JP5725566B2 - 反応方法 - Google Patents
反応方法 Download PDFInfo
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- JP5725566B2 JP5725566B2 JP2012238412A JP2012238412A JP5725566B2 JP 5725566 B2 JP5725566 B2 JP 5725566B2 JP 2012238412 A JP2012238412 A JP 2012238412A JP 2012238412 A JP2012238412 A JP 2012238412A JP 5725566 B2 JP5725566 B2 JP 5725566B2
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- 238000006243 chemical reaction Methods 0.000 title claims description 68
- 238000000034 method Methods 0.000 title claims description 31
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 35
- 229910052799 carbon Inorganic materials 0.000 claims description 27
- 239000000376 reactant Substances 0.000 claims description 27
- 229910044991 metal oxide Inorganic materials 0.000 claims description 23
- 150000004706 metal oxides Chemical class 0.000 claims description 23
- 239000007791 liquid phase Substances 0.000 claims description 21
- 239000010409 thin film Substances 0.000 claims description 16
- 229910052751 metal Inorganic materials 0.000 claims description 13
- 239000002184 metal Substances 0.000 claims description 13
- 150000003839 salts Chemical class 0.000 claims description 10
- 238000006460 hydrolysis reaction Methods 0.000 claims description 9
- 238000006482 condensation reaction Methods 0.000 claims description 8
- 239000000047 product Substances 0.000 claims description 6
- 239000007795 chemical reaction product Substances 0.000 claims description 5
- 239000002105 nanoparticle Substances 0.000 description 30
- 239000003273 ketjen black Substances 0.000 description 13
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 9
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 9
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 6
- 229910021393 carbon nanotube Inorganic materials 0.000 description 6
- 239000002041 carbon nanotube Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 239000011164 primary particle Substances 0.000 description 5
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 4
- 238000003917 TEM image Methods 0.000 description 4
- 229910052744 lithium Inorganic materials 0.000 description 4
- 229910001416 lithium ion Inorganic materials 0.000 description 4
- 238000003980 solgel method Methods 0.000 description 4
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000003990 capacitor Substances 0.000 description 3
- 150000001721 carbon Chemical class 0.000 description 3
- 239000007772 electrode material Substances 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 238000004146 energy storage Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910001925 ruthenium oxide Inorganic materials 0.000 description 3
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000008151 electrolyte solution Substances 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 229910000000 metal hydroxide Inorganic materials 0.000 description 2
- 150000004692 metal hydroxides Chemical class 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- 229910052684 Cerium Inorganic materials 0.000 description 1
- 206010011224 Cough Diseases 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 239000006230 acetylene black Substances 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 229910003481 amorphous carbon Inorganic materials 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- 229910021383 artificial graphite Inorganic materials 0.000 description 1
- 229910052790 beryllium Inorganic materials 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 235000019241 carbon black Nutrition 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052747 lanthanoid Inorganic materials 0.000 description 1
- 150000002602 lanthanoids Chemical class 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 229910021382 natural graphite Inorganic materials 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- YBCAZPLXEGKKFM-UHFFFAOYSA-K ruthenium(iii) chloride Chemical compound [Cl-].[Cl-].[Cl-].[Ru+3] YBCAZPLXEGKKFM-UHFFFAOYSA-K 0.000 description 1
- 239000011163 secondary particle Substances 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Electric Double-Layer Capacitors Or The Like (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Oxygen, Ozone, And Oxides In General (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
- Carbon And Carbon Compounds (AREA)
Description
さらに、このような液相反応によって生成される水酸化金属水和物が電気エネルギー貯蔵素子として用いられる試みがある(特許文献3)
本発明の反応方法は、例えば図1に示すような反応器を用いて行うことができる。図1に示すように、反応器は開口部にせき板1−2を有する外筒1と貫通孔2−1を有し旋回する内筒2からなる。この反応器の内筒内部に反応物を投入し、内筒を旋回することによってその遠心力で内筒内部の反応物が内筒の貫通孔を通って外筒の内壁1−3に移動する。この時反応物は内筒の遠心力によって外筒の内壁に衝突し、薄膜状となって内壁の上部へずり上がる。この状態では反応物には内壁との間のずり応力と内筒からの遠心力の双方が同時に加わり、薄膜状の反応物に大きな機械的エネルギーが加わることになる。この機械的なエネルギーが反応に必要な化学エネルギー、いわゆる活性化エネルギーに転化するものと思われるが、短時間で反応が進行する。
旋回反応器の中に40mlのイソプロピルアルコール、1.25gのチタンテトラブトキシド、1gのケッチェンブラック(ケッチェン・ブラック・インターナショナル社製、商品名:ケッチェンブラックEC600JD、空隙率78Vol.%、一次粒子径40nm、平均二次粒径337.8nm)を加え、反応器の中でこれらを撹拌した。さらに、1gの水を添加して、66,000N(kgms-2)の遠心力で10分間、内筒を旋回して外筒の内壁に反応物の薄膜を形成するとともに、反応物にずり応力と遠心力を加えて化学反応を促進させ、酸化チタニウムナノ粒子を高分散担持させたケッチェンブラックを得た。
ケッチェンブラックに変えて、1gのカーボンナノチューブ(株式会社ジェムコ製)を用いて、実施例1と同様にして、酸化チタニウムナノ粒子を高分散担持させたカーボンナノチューブを得た。酸化チタニウムナノ粒子の一次粒子径は1〜10nmであった。
イソプロピルアルコール、チタンテトラブトキシド、ケッチェンブラックに変えて、40mlの水、1.965gの塩化ルテニウム、1gのカーボンナノチューブ(株式会社ジェムコ製)を用いて、実施例1と同様にして、酸化ルテニウムナノ粒子を高分散担持させたカーボンナノチューブを得た。図3にこの構造体のTEM像を示す。図3においては、一次粒子径1〜10nmの酸化ルテニウムナノ粒子がケッチェンブラックに高分散担持していることが分かる。
従来のゾル−ゲル法によって、すなわち本発明の化学反応を行わず、実施例1と同様にして、酸化チタニウム粒子が担持したケッチェンブラックを得た。酸化チタニウム粒子の一次粒子径は10〜50nmであった。
1−2…せき板
1−3…内壁
2…内筒
2−1…貫通孔
Claims (7)
- 液相反応の過程で、外筒と旋回する内筒を備えた反応器内で、内筒の旋回により、内筒内の反応物である金属塩を外筒の内壁に衝突させて当該反応物にずり応力と遠心力を加え、当該反応物の液相反応を促進させて金属酸化物を生成する反応方法。
- 液相反応の過程で、外筒と旋回する内筒を備えた反応器内で、内筒の旋回により、内筒内の反応物である金属塩とカーボンを外筒の内壁に衝突させて当該反応物とカーボンにずり応力と遠心力を加え、当該反応物の液相反応を促進させて生成物である金属酸化物を生成すると同時に生成物とカーボンを分散させる反応方法。
- 前記反応器の外筒の内壁で反応物を含む薄膜を生成し、この薄膜にずり応力と遠心力を加えて、液相反応を促進させる請求項1又は2に記載の反応方法。
- 前記反応器が、外筒と内筒の同心円筒からなり、内筒の側面に貫通孔を備えるとともに、外筒の開口部にせき板を配置してなり、内筒の旋回による遠心力によって内筒内の反応物を内筒の貫通孔を通じて外筒の内壁面に移動させ、外筒の内壁面に反応物を含む薄膜を生成するとともに、この薄膜にずり応力と遠心力を加えて液相反応を促進させる請求項3記載の反応方法。
- 前記薄膜が5mm以下である請求項3又は4に記載の反応方法。
- 前記反応器の内筒内の反応物に加えられる遠心力が1500N(kgms−2)以上である請求項4又は5に記載の反応方法。
- 液相反応が金属塩の加水分解反応および/または縮合反応である請求項1〜6のいずれか1項に記載の反応方法。
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JP3149375B2 (ja) * | 1997-01-14 | 2001-03-26 | 株式会社ジーナス | 微粒化方法及びその装置 |
JP2000036441A (ja) * | 1998-07-17 | 2000-02-02 | Fuji Electric Co Ltd | 電気エネルギー貯蔵素子およびその製造方法 |
JP4297533B2 (ja) * | 1998-10-13 | 2009-07-15 | ホソカワミクロン株式会社 | リチウムイオン電池材料の製造方法 |
JP2004307912A (ja) * | 2003-04-04 | 2004-11-04 | Murata Mfg Co Ltd | 金属粉末の製造方法および導電性ペースト |
JP2004323884A (ja) * | 2003-04-23 | 2004-11-18 | Sumitomo Metal Mining Co Ltd | 超微粒子のニッケル粉末及びその製造方法 |
JP4488779B2 (ja) * | 2003-09-30 | 2010-06-23 | 三洋電機株式会社 | 非水電解液二次電池用電極の製造方法及び非水電解液二次電池 |
JP2005169315A (ja) * | 2003-12-12 | 2005-06-30 | Hosokawa Funtai Gijutsu Kenkyusho:Kk | 合成粉体製造方法 |
JP4462483B2 (ja) * | 2004-03-25 | 2010-05-12 | 日立マクセル株式会社 | 微粒子担持カーボン粒子の製造方法および該製造方法で製造された微粒子担持カーボン粒子 |
CN1964917B (zh) * | 2004-06-11 | 2012-07-18 | 国立大学法人东京农工大学 | 内包氧化钌的纳米碳复合结构体 |
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