JP2023515491A - 複合繊維、これを含む固体電解質、及びこれを含む金属空気電池 - Google Patents
複合繊維、これを含む固体電解質、及びこれを含む金属空気電池 Download PDFInfo
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- JP2023515491A JP2023515491A JP2022549878A JP2022549878A JP2023515491A JP 2023515491 A JP2023515491 A JP 2023515491A JP 2022549878 A JP2022549878 A JP 2022549878A JP 2022549878 A JP2022549878 A JP 2022549878A JP 2023515491 A JP2023515491 A JP 2023515491A
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- solid electrolyte
- chitosan
- composite fiber
- cellulose
- bound
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- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 1
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 1
- 229920000557 Nafion® Polymers 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 description 1
- 239000005708 Sodium hypochlorite Substances 0.000 description 1
- 229920004893 Triton X-165 Polymers 0.000 description 1
- YISUXFFRHDTCJW-UHFFFAOYSA-N [S].[P].[Cu] Chemical compound [S].[P].[Cu] YISUXFFRHDTCJW-UHFFFAOYSA-N 0.000 description 1
- ZBIKORITPGTTGI-UHFFFAOYSA-N [acetyloxy(phenyl)-$l^{3}-iodanyl] acetate Chemical compound CC(=O)OI(OC(C)=O)C1=CC=CC=C1 ZBIKORITPGTTGI-UHFFFAOYSA-N 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 1
- 238000004061 bleaching Methods 0.000 description 1
- 229910021538 borax Inorganic materials 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000002738 chelating agent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- UHZZMRAGKVHANO-UHFFFAOYSA-M chlormequat chloride Chemical compound [Cl-].C[N+](C)(C)CCCl UHZZMRAGKVHANO-UHFFFAOYSA-M 0.000 description 1
- 235000015165 citric acid Nutrition 0.000 description 1
- 230000001112 coagulating effect Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- AXZAYXJCENRGIM-UHFFFAOYSA-J dipotassium;tetrabromoplatinum(2-) Chemical compound [K+].[K+].[Br-].[Br-].[Br-].[Br-].[Pt+2] AXZAYXJCENRGIM-UHFFFAOYSA-J 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 125000004029 hydroxymethyl group Chemical group [H]OC([H])([H])* 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 239000003014 ion exchange membrane Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- LWXVCCOAQYNXNX-UHFFFAOYSA-N lithium hypochlorite Chemical compound [Li+].Cl[O-] LWXVCCOAQYNXNX-UHFFFAOYSA-N 0.000 description 1
- MHCFAGZWMAWTNR-UHFFFAOYSA-M lithium perchlorate Chemical compound [Li+].[O-]Cl(=O)(=O)=O MHCFAGZWMAWTNR-UHFFFAOYSA-M 0.000 description 1
- 229910001486 lithium perchlorate Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- -1 oxyl Chemical group 0.000 description 1
- QNGNSVIICDLXHT-UHFFFAOYSA-N para-ethylbenzaldehyde Natural products CCC1=CC=C(C=O)C=C1 QNGNSVIICDLXHT-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- SATVIFGJTRRDQU-UHFFFAOYSA-N potassium hypochlorite Chemical compound [K+].Cl[O-] SATVIFGJTRRDQU-UHFFFAOYSA-N 0.000 description 1
- 229910001487 potassium perchlorate Inorganic materials 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000005956 quaternization reaction Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000010517 secondary reaction Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- XUXNAKZDHHEHPC-UHFFFAOYSA-M sodium bromate Chemical compound [Na+].[O-]Br(=O)=O XUXNAKZDHHEHPC-UHFFFAOYSA-M 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 description 1
- 235000009518 sodium iodide Nutrition 0.000 description 1
- PFUVRDFDKPNGAV-UHFFFAOYSA-N sodium peroxide Chemical compound [Na+].[Na+].[O-][O-] PFUVRDFDKPNGAV-UHFFFAOYSA-N 0.000 description 1
- 239000004328 sodium tetraborate Substances 0.000 description 1
- 235000010339 sodium tetraborate Nutrition 0.000 description 1
- NYCVSSWORUBFET-UHFFFAOYSA-M sodium;bromite Chemical compound [Na+].[O-]Br=O NYCVSSWORUBFET-UHFFFAOYSA-M 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- KBLZDCFTQSIIOH-UHFFFAOYSA-M tetrabutylazanium;perchlorate Chemical compound [O-]Cl(=O)(=O)=O.CCCC[N+](CCCC)(CCCC)CCCC KBLZDCFTQSIIOH-UHFFFAOYSA-M 0.000 description 1
- 238000004148 unit process Methods 0.000 description 1
- RXBXBWBHKPGHIB-UHFFFAOYSA-L zinc;diperchlorate Chemical compound [Zn+2].[O-]Cl(=O)(=O)=O.[O-]Cl(=O)(=O)=O RXBXBWBHKPGHIB-UHFFFAOYSA-L 0.000 description 1
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Abstract
Description
バクテリア菌株として、アセトバクター・キシリナムを準備し、キトサン誘導体を準備した。キトサン誘導体は、1gのキトサン塩化物を、1%(v/v)の水性酢酸で溶解させた懸濁液を、1Mのグリシジルトリメチルアンモニウムクロリドで、N2雰囲気で、65℃で24時間処理した後、沈殿させ、エタノールで複数回ろ過して製造した。
前記ベース複合繊維の表面が酸化された第1の複合繊維(TEMPO-酸化されたCBC(oCBCs))は、図7に示しているように、2,2,6,6-テトラメチルピペリジン-1-オキシル(TEMPO)、臭素化ナトリウム(NaBr)、及び次亜塩素酸ナトリウム(NaClO)を用いる酸化反応により、ヒドロキシメチル及びオルト・パラ配向性(ortho para directing)のアセトアミドベース複合繊維(CBC)をTEMPOの酸化物に共役(conjugation)する方法で設計された。
前記ベース複合繊維に、窒素を有する第1の機能基が結合された第2の複合(Covalently quaternized CBC(qCBC))は、図8に示しているように、1,4-ジアザビシクロ[2.2.2]オクタンを用いたカップリング剤による臭素化されたベース複合繊維(CBC)、及び4次アミングループの共役する方法で製造された。
固体電解質は、図8に示しているように、前記第1の複合繊維(oCBC)及び前記第2の複合繊維(qCBC)を用いたゼラチン工程で製造した。具体的に、超音波を用いて、前記第1の複合繊維(oCBC)及び前記第2の複合繊維(qCBC)を、同一の重量比で、メチレンクロリド及び1,2-プロパンジオール及びアセトンの混合物(8:1:1 v/v/v%)で溶解させ、架橋剤として1wt%のグルタルアルデヒド、及び開始剤として0.3wt%のN、N-ジエチル-N-メチル-N-(2-メトキシエチル)アンモニウムビス(トリフルオロメタンスルホニル)イミドを添加した。
前述した実験例1-1のベース複合繊維の製造方法において、キトサン誘導体を省略し、脱塩過程を省略して、キトサンを含まないバクテリアセルロースを製造した。
グルコース(2wt%)、ペプトン(0.5wt%)、酵母(0.5wt%)、リン酸二ナトリウム(0.2wt%)、及びクエン酸(0.1wt%)を含む培養培地を用い、キトサン誘導体を省略し、脱塩過程を省略して、実験例1-1と同一の方法でバクテリアセルロースを製造した。
サトウキビバガス(bagasse)を準備し、エタノールに、脱イオン水、NaOH、及び硝酸を混合した溶媒を準備した。溶媒に、サトウキビバガスを分散させて洗浄した後に、ろ過し、中性pHとなるまで、脱イオン水で複数回洗浄した。
前記実験例1-4と同一の方法で固体電解質を製造する一方、実験例1-2の第1の複合繊維(oCBC)の割合、及び実験例1-3の第2の複合繊維(qCBC)の割合を、下記表3のように調節して、実験例2-1乃至実験例2-5による固体電解質を製造した。
前記実験例により、ベース複合繊維を製造する一方、キトサン誘導体の添加割合を調節して、キトサン含量が互いに異なるベース複合繊維を製造した。以後、前記実験例1-4により、キトサン含量が互いに異なるベース複合繊維を用いて、固体電解質を製造した。
前記実験例3-1乃至3-5に対する比較例として、純粋キトサンを準備した。
Claims (20)
- バクテリアセルロースと、前記バクテリアセルロースに結合されたキトサンとを有するベース複合繊維を含むことを特徴とする固体電解質。
- 前記ベース複合繊維は、結晶質相及び非晶質相が混在していることを特徴とする請求項1に記載の固体電解質。
- 前記キトサンが結合された前記バクテリアセルロースの表面が酸化されることを特徴とする請求項1に記載の固体電解質。
- 前記キトサンが結合された前記バクテリアセルロースの表面は、TEMPO水溶液を用いて酸化されることを特徴とする請求項3に記載の固体電解質。
- 前記キトサンが結合された前記バクテリアセルロースの表面は、窒素を有する第1の機能基と結合されることを特徴とする請求項1に記載の固体電解質。
- 前記ベース複合繊維の表面が酸化された第1の複合繊維と、
前記ベース複合繊維の表面が、窒素を有する第1の機能基と結合された第2の複合繊維とを含むことを特徴とする請求項1に記載の固体電解質。 - 前記第1の複合繊維の割合は、30wt%超え70wt%未満であり、
前記第2の複合繊維の割合は、70wt%未満30wt%超えであることを特徴とする請求項7に記載の固体電解質。 - 前記第1の複合繊維及び前記第2の複合繊維は、架橋結合されることを特徴とする請求項7に記載の固体電解質。
- セルロースを含むメンブレンと、
前記メンブレンの前記セルロースに結合され、30wt%超え70wt%未満のキトサンとを含むことを特徴とする固体電解質。 - 前記キトサンが50wt%の場合、XPS分析結果、C1sスペクトルでC-N結合の割合が最大値を有することを特徴とする請求項10に記載の固体電解質。
- 前記セルロースは、バクテリアセルロースを含むことを特徴とする請求項10に記載の固体電解質。
- 前記キトサンの割合によって、結晶性、イオン伝導度、及び膨潤比が制御されることを特徴とする請求項10に記載の固体電解質。
- 前記キトサンの割合が増加するほど、結晶性が逐次減少することを特徴とする請求項13に記載の固体電解質。
- キトサン誘導体を準備するステップと、
前記キトサン誘導体から、セルロースに結合されたキトサンが生成されるステップと、
前記キトサンが結合された前記セルロースを用いて、固体電解質を製造するステップとを含むことを特徴とする固体電解質の製造方法。 - 前記キトサン誘導体の割合によって、結晶性、イオン伝導度、及び膨潤比が制御されることを特徴とする請求項15に記載の固体電解質の製造方法。
- 前記セルロースは、バクテリアセルロースを含むことを特徴とする請求項15に記載の固体電解質の製造方法。
- 前記セルロースに結合された前記キトサンが生成されるステップは、
前記キトサン誘導体を有する培養培地を準備するステップと、
前記培養培地内にバクテリア菌株を注入し培養するステップとを含むことを特徴とする請求項17に記載の固体電解質の製造方法。 - 更に、酸化剤を用いて、前記キトサンが結合された前記セルロースの表面を酸化させて、第1の複合繊維を製造するステップ、又は、
前記キトサンが結合された前記セルロースの表面に臭素を結合させ、窒素を含む第1の機能基を臭素と置換させて、第2の複合繊維を製造するステップを含むことを特徴とする請求項15に記載の固体電解質の製造方法。 - 更に、酸化剤を用いて、前記キトサンが結合された前記セルロースの表面を酸化させて、第1の複合繊維を製造するステップと、
前記キトサンが結合された前記セルロースの表面に臭素を結合させ、窒素を含む第1の機能基を臭素と置換させて、第2の複合繊維を製造するステップと、
前記第1の複合繊維及び前記第2の複合繊維を架橋させるステップとを含むことを特徴とする請求項15に記載の固体電解質の製造方法。
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Application Number | Priority Date | Filing Date | Title |
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KR20200021253 | 2020-02-20 | ||
KR10-2020-0021252 | 2020-02-20 | ||
KR20200021252 | 2020-02-20 | ||
KR10-2020-0021253 | 2020-02-20 | ||
KR20200021894 | 2020-02-21 | ||
KR10-2020-0021894 | 2020-02-21 | ||
KR1020200164652A KR20210106328A (ko) | 2020-02-20 | 2020-11-30 | 복합 섬유, 이를 포함하는 고체 전해질, 및 이를 포함하는 금속 공기 전지 |
KR10-2020-0164653 | 2020-11-30 | ||
KR10-2020-0164652 | 2020-11-30 | ||
KR1020200164653A KR20210106329A (ko) | 2020-02-20 | 2020-11-30 | 복합 섬유, 이를 포함하는 고체 전해질, 및 이를 포함하는 금속 공기 전지 |
PCT/KR2021/002214 WO2021167431A1 (ko) | 2020-02-20 | 2021-02-22 | 복합 섬유, 이를 포함하는 고체 전해질, 및 이를 포함하는 금속 공기 전지 |
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CN104874427A (zh) * | 2015-04-03 | 2015-09-02 | 南京理工大学 | 一种燃料电池用碱性阴离子交换复合膜及其制备方法 |
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EP3130025B1 (en) * | 2014-05-15 | 2021-07-07 | Amtek Research International, LLC. | Covalently cross-linked gel electrolytes |
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WO2013042720A1 (ja) * | 2011-09-20 | 2013-03-28 | 日産化学工業株式会社 | セルロースファイバーをバインダーとして含有するリチウム二次電池電極形成用スラリー組成物及びリチウム二次電池用電極 |
CN104874427A (zh) * | 2015-04-03 | 2015-09-02 | 南京理工大学 | 一种燃料电池用碱性阴离子交换复合膜及其制备方法 |
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WO2021167431A1 (ko) | 2021-08-26 |
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US20210408567A1 (en) | 2021-12-30 |
EP4109635A1 (en) | 2022-12-28 |
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