JP2024511790A - ミクロ細孔性炭素材料の製造方法 - Google Patents
ミクロ細孔性炭素材料の製造方法 Download PDFInfo
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- 239000003575 carbonaceous material Substances 0.000 title claims abstract description 41
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 19
- 239000007789 gas Substances 0.000 claims abstract description 79
- 239000000463 material Substances 0.000 claims abstract description 54
- 229910052736 halogen Inorganic materials 0.000 claims abstract description 35
- 150000002367 halogens Chemical class 0.000 claims abstract description 35
- 229910052751 metal Inorganic materials 0.000 claims abstract description 27
- 239000002184 metal Substances 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 27
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000002245 particle Substances 0.000 claims description 22
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 20
- 239000000203 mixture Substances 0.000 claims description 20
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 16
- 238000010926 purge Methods 0.000 claims description 15
- 229910052799 carbon Inorganic materials 0.000 claims description 12
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 12
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 12
- 229910052786 argon Inorganic materials 0.000 claims description 10
- 238000005243 fluidization Methods 0.000 claims description 10
- 239000001307 helium Substances 0.000 claims description 5
- 229910052734 helium Inorganic materials 0.000 claims description 5
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 5
- 229910052743 krypton Inorganic materials 0.000 claims description 4
- DNNSSWSSYDEUBZ-UHFFFAOYSA-N krypton atom Chemical compound [Kr] DNNSSWSSYDEUBZ-UHFFFAOYSA-N 0.000 claims description 4
- 229910052754 neon Inorganic materials 0.000 claims description 4
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 claims description 4
- 229910052724 xenon Inorganic materials 0.000 claims description 4
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 4
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 3
- 229910039444 MoC Inorganic materials 0.000 claims description 3
- 229910052801 chlorine Inorganic materials 0.000 claims description 3
- 239000000460 chlorine Substances 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 229910003468 tantalcarbide Inorganic materials 0.000 claims description 3
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 claims description 3
- INZDTEICWPZYJM-UHFFFAOYSA-N 1-(chloromethyl)-4-[4-(chloromethyl)phenyl]benzene Chemical compound C1=CC(CCl)=CC=C1C1=CC=C(CCl)C=C1 INZDTEICWPZYJM-UHFFFAOYSA-N 0.000 claims description 2
- QIJNJJZPYXGIQM-UHFFFAOYSA-N 1lambda4,2lambda4-dimolybdacyclopropa-1,2,3-triene Chemical compound [Mo]=C=[Mo] QIJNJJZPYXGIQM-UHFFFAOYSA-N 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- UNASZPQZIFZUSI-UHFFFAOYSA-N methylidyneniobium Chemical compound [Nb]#C UNASZPQZIFZUSI-UHFFFAOYSA-N 0.000 claims description 2
- NFFIWVVINABMKP-UHFFFAOYSA-N methylidynetantalum Chemical compound [Ta]#C NFFIWVVINABMKP-UHFFFAOYSA-N 0.000 claims description 2
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 claims description 2
- 239000011148 porous material Substances 0.000 description 32
- 239000011261 inert gas Substances 0.000 description 10
- 238000009826 distribution Methods 0.000 description 9
- 238000002161 passivation Methods 0.000 description 8
- 238000003795 desorption Methods 0.000 description 7
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 5
- 229910021401 carbide-derived carbon Inorganic materials 0.000 description 5
- 238000012545 processing Methods 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- 238000004146 energy storage Methods 0.000 description 4
- 238000011156 evaluation Methods 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- 238000003775 Density Functional Theory Methods 0.000 description 3
- 230000004913 activation Effects 0.000 description 3
- 238000000137 annealing Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 150000001247 metal acetylides Chemical class 0.000 description 3
- 229910052752 metalloid Inorganic materials 0.000 description 3
- 150000002738 metalloids Chemical class 0.000 description 3
- 229910001868 water Inorganic materials 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000004438 BET method Methods 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 229910002091 carbon monoxide Inorganic materials 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 125000005843 halogen group Chemical group 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 2
- 238000004375 physisorption Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000004566 IR spectroscopy Methods 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 229910034327 TiC Inorganic materials 0.000 description 1
- 229910009361 YP-50F Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000002902 bimodal effect Effects 0.000 description 1
- 210000004027 cell Anatomy 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000008094 contradictory effect Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000005087 graphitization Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910001507 metal halide Inorganic materials 0.000 description 1
- -1 metal halide compound Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000012229 microporous material Substances 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 229910003465 moissanite Inorganic materials 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000012254 powdered material Substances 0.000 description 1
- 238000001812 pycnometry Methods 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 238000005549 size reduction Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 210000000352 storage cell Anatomy 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000009489 vacuum treatment Methods 0.000 description 1
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Abstract
Description
a)流動床反応器内にて、ハロゲンガス、またはハロゲンガスを含むガス混合物を用いて800℃以上1300℃以下(両端の値を含む)の温度にて粒状金属炭化物材料を流動化するステップ、
b)ステップa)で得られた生成物を、150℃以上250℃以下の温度(両端の値を含む)にて、かつ1ミリバール以上300ミリバール以下(両端の値を含む)の圧力の真空下にて維持するステップ、
そして、ステップa)の後で、またはステップa)に引き続いて、
c)水素ガスの雰囲気下で、または、ガス混合物の総体積に対して少なくとも30体積%の水素を含むガス混合物の雰囲気下で、800℃以上1300℃以下(両端の値を含む)の温度に維持するステップ、及び、
d)10μm以上30μm以下(両端の値を含む)の粒径D90、及び1.5μm以上2μm以下(両端の値を含む)の粒径D10となるまで粉砕するステップ。
以下、図1~図3を参照する。図2および図3は、SiCをベースとして前述の方法によって得られたミクロ細孔性炭素材料の特徴を示す。
本件方法が、上述のように、炭化物材料としてTiCを使用して実行される。細孔サイズの分布はSiCと似ているが、主ピークは8.5Åにある。炭素材料の表面積は約1681m2/g、総細孔容積は0.8cm3/gである。このうち、ミクロ細孔容積は0.6cm3/gを占め、ミクロ細細孔表面積は約1448m2/gである。
市販の活性炭は、例えばクラレ社から商品名YP-50Fとして入手可能である。細孔サイズの主ピークは8Åである。炭素材料は、表面積が約1707m2/gで、総細孔容積が0.9cm3/gである。ミクロ細孔容積が0.6cm3/gであり、ミクロ細孔表面積が1289m2/gである。
US2012/0148473A1は、金属および/または半金属を高温で高純度に熱化学エッチングすることによって金属炭化物から炭素を製造する方法を開示している。
S. Osswald、J. Chmiola, Y. Gogotsi, 「真空アニーリングによる炭化物由来炭素の構造進化」, CARBON、vol.50, no. 13, 2012?06?17, 4880~4886 pages, XP55938907, GB, ISSN: 0008?6223, doi:10.1016/j.carbon.2012.06.016は、炭化物由来炭素の高温処理を開示している。真空アニーリングは、1500℃まで細孔サイズに大きな変化を与えることなく、炭化チタン由来カーボンの細孔容積と表面積を増加させる。この処理により、サブナノメートルの細孔性と最大2000m 2 /gまでの比表面積を備えた微孔質炭素が生成される。一方、1600℃を超える温度でサンプルを処理すると、黒鉛化とミクロ細孔構造の崩壊により細孔サイズが1nmを超えて増加する。この結果は、真空処理を用いて細孔構造をさらに調整できることを示している。したがって、炭化物由来の炭素の真空アニーリングは、気相または液相の活性化などの従来の微細構造変性の方法に代わる適切な方法である。
WO2017/207593A1は、気相活性化による初期多孔質炭素材料の物理的活性化を開示している。所定の表面積と細孔サイズを備えたナノ多孔質炭素材料を選択し、500℃~900℃の温度範囲で炭素を加熱し、水蒸気と反応させることで活性化する。
WO2005/118471A1は、細孔径分布が修正・変更されたミクロ細孔性炭素を製造する方法を開示している。炭素は、金属炭化物またはメタロイド(半金属)炭化物から由来し得る。
Claims (11)
- ミクロ細孔性炭素材料を製造する方法であって、
a)流動床反応器内にて、800℃から1300℃までの温度で、ハロゲンガスまたはハロゲンガスを含むガス混合物を用いて粒状金属炭化物材料を流動化するステップ;
b)ステップa)で得られた生成物を、150℃から最大250℃までの温度にて、1ミリバールから300ミリバールまでの圧力で真空下に維持するステップと、
このステップb)の後に、またはこのステップb)に引き続いて、
c)水素ガスの雰囲気下で、または、ガス混合物の総体積に基づいて少なくとも30体積%の水素を含むガス混合物の雰囲気下で、800℃から1300℃までの温度に維持するステップと、
d)10μm~30μmのD90粒径および1.5μm~2μmのD10粒径までに粉砕するステップと、を含む方法。 - ステップa)が、ハロゲンガスまたは前記ガス混合物を用いて流動化した後、800℃から1300℃までの温度で、流動床反応器内にてパージガスを用いて流動化するステップを含み、パージガスは、この温度で少なくとも炭素と反応しない、請求項1に記載の方法。
- 前記パージガスが、ヘリウム、ネオン、アルゴン、クリプトン、およびキセノンからなる群から選択されるか、または前記パージガスがアルゴンである、請求項2に記載の方法。
- 前記金属炭化物材料が、炭化バナジウム材料、炭化チタン材料、炭化モリブデン材料、炭化ケイ素材料、炭化タングステン材料、炭化タンタル材料、および炭化ニオブからなる群から選択されるか、または、
前記金属炭化物材料が炭化ケイ素材料であり、ハロゲンガスは塩素である、請求項1~3のいずれかに記載の方法。 - ステップa)において、ハロゲンガスは、化学量論的に必要な量の100%から110%までの量が供給される、請求項1~4のいずれかに記載の方法。
- ステップb)において、真空が、5ミリバール~200ミリバール、好ましくは5ミリバール~80ミリバール、より好ましくは8ミリバール~15ミリバール、より好ましくは5ミリバール~15ミリバール、より好ましくは10ミリバールである、請求項1~5のいずれかに記載の方法。
- ステップa)は、8時間から13時間までの期間にわたって実施され、
ステップb)は、12時間から30時間までの期間にわたって実施され、
ステップc)は、2時間から4時間までの期間にわたって実行される、請求項1~6のいずれかに記載の方法。 - ステップa)において、ハロゲンガスによる流動化は、9時間から11時間までの期間にわたって実行され、パージガスによる流動化は、1.5時間から2.5時間までの期間にわたって実行され、
ステップb)は、22時間から26時間までの期間にわたって実施される、請求項7に記載の方法。 - ステップc)がステップd)の前に実行されるか、または、
ステップd)がステップc)の前に実行されるか、または、
ステップc)がステップd)の前に実行されてから、ステップc)が、より短い時間で再度実行される、請求項1~8のいずれかに記載の方法。 - ステップb)が流動床反応器を使用して実施される、請求項1~9のいずれかに記載の方法。
- ステップc)が、流動床反応器を使用して、またはロータリーキルンを使用して実行される、請求項1~10のいずれかに記載の方法。
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