JP6895532B2 - イオン交換膜及びその製造方法、並びにこれを含むエネルギー貯蔵装置 - Google Patents
イオン交換膜及びその製造方法、並びにこれを含むエネルギー貯蔵装置 Download PDFInfo
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- JP6895532B2 JP6895532B2 JP2019548730A JP2019548730A JP6895532B2 JP 6895532 B2 JP6895532 B2 JP 6895532B2 JP 2019548730 A JP2019548730 A JP 2019548730A JP 2019548730 A JP2019548730 A JP 2019548730A JP 6895532 B2 JP6895532 B2 JP 6895532B2
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- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
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- 230000002441 reversible effect Effects 0.000 description 1
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- 230000001568 sexual effect Effects 0.000 description 1
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- 238000001308 synthesis method Methods 0.000 description 1
- JBQYATWDVHIOAR-UHFFFAOYSA-N tellanylidenegermanium Chemical compound [Te]=[Ge] JBQYATWDVHIOAR-UHFFFAOYSA-N 0.000 description 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
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- 125000002023 trifluoromethyl group Chemical group FC(F)(F)* 0.000 description 1
- 229930195735 unsaturated hydrocarbon Natural products 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
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Description
多孔度(%)=(多孔性支持体中の空気の体積/多孔性支持体の全体積)×100
一面のイオン伝導体層の厚さ比率(長さ%)=(一面のイオン伝導体層の厚さ/イオン交換膜の全厚さ)×100
<製造例1:スルホン化されたポリエーテルスルホン−エーテルケトンブロック共重合体の製造>
下記反応式3を用いてイオン伝導体を製造した。
SDCDPS(3,3−disulfonated−4,4’−dichlorodiphenyl sulfone)とビスフェノールA(bisphenol A)を、炭酸カリウム(Potassium carbonate)の存在下に、DMAc/トルエン共溶媒を用いて、160〜180℃の範囲で30時間反応した後、精製水に吐出して洗浄した後に、熱風乾燥した。
ビスフェノールA(bisphenol A)と1,3−ビス(4−クロロベンゾイル)ベンゼン(1,3−bis(4−chlorobenzoyol)benzene)を、炭酸カリウム(Potassium carbonate)の存在下に、DMAc/トルエン共溶媒を用いて、160〜180℃の範囲で30時間反応させた後、精製水に吐出して洗浄した後に熱風乾燥した。
前記製造された親水性領域及び疎水性領域を、炭酸カリウム(Potassium carbonate)の存在下に、DMAc/トルエン共溶媒を用いて160〜180℃の範囲で30時間反応後、精製水に吐出して洗浄した後に熱風乾燥した。
前記製造された重合体をジクロロメタン(dichloromethane)に溶解させた後、5倍の過剰量のクロロスルホン酸(chlorosulfonic acid)/DCM溶液に、徐々に入れて24時間撹拌した。前記溶液を廃棄し、析出された固形物を精製水にて洗浄した後に熱風乾燥した。
前記製造例1で製造された重合体を、DMAcに20重量%で溶解させた後に製膜し、シート状のイオン伝導体を製造した。
ウェットレイング方法を用いてポリフェニレンスルフィド(PPS)材質のマイクロポアを有する多孔性支持体を製造した。前記製造された多孔性支持体は、坪量が19.4g/m2で、多孔度が62%で、厚さが34μmであり、1〜1000μmのサイズのマイクロポアが分散されており、空隙の全体積に対する、マイクロポアのうちの31μm以上のサイズのポアの体積は、3体積%だった。マイクロポアの平均サイズは14.0603μmであり、最大サイズは657.8279μmだった。前記製造された多孔性支持体における、ポアサイズ(μm)に対するポア分布(体積%)を、CFP方法で測定し、その結果を図5にグラフで示した。
ポリアミド酸(polyamic acid)をジメチルホルムアミドに溶解させ、480poiseの紡糸溶液5Lを製造した。製造された紡糸溶液を溶液タンクに移送した後、これを、定量ギアポンプを用いて、20個のノズルが構成されており、高電圧として3kVが印加されている紡糸チャンバーに供給して紡糸し、ナノ繊維前駆体のウェブを製造した。この際、溶液供給量は1.5ml/minだった。製造されたナノ繊維前駆体のウェブを350℃で熱処理し、ナノポアを有する多孔性支持体(多孔度:80体積%)を製造した。
比較例2としては、フッ素系イオン交換膜であって、商業的に販売されるイオン交換膜であるデュポン社のNafion212を使用した。
比較例3としては、前記製造例1〜3と同じ方法で製造したが、マイクロポアサイズが31μm未満である、気孔が分散しているものを使用した。マイクロポアの平均サイズは8.3017μmであり、最大サイズは25.9855μmだった。前記使用された多孔性支持体における、ポアサイズ(μm)に対するポア分布(体積%)を、CFP方法で測定し、その結果を図6にグラフで示した。
前記製造例3(実施例1)及び比較製造例1〜3(比較例1〜3)で製造された強化複合膜の形態のイオン交換膜について、膨潤性(swelling ratio)、イオン伝導度(Ion−Conductivity)、及び、エネルギー貯蔵システム(VRFB)におけるエネルギー効率(EE,Energy Efficiency)を測定し、その結果を表1に示した。
(Twet−Tdry/Tdry)×100=△T(厚さに対する膨潤比、%)
(Lwet−Ldry/Ldry)×100=△L(面積に対する膨潤比、%)
膜抵抗(R)=(R1−R2)×(膜の有効面積)
イオン伝導度(S/cm)=1/R×t
CE=QD/QC
VE=EAD/EAC
EE=CE×VE
11,13 多孔性支持体
12,14 イオン伝導体層
102 セルハウジング
102A 陽極セル
102B 陰極セル
104 イオン交換膜
106 陽極
108 陰極
110 陽極電解質貯蔵タンク
112 陰極電解質貯蔵タンク
114,116 ポンプ
118 電源/負荷
201 イオン交換膜
202 電極
203 ポンプ
204 1M H2SO4
205 LCRメーター
Claims (14)
- 多数の空隙(pore)を含む多孔性支持体、及び、該多孔性支持体の空隙を充填しているイオン伝導体を含み、前記多孔性支持体は31〜1000μmのサイズのマイクロポア(micropore)を含み、
前記多孔性支持体は、前記空隙の全体積に対して31〜1000μmのサイズのマイクロポアを1〜20体積%で含む、イオン交換膜。 - 前記多孔性支持体の多孔度は、45%以上である、請求項1に記載のイオン交換膜。
- 前記多孔性支持体の厚さは、1〜200μmである、請求項1に記載のイオン交換膜。
- 多数の空隙(pore)を含む多孔性支持体、及び、該多孔性支持体の空隙を充填しているイオン伝導体を含み、前記多孔性支持体は31〜1000μmのサイズのマイクロポア(micropore)を含むイオン交換膜であって、
前記イオン伝導体は、前記イオン交換膜の全重量に対して30〜70重量%で含まれる、イオン交換膜。
- 前記イオン交換膜は、前記多孔性支持体の一面又は両面に位置するイオン伝導体層をさらに含み、
前記一面のイオン伝導体層の厚さは、1〜30μmである、請求項1に記載のイオン交換膜。 - 前記一面のイオン伝導体層の厚さは、前記イオン交換膜の全厚さに対して1〜50長さ%である、請求項5に記載のイオン交換膜。
- 前記多孔性支持体は、無作為に配向された複数本の繊維からなる、請求項1に記載のイオン交換膜。
- 多数の空隙を含む多孔性支持体を製造する段階、及び前記多孔性支持体の空隙にイオン伝導体を充填する段階を含み、前記多孔性支持体は31〜1000μmのサイズのマイクロポアを含み、
前記多孔性支持体は、前記空隙の全体積に対して31〜1000μmのサイズのマイクロポアを1〜20体積%で含む、イオン交換膜の製造方法。 - 前記多孔性支持体を製造する段階は、カーディング(carding)、ガーネッティング(garneting)、エアレイング(air−laying)、ウェットレイング(wet−laying)、メルトブローイング(melt blowing)、スパンボンディング(spunbonding)及びステッチボンディング(stitch bonding)からなる群から選ばれるいずれか一の方法によって製造する、請求項8に記載のイオン交換膜の製造方法。
- 前記多孔性支持体の空隙にイオン伝導体を充填する段階は、前記イオン伝導体をコートしてシート状に製造する段階、及び、前記シート状のイオン伝導体を前記多孔性支持体の空隙に溶融含浸させる段階を含む、請求項8に記載のイオン交換膜の製造方法。
- 前記溶融含浸は、1〜20MPaの圧力で150〜240℃で行われる、請求項10に記載のイオン交換膜の製造方法。
- 請求項1のイオン交換膜を含むエネルギー貯蔵装置。
- 前記エネルギー貯蔵装置は燃料電池である、請求項12に記載のエネルギー貯蔵装置。
- 前記エネルギー貯蔵装置はレドックス・フロー電池(redox flow battery)である、請求項12に記載のエネルギー貯蔵装置。
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