JP5399239B2 - ナノ結晶金属酸化物の製造方法 - Google Patents
ナノ結晶金属酸化物の製造方法 Download PDFInfo
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- JP5399239B2 JP5399239B2 JP2009518789A JP2009518789A JP5399239B2 JP 5399239 B2 JP5399239 B2 JP 5399239B2 JP 2009518789 A JP2009518789 A JP 2009518789A JP 2009518789 A JP2009518789 A JP 2009518789A JP 5399239 B2 JP5399239 B2 JP 5399239B2
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- metal oxide
- oxide
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- 238000004519 manufacturing process Methods 0.000 title claims description 35
- 229910044991 metal oxide Inorganic materials 0.000 title claims description 30
- 150000004706 metal oxides Chemical class 0.000 title claims description 30
- 239000002245 particle Substances 0.000 claims description 22
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 9
- 239000000725 suspension Substances 0.000 claims description 8
- 230000010349 pulsation Effects 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 5
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims description 4
- 239000005751 Copper oxide Substances 0.000 claims description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 4
- 229910000431 copper oxide Inorganic materials 0.000 claims description 4
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims description 4
- 239000002159 nanocrystal Substances 0.000 claims description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 4
- 239000002002 slurry Substances 0.000 claims description 3
- 239000011787 zinc oxide Substances 0.000 claims description 2
- 230000001788 irregular Effects 0.000 claims 1
- 239000002923 metal particle Substances 0.000 claims 1
- 238000005507 spraying Methods 0.000 claims 1
- 239000007858 starting material Substances 0.000 description 21
- 239000000843 powder Substances 0.000 description 17
- 238000000034 method Methods 0.000 description 15
- 239000003054 catalyst Substances 0.000 description 14
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 9
- 238000002485 combustion reaction Methods 0.000 description 8
- 238000009826 distribution Methods 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 239000012530 fluid Substances 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 238000001704 evaporation Methods 0.000 description 5
- 230000008020 evaporation Effects 0.000 description 5
- 238000003786 synthesis reaction Methods 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 238000007796 conventional method Methods 0.000 description 4
- -1 mixed metal oxides Chemical class 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000012159 carrier gas Substances 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 239000002105 nanoparticle Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- BDAGIHXWWSANSR-UHFFFAOYSA-M Formate Chemical compound [O-]C=O BDAGIHXWWSANSR-UHFFFAOYSA-M 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
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- 238000000197 pyrolysis Methods 0.000 description 2
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- 239000004408 titanium dioxide Substances 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical class [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 229910017773 Cu-Zn-Al Inorganic materials 0.000 description 1
- 206010027476 Metastases Diseases 0.000 description 1
- 229910018657 Mn—Al Inorganic materials 0.000 description 1
- 208000034809 Product contamination Diseases 0.000 description 1
- 150000001242 acetic acid derivatives Chemical class 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000007900 aqueous suspension Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 150000003841 chloride salts Chemical class 0.000 description 1
- 239000000567 combustion gas Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000002178 crystalline material Substances 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000010335 hydrothermal treatment Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 238000010297 mechanical methods and process Methods 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 229910001960 metal nitrate Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000009401 metastasis Effects 0.000 description 1
- 229910003455 mixed metal oxide Inorganic materials 0.000 description 1
- 229910052863 mullite Inorganic materials 0.000 description 1
- 239000002707 nanocrystalline material Substances 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 150000002902 organometallic compounds Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000000541 pulsatile effect Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000010517 secondary reaction Methods 0.000 description 1
- 150000003377 silicon compounds Chemical class 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229910052566 spinel group Inorganic materials 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 238000007704 wet chemistry method Methods 0.000 description 1
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Description
[変形例1]
噴霧乾燥粉体の反応チャンバへの直接投入
金属酸化物を含み、噴霧乾燥された(必須ではない)粉体をシェンク(Schenk)ディスペンサーを用いて投入した。反応器における粉体の滞留時間は510〜700msであった。投入量を1時間あたり約10キログラムとした。温度は245〜265℃であった。
懸濁液の投入
水性懸濁液(30%固形分)を沈殿した出発生成物の濾過ケーキ2つから調製し、この懸濁液を反応器の燃焼チャンバに2−コンポーネントノズルを用いて噴霧した。本方法は、460℃〜680℃の温度で実施した。
溶液の注入
Cu−Zn−Alのギ酸塩(あるいはCu−Mn−Alギ酸塩)の水性溶液(約40%)をシュリック(Schlick)ノズルを用いて燃焼チャンバに噴霧した。本発明に係る製造方法を実施するために、温度範囲は350℃〜460℃とした。対応する溶液を一層低濃度(10〜30%)で使用することができることがさらに明らかになった。材料のBET表面積は60(Cu/Mn/Al混合酸化物)と70m2/g(Cu/Zn/Al混合酸化物)との間であった。従来の「湿式化学」法によって製造されたCu/Zn/Al混合酸化物の場合にはBET表面積が15〜35m2/gであった。本発明に係る材料の細孔容積分布を表1に示す。
本発明に係る製造方法を用いて得られうるナノ結晶粉体において、異なる出発材料を使用することにより、例えば、BET表面積および粒子サイズの点で異なる粉体特性を得ることも可能である。
Claims (3)
- a)気体を用いて金属酸化物を噴霧して反応チャンバに導入する工程と、
b)処理ゾーン中の前記金属酸化物を、240〜700℃の温度で15〜40バールの圧力で脈動流により熱処理する工程と、
c)ナノ結晶金属酸化物粒子を形成する工程と、
d)前記工程b)およびc)で得た前記ナノ結晶金属酸化物粒子を反応器から取り出す工程と、
を含み、
前記金属酸化物は溶液、スラリー、懸濁液、または固体凝集物の形態で前記反応チャンバに導入され、
一つまたは複数の、同一のまたは異なる金属酸化物を用い、
前記脈動流の脈動は規則的または不規則的であり、
前記処理ゾーンにおける熱処理後に、形成した前記ナノ結晶金属粒子を前記反応チャンバの低温ゾーンに移動させる、ナノ結晶金属酸化物粒子の製造方法。 - 前記ナノ結晶金属酸化物粒子の結晶子サイズが10nm〜10μmの範囲である、請求項1に記載の製造方法。
- 前記ナノ結晶金属酸化物粒子が、銅酸化物、亜鉛酸化物、およびアルミニウム酸化物;または銅酸化物、マンガン酸化物、およびアルミニウム酸化物を含有する、請求項1または2に記載の製造方法。
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DE102006032452A DE102006032452B4 (de) | 2006-07-13 | 2006-07-13 | Verfahren zur Herstellung nanokristalliner Metalloxide |
PCT/EP2007/006158 WO2008006565A1 (de) | 2006-07-13 | 2007-07-11 | Verfahren zur herstellung nanokristalliner metalloxide |
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CN (1) | CN101489667B (ja) |
DE (1) | DE102006032452B4 (ja) |
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WO2008006565A1 (de) | 2008-01-17 |
EP2054152A1 (de) | 2009-05-06 |
EP2054152B1 (de) | 2016-04-13 |
JP2009542573A (ja) | 2009-12-03 |
DK2335821T3 (en) | 2016-06-27 |
EA200970119A1 (ru) | 2009-06-30 |
CN101489667A (zh) | 2009-07-22 |
EP2335821A1 (de) | 2011-06-22 |
EA016985B1 (ru) | 2012-08-30 |
DK2054152T3 (en) | 2016-06-13 |
CN101489667B (zh) | 2012-09-12 |
US9579631B2 (en) | 2017-02-28 |
US20090325794A1 (en) | 2009-12-31 |
EP2335821B1 (de) | 2016-03-16 |
PL2054152T3 (pl) | 2016-10-31 |
DE102006032452B4 (de) | 2013-10-02 |
DE102006032452A1 (de) | 2008-01-17 |
JP5898160B2 (ja) | 2016-04-06 |
JP2014111520A (ja) | 2014-06-19 |
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