、ペンタブロックのイソプレン部分中のC=C不飽和を除去した。次に、i−無水酪酸/硫酸試薬を用いて、ブロックポリマーを(さらなる処理、酸化、洗浄または「仕上作業」もせずに)直接スルホン化した。水素化ブロック共重合体溶液を、ヘプタン(およそブロック共重合体溶液の体積あたり等体積のヘプタン)の添加により希釈して約10%の固体とした。十分なi−無水酪酸および硫酸(1/1(モル/モル))を添加して、1gのブロック共重合体あたり2.0meqのスルホン化ポリスチレン官能価を得た。エタノール(1モルのi−無水酪酸あたり2モルのエタノール)の添加により、スルホン化反応を終わらせた。得られるスルホン化ブロック共重合体は、電位差滴定により、ポリマー1gあたり2.0meqの−SO3Hの「イオン交換容量(IEC)」を有することが見出された。スルホン化ポリマーの溶液は、ヘプタン、シクロヘキサンおよびi−酪酸エチルの混合物中約10% wt/wtの固体レベルを有した。スルホン化ブロック共重合体を、以降、SBC−2.0と呼ぶ。
カーボンブラックは受け取ったまま使用した。粉末は、20μmの平均粒度を有すると述べられていた。
カーボンブラック(100g)をガラス容器に秤量した。シクロヘキサン(250g)を粉末の上に注入し、泥のテクスチャを有する濃厚な混合物を得た。SBC−2.0(シクロヘキサン/ヘプタン溶媒混合物中10重量%)の溶液(62.3gの溶液、約6.23gのSBC−2.0)を、カーボンブラックおよびシクロヘキサンの混合物に添加した。得られる分散体を含有する容器を機械的振盪機の上に置き、2時間かき混ぜた。驚くことに、得られる均一な懸濁液は、出発炭素粉末/シクロヘキサン泥よりも粘度が顕著に低かった。このようにして得た懸濁液は、約2.0重量%のSBC−2.0および約32重量%のカーボンブラックを含んでいた。SBC−2.0とカーボンブラックの重量比は約0.0623であった。
実施例1で得た懸濁液のアリコート(懸濁液207.3g、SBC−2.0 4.14g、カーボンブラック66.3g)を、新しい容器に移した。さらなるSBC−2.0溶液(溶液31.6g、SBC−2.0約3.16g)を、新しい容器中の懸濁液アリコートに添加した。新しい懸濁液を含有する容器を機械的振盪機の上に置き、2時間かき混ぜた。この新しい懸濁液の粘度は、実施例1の懸濁液について観察したものよりも顕著に低かった。このようにして得た懸濁液は、約3.1重量%のSBC−2.0および約28重量%のカーボンブラックを含んでいた。SBC−2.0とカーボンブラックの重量比は、約0.110であった。
実施例2で得た懸濁液のアリコート(懸濁液119.3g、SBC−2.0 3.65g、カーボンブラック33.1g)を、新しい容器に移した。さらなるSBC−2.0溶液(溶液32.2g、SBC−2.0約3.22g)を、新しい容器中の懸濁液アリコートに添加した。新しい懸濁液を含有する容器を機械的振盪機の上に置き、2時間かき混ぜた。この新しい懸濁液の粘度は、実施例2の懸濁液について観察したものよりも顕著に低かった。このようにして得た懸濁液は、約4.5重量%のSBC−2.0および約22重量%のカーボンブラックを含んでいた。SBC−2.0とカーボンブラックの重量比は、約0.208であった。
実施例3で得た懸濁液のアリコート(懸濁液75.7g、SBC−2.0 3.43g、カーボンブラック16.5g))を、新しい容器に移した。さらなるSBC−2.0溶液(溶液31.9g、SBC−2.0約3.19g)を、新しい容器中の懸濁液アリコートに添加した。新しい懸濁液を含有する容器を機械的振盪機の上に置き、2時間かき混ぜた。この新しい懸濁液の粘度は、実施例3の懸濁液について観察したものよりも顕著に低かった。このようにして得た懸濁液は、約6.1重量%のSBC−2.0および約15重量%のカーボンブラックを含んでいた。SBC−2.0とカーボンブラックの重量比は、約0.401であった。
実施例4で得た懸濁液のアリコート(懸濁液53.8g、SBC−2.0 3.31g、カーボンブラック8.25g))を、新しい容器に移した。 さらなるSBC−2.0溶液(溶液31.5g、SBC−2.0約3.15g)を、新しい容器中の懸濁液アリコートに添加した。新しい懸濁液を含有する容器を機械的振盪機の上に置き、2時間かき混ぜた。この新しい懸濁液の粘度は、実施例4の懸濁液について観察したものよりも顕著に低かった。このようにして得た懸濁液は、約7.6重量%のSBC−2.0および約9.6重量%のカーボンブラックを含んでいた。SBC−2.0とカーボンブラックの重量比は、約0.783であった。
実施例2から4で得た懸濁液を、懸濁液のアリコートをアルミニウム鍋に注入し、溶媒が室温で蒸発されることにより、固体フィルムにキャストした。実施例5から11で得た懸濁液は、10ミルのドクターブレードを用いてMylar剥離面の上にキャストした。懸濁液は均一なフィルムに乾燥した。実施例1から5に従うブレンドから得たフィルムの水蒸気透過速度を、逆カップ法を用いて調査した。実施例6から11に従うブレンドから得たフィルムの水蒸気透過速度を、直立カップ法を用いて調査した。データを次の表2aおよび2bにまとめる。
実施例7の膜およびSBC−2.0の比較膜を、UL94HBに従って難燃性について試験した。試験結果を次の表3にまとめる。
前述の実験の項において言及されるように、シクロヘキサンとカーボンブラックを組み合わせることにより、泥のようなテクスチャを有する混合物が得られた。シクロヘキサンはカーボンブラックと強く相互作用しないので、混合物は、水中の砂に類似したスラリーのような稠度を有した。シクロヘキサン/ヘプタン溶媒系中の少量のSBC−2.0をこのスラリーに添加することにより、驚くことに、低粘度の、炭素粒子の安定した懸濁液が生じた(実施例1)。この懸濁液は稠度が均一で、粘度が予想外に低かった。
Claims (7)
- (a)少なくとも2つのポリマー末端ブロックAと、少なくとも1つのポリマー内部ブロックBとを含む、少なくとも1つのスルホン化ブロック共重合体であって、各Aブロックが、スルホン酸もしくはスルホネート官能基を本質的に含有せず、各Bブロックが、前記Bブロックのモノマー単位の数に基づいて10から100モルパーセントまでのスルホン酸もしくはスルホネート官能基を含有するポリマーブロックである、スルホン化ブロック共重合体と;
(b)粒状炭素と;
を含み、スルホン化ブロック共重合体に対する粒状炭素の重量比が、少なくとも0.01である、組成物を含む、膜。 - スルホン化ブロック共重合体に対する粒状炭素の重量比が、0.01〜16である、請求項1に記載の膜。
- スルホン化ブロック共重合体に対する粒状炭素の重量比が、0.05〜4である、請求項1に記載の膜。
- 更に液体成分を含み、前記液体成分が、非プロトン性溶媒もしくはプロトン性溶媒、または少なくとも1種の非プロトン性溶媒と少なくとも1種のプロトン性溶媒の混合物である、請求項1〜3のいずれか一項に記載の膜。
- 請求項1〜4のいずれか一項に記載の膜の製造のための方法であって、
i)(a)少なくとも2つのポリマー末端ブロックAと、少なくとも1つのポリマー内部ブロックBとを含む、少なくとも1つのスルホン化ブロック共重合体であって、各Aブロックが、スルホン酸もしくはスルホネート官能基を本質的に含有せず、各Bブロックが、前記Bブロックのモノマー単位の数に基づいて10から100モルパーセントまでのスルホン酸もしくはスルホネート官能基を含有するポリマーブロックである、スルホン化ブロック共重合体;
(b)粒状炭素;および
(c)前記液体成分として少なくとも1種類の有機溶媒;
を含む分散体を提供する工程と;
ii)前記分散体をキャストする工程と;
iii)前記1または複数の有機溶媒(c)を蒸発させて、膜を得る工程と;ならびに
iv)場合により、(iii)で得た前記膜を水または水性媒体に浸漬する工程と
を含む、方法。 - 請求項1〜4のいずれか一項に記載の膜を含む、燃料電池、電池、または、エネルギーの貯蔵、ハーベスティングもしくは回収のための、逆電気透析もしくは電気透析のための、湿度を制御するための、圧力遅延浸透、正浸透もしくは逆浸透のための、電気脱イオン化もしくは容量性脱イオン化のための、または気体もしくは液体を精製もしくは解毒するための、装置。
- 基材と、請求項1〜4のいずれか一項に記載の少なくとも1つの膜とを含む、コーティングされた物品。
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WO2013138146A1 (en) | 2013-09-19 |
US10233323B2 (en) | 2019-03-19 |
JP2015510026A (ja) | 2015-04-02 |
CN104220152A (zh) | 2014-12-17 |
KR101700020B1 (ko) | 2017-01-25 |
EP2825298A4 (en) | 2015-11-18 |
TW201341458A (zh) | 2013-10-16 |
TWI654241B (zh) | 2019-03-21 |
EP2825298A1 (en) | 2015-01-21 |
RU2609477C2 (ru) | 2017-02-02 |
RU2014141504A (ru) | 2016-05-10 |
KR20140143797A (ko) | 2014-12-17 |
US20130240438A1 (en) | 2013-09-19 |
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