JPWO2020040218A1 - グラフェンオキサイド吸着材及びその製造方法 - Google Patents
グラフェンオキサイド吸着材及びその製造方法 Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 203
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 176
- 239000003463 adsorbent Substances 0.000 title claims abstract description 152
- 238000004519 manufacturing process Methods 0.000 title claims description 21
- 239000011229 interlayer Substances 0.000 claims abstract description 97
- 239000000463 material Substances 0.000 claims abstract description 19
- 239000011148 porous material Substances 0.000 claims abstract description 16
- 239000000126 substance Substances 0.000 claims description 132
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 85
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 27
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 27
- 238000000034 method Methods 0.000 claims description 26
- 239000002904 solvent Substances 0.000 claims description 26
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 24
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 21
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 20
- 229910002804 graphite Inorganic materials 0.000 claims description 17
- 239000010439 graphite Substances 0.000 claims description 17
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 16
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 16
- 238000004108 freeze drying Methods 0.000 claims description 16
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 15
- 239000006185 dispersion Substances 0.000 claims description 14
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 8
- JVSWJIKNEAIKJW-UHFFFAOYSA-N dimethyl-hexane Natural products CCCCCC(C)C JVSWJIKNEAIKJW-UHFFFAOYSA-N 0.000 claims description 6
- 238000000926 separation method Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-ZSJDYOACSA-N Heavy water Chemical compound [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 51
- 238000001179 sorption measurement Methods 0.000 description 28
- 239000010410 layer Substances 0.000 description 20
- 150000001875 compounds Chemical class 0.000 description 14
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 description 12
- 239000007788 liquid Substances 0.000 description 12
- 238000001035 drying Methods 0.000 description 11
- 239000007864 aqueous solution Substances 0.000 description 8
- 239000000243 solution Substances 0.000 description 8
- 239000007789 gas Substances 0.000 description 7
- 239000011259 mixed solution Substances 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- 238000003795 desorption Methods 0.000 description 5
- 238000007710 freezing Methods 0.000 description 5
- 230000008014 freezing Effects 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 125000000524 functional group Chemical group 0.000 description 4
- 238000009830 intercalation Methods 0.000 description 4
- 230000002687 intercalation Effects 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 229920006395 saturated elastomer Polymers 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 238000002411 thermogravimetry Methods 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- XLYOFNOQVPJJNP-DYCDLGHISA-N deuterium hydrogen oxide Chemical compound [2H]O XLYOFNOQVPJJNP-DYCDLGHISA-N 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000012286 potassium permanganate Substances 0.000 description 2
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000002542 deteriorative effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000010981 drying operation Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000005457 ice water Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000009878 intermolecular interaction Effects 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910001507 metal halide Inorganic materials 0.000 description 1
- 150000005309 metal halides Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 235000010344 sodium nitrate Nutrition 0.000 description 1
- 239000004317 sodium nitrate Substances 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000005199 ultracentrifugation Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
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Abstract
Description
図2に示す方法で、グラフェンオキサイド吸着材を製造した。まず、容器に、0.5gのグラファイト粉末を測り取り、2.5gのリン酸水溶液(H3PO4水溶液、濃度:85質量%)、20gの濃硫酸(H2SO4、濃度:97質量%)、2.5gの過マンガン酸カリウム(KMnO4)粉末を加え混合溶液を調製して、35℃で2時間撹拌した。次いで、上記混合溶液に、50mLの水(H2O)を加え、よく撹拌した。その後、上記混合溶液に、1mLの過酸化水素水(H2O2、濃度:10質量%)を加え、25℃で30分間撹拌した。この過程で、グラファイトのグラフェン層を酸化し、表面官能基を生じさせ、さらに酸化したグラフェン層をグラファイトからはく離させることによって層状グラフェンオキサイドを含む溶液を調製した。
得られたグラフェンオキサイド吸着材の軽水及び重水に対する吸着性能を評価した。結果を図3に示す。図3は、グラフェンオキサイド吸着材における、軽水と重水との吸着量を示す吸着等温線である。当該吸着等温線の縦軸は水の吸着量(Water adsorption volume[mmol/g])を示し、横軸は吸着平衡時の水蒸気の圧力(P/P0[−])を示す。図3中、黒塗りの円(実線)は吸着時の軽水の吸着量、白抜きの円(破線)は脱離時の軽水の吸着量、黒塗りの三角形(実線)は吸着時の重水の吸着量、白塗りの三角形(破線)は脱離時の重水の吸着量を示している。
実施例1のGO吸着材の安定性を確認するため、熱重量測定を行った。熱重量測定においては、GO吸着材を静置し、1分ごとにN2ガスを150mL供給するとともに、1分ごとに系の温度を室温から1Kずつ上昇させて行った。実験は3つのサンプルで行った。結果を図5に示す。
実施例1のGO吸着材を80℃で120分間加熱処理して、グラフェンオキサイド吸着材を得た。かかる操作は、実施例1の凍結乾燥に代えて、通常の乾燥操作を行ったものに相当する。得られたグラフェンオキサイド吸着材の軽水及び重水に対する吸着性能を評価した。結果を図4に示す。
以下に示すモディファイド・ハマーズメソッドを用いて、グラフェンオキサイド分散液を調製し、これを加熱乾燥することによってグラフェンオキサイド吸着材を得た。
Claims (8)
- 互いに重なり合う複数の層状グラフェンオキサイドと、
前記複数の層状グラフェンオキサイド間に介在する層間物質と、
前記複数の層状グラフェンオキサイドと前記層間物質とで構成される細孔と、を有する、グラフェンオキサイド吸着材。 - 前記層間物質が、水、メタノール、エタノール、アセトン、テトラヒドロフラン、ジメチルホルムアミド、アセトニトリル、ジメチルスルホキシド、及びヘキサンからなる群より選択される少なくとも1種を含む、請求項1に記載のグラフェンオキサイド吸着材。
- 前記層状グラフェンオキサイドの層間距離が0.335〜2.50nmである、請求項1又は2に記載のグラフェンオキサイド吸着材。
- 前記層間物質と同じ物質を吸着させるために用いられる、請求項1〜3のいずれか一項に記載のグラフェンオキサイド吸着材。
- 請求項1〜3のいずれか一項に記載のグラフェンオキサイド吸着材に、吸着対象となる物質とその他の物質とを含む気体を接触させ、吸着対象となる物質を吸着させる工程を含む、物質の分離方法。
- 層間物質となる物質を含有する溶媒と、層状グラフェンオキサイドとを含むグラフェンオキサイド分散液を凍結乾燥し、前記溶媒の含有量を低減してグラフェンオキサイド吸着材を得る工程を有する、グラフェンオキサイド吸着材の製造方法。
- 前記層間物質が、水、メタノール、エタノール、アセトン、テトラヒドロフラン、ジメチルホルムアミド、アセトニトリル、ジメチルスルホキシド、及びヘキサンからなる群より選択される少なくとも1種を含む、請求項6に記載のグラフェンオキサイド吸着材の製造方法。
- 前記層状グラフェンオキサイドの層間距離が0.335〜2.50nmとなるように前記溶媒の含有量を低減する、請求項6又は7に記載のグラフェンオキサイド吸着材の製造方法。
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JP2006320853A (ja) * | 2005-05-20 | 2006-11-30 | Hitachi Powdered Metals Co Ltd | 黒鉛系水素吸蔵材料及びその製造方法 |
WO2017047872A1 (ko) * | 2015-09-18 | 2017-03-23 | 한국과학기술원 | 에너지 저장 물질로 유용한 다공성 나노구조체 및 이의 제조 방법 |
JP2018038987A (ja) * | 2016-09-09 | 2018-03-15 | 公立大学法人兵庫県立大学 | 水素吸蔵炭素材料及びその製造方法 |
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JP2004210583A (ja) * | 2002-12-27 | 2004-07-29 | Japan Science & Technology Agency | 新規メソポーラス炭素構造体の製造法 |
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JP7315152B2 (ja) | 2023-07-26 |
AU2019324724A1 (en) | 2021-02-18 |
EP3842137A1 (en) | 2021-06-30 |
CN112584923A (zh) | 2021-03-30 |
EP3842137A4 (en) | 2022-05-18 |
TW202017649A (zh) | 2020-05-16 |
US20210300761A1 (en) | 2021-09-30 |
WO2020040218A1 (ja) | 2020-02-27 |
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