JP6922893B2 - 吸着材 - Google Patents
吸着材 Download PDFInfo
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- JP6922893B2 JP6922893B2 JP2018505790A JP2018505790A JP6922893B2 JP 6922893 B2 JP6922893 B2 JP 6922893B2 JP 2018505790 A JP2018505790 A JP 2018505790A JP 2018505790 A JP2018505790 A JP 2018505790A JP 6922893 B2 JP6922893 B2 JP 6922893B2
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- Prior art keywords
- carbon nanohorn
- fibrous
- type
- carbon
- nanohorn aggregate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 239000003463 adsorbent Substances 0.000 title claims description 41
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 142
- 229910052799 carbon Inorganic materials 0.000 claims description 122
- 239000002116 nanohorn Substances 0.000 claims description 108
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 11
- 241000132500 Dahlia <angiosperm> Species 0.000 claims description 10
- 235000012040 Dahlia pinnata Nutrition 0.000 claims description 10
- 239000002356 single layer Substances 0.000 claims description 10
- 239000002041 carbon nanotube Substances 0.000 claims description 5
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 5
- 229910021389 graphene Inorganic materials 0.000 claims description 5
- 239000010457 zeolite Substances 0.000 claims description 5
- 229910021536 Zeolite Inorganic materials 0.000 claims description 4
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- 239000006229 carbon black Substances 0.000 claims description 3
- 239000000741 silica gel Substances 0.000 claims description 3
- 229910002027 silica gel Inorganic materials 0.000 claims description 3
- 239000011148 porous material Substances 0.000 description 24
- 239000007789 gas Substances 0.000 description 21
- 239000003054 catalyst Substances 0.000 description 19
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- 239000012298 atmosphere Substances 0.000 description 11
- 238000001179 sorption measurement Methods 0.000 description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- 239000007788 liquid Substances 0.000 description 10
- 230000015572 biosynthetic process Effects 0.000 description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 7
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- 229910052751 metal Inorganic materials 0.000 description 7
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- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 125000000524 functional group Chemical group 0.000 description 6
- 238000000608 laser ablation Methods 0.000 description 6
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- 238000007254 oxidation reaction Methods 0.000 description 6
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- 239000001257 hydrogen Substances 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- 229910052742 iron Inorganic materials 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 229910001873 dinitrogen Inorganic materials 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 150000002431 hydrogen Chemical class 0.000 description 4
- 229910017604 nitric acid Inorganic materials 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 230000009467 reduction Effects 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 238000013268 sustained release Methods 0.000 description 4
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- 239000003795 chemical substances by application Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
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- 239000002657 fibrous material Substances 0.000 description 3
- 239000011261 inert gas Substances 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- 239000012299 nitrogen atmosphere Substances 0.000 description 3
- 230000001590 oxidative effect Effects 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 2
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 2
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 229910003481 amorphous carbon Inorganic materials 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 239000012808 vapor phase Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000003570 air Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000001241 arc-discharge method Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052792 caesium Inorganic materials 0.000 description 1
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 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
- 238000006243 chemical reaction Methods 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000004332 deodorization Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000005227 gel permeation chromatography Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000005087 graphitization Methods 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 239000003273 ketjen black Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 229910021392 nanocarbon Inorganic materials 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- SBIBMFFZSBJNJF-UHFFFAOYSA-N selenium;zinc Chemical compound [Se]=[Zn] SBIBMFFZSBJNJF-UHFFFAOYSA-N 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 238000002411 thermogravimetry Methods 0.000 description 1
- 239000002441 uremic toxin Substances 0.000 description 1
- 239000013585 weight reducing agent Substances 0.000 description 1
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- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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Description
また、前記吸着材は、さらに前記繊維状のカーボンナノホーン集合体を構成しない、種型、つぼみ型、ダリア型、ペタルダリア型、ペタル型の球状カーボンナノホーン集合体を含むことを特徴としている。
さらに前記カーボンナノホーン集合体に含まれる単層カーボンナノホーンの一部が開孔部を有することを特徴とする吸着材が提供される。
さらに、前記吸着材は、活性炭、カーボンブラック、カーボンナノチューブ、グラフェン、ゼオライト、シリカゲル、アルミナの少なくとも一種類が含まれることを特徴とする。
(1)触媒含有炭素ターゲットを配置した容器内を、不活性ガス、窒素ガス、または、混合雰囲気下にする工程と、
(2)該ターゲットを蒸発させる工程と、
(3)得られたカーボンナノホーン集合体に開孔部を形成する工程と、
を含む方法により製造することができる。
図1及び図2は、本発明の一実施形態例に係る繊維状のカーボンナノホーン集合体の透過型電子顕微鏡(TEM)写真である。本実施形態例に係る繊維状のカーボンナノホーン集合体を構成している各単層カーボンナノホーンは、従来からの球状のカーボンナノホーン集合体を構成する単層カーボンナノホーンと同じである。本実施形態例に係る繊維状のカーボンナノホーン集合体は、種型、つぼみ型、ダリア型、ペタルダリア型、ペタル型(グラフェンシート構造)のカーボンナノホーン集合体が繋がって形成されており、すなわち、繊維状構造中に1種類または複数のこれらカーボンナノホーン集合体が含まれている。また、触媒金属を使用したターゲットを蒸発させて作製するため、繊維状のカーボンナノホーン集合体や球状のカーボンナノホーン集合体(図3)の内部または外部に、触媒金属が存在する(図2中の非透過の粒子)。本発明に係る製造方法により繊維状のカーボンナノホーン集合体を製造すると、球状のカーボンナノホーン集合体が同時に生成される。図3は、本発明によって作製された繊維状のカーボンナノホーン集合体と球状のカーボンナノホーン集合体の走査型電子顕微鏡(SEM)写真である。図3のように繊維状と球状の生成物が存在するため、繊維状生成物が凝集しにくい構造になる。また、繊維状生成物であるため、従来の球状カーボンナノホーンに比べ隙間を多くすることができる。本明細書では、繊維状のカーボンナノホーン集合体と球状のカーボンナノホーン集合体とを合わせて、単にカーボンナノホーン集合体と呼ぶことがある。なお、繊維状のカーボンナノホーン集合体と球状のカーボンナノホーン集合体とは、遠心分離法や、溶媒に分散した後沈降速度の違い、ゲル透過クロマトグラフィーなどを利用して分離することが可能である。さらに、カーボンナノホーン集合体以外の不純物が含まれる場合、遠心分離法、沈降速度の違い、サイズによる分離により除去できる。また、生成条件を変えることで、繊維状のカーボンナノホーン集合体と球状のカーボンナノホーン集合体の比率を変えることが可能である。繊維状カーボンナノホーン集合体の量を増やすことで、吸着させる気体や液体の流速を高くすることができる。なお、ここでいう「繊維状」とは、上記の分離操作を行ってもその形状をある程度維持できるものをいい、単に球状のカーボンナノホーン集合体が複数連なって、一見繊維状に見えるものとは異なる。
以上のようにして得られる繊維状カーボンナノホーン及びカーボンナノホーン集合体は、その炭素骨格の一部が触媒金属元素、窒素原子等で置換されていてもよい。
また、本発明に係る吸着材に徐放性の薬剤などを吸着させ、徐放剤として用いることもできる。本発明に係る吸着材、特に開孔を形成した吸着材は吸着能に優れ、より多くの薬剤を吸着、開孔内に取り込むことができ、徐放寿命の長い徐放剤が提供可能となる。
窒素雰囲気下で、鉄を約5質量%含有した炭素ターゲットにCO2レーザーを照射することで、繊維状カーボンナノホーン集合体と球状カーボンナノホーン集合体を作製した(サンプル1)。実験の詳細を以下に示す。鉄を含有した炭素ターゲットを、2rpmで回転させた。CO2レーザーのエネルギー密度は、150kW/cm2で連続的に照射し、チャンバー温度は室温であった。チャンバー内は、窒素ガス流量が10L/minになるように調整した。圧力は933.254〜1266.559hPa(700〜950Torr)に制御した。また、比較サンプルとして、触媒を含有しない炭素ターゲットを使用して窒素雰囲気下で、他の条件は同じでレーザーアブレーションしたサンプルも作製した(サンプル2)。
サンプル1及びサンプル2を空気中で熱処理した。サンプル1は、460℃まで1℃/分で昇温し、そのまま室温に戻した(サンプル3)。サンプル2は、500℃まで1℃/分で昇温し、そのまま室温に戻した(サンプル4)。ここで、熱処理温度が違うのは、サンプル1は触媒が含まれるため、燃焼温度が少し低くなるためである。
以上で得られたサンプル1〜4を、77Kでの窒素吸着法によって比表面積及び細孔容積(1〜100nm)を測定した。図4と図5は、それぞれ77Kでの窒素の吸着等温線と細孔分布である。表1には、比表面積と細孔容積をそれぞれ示す。比表面積、細孔容積は、繊維状カーボンナノホーン集合体を含むサンプル1の方が含まないサンプル2より大きいことが分かった。また、酸化処理により開孔を形成したサンプル3とサンプル4においても、繊維状カーボンナノホーン集合体を含むサンプル3の方が比表面積と細孔容積が大きく向上することが分かった。
この出願は、2016年3月16日に出願された日本出願特願2016−52228を基礎とする優先権を主張し、その開示の全てをここに取り込む。
Claims (7)
- 複数の単層カーボンナノホーンが繊維状に集合している繊維状カーボンナノホーン集合体を含むことを特徴とする吸着材。
- 前記繊維状カーボンナノホーン集合体の直径が30nm〜200nm、長さが1μm〜100μmであることを特徴とする請求項1に記載の吸着材。
- 各々の単層カーボンナノホーンは、直径が1nm〜5nm、長さが30nm〜100nmであり、先端がホーン状であることを特徴とする請求項1又は2に記載の吸着材。
- 前記繊維状カーボンナノホーン集合体は、種型、ダリア型、つぼみ型、ペタルダリア型、ペタル型の少なくとも一種類のカーボンナノホーン集合体が繊維状に繋がったものである請求項1乃至3のいずれか1項に記載の吸着材。
- さらに前記繊維状カーボンナノホーン集合体を構成しない、種型、つぼみ型、ダリア型、ペタルダリア型、ペタル型の少なくとも一種類の球状カーボンナノホーン集合体が含まれることを特徴とする請求項4に記載の吸着材。
- 前記単層カーボンナノホーンの一部が開孔部を有することを特徴とする請求項1乃至5のいずれか1項に記載の吸着材。
- さらに、活性炭、カーボンブラック、カーボンナノチューブ、グラフェン、ゼオライト、シリカゲル、アルミナの少なくとも一種類が含まれることを特徴とする請求項1乃至6のいずれか1項に記載の吸着材。
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