JP2008019106A - 金属酸化物粒子の製造方法 - Google Patents
金属酸化物粒子の製造方法 Download PDFInfo
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- JP2008019106A JP2008019106A JP2006190335A JP2006190335A JP2008019106A JP 2008019106 A JP2008019106 A JP 2008019106A JP 2006190335 A JP2006190335 A JP 2006190335A JP 2006190335 A JP2006190335 A JP 2006190335A JP 2008019106 A JP2008019106 A JP 2008019106A
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- 229910044991 metal oxide Inorganic materials 0.000 title claims abstract description 93
- 150000004706 metal oxides Chemical class 0.000 title claims abstract description 93
- 239000002245 particle Substances 0.000 title claims abstract description 85
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 29
- 150000001412 amines Chemical class 0.000 claims abstract description 28
- 239000007864 aqueous solution Substances 0.000 claims abstract description 27
- 229910052751 metal Inorganic materials 0.000 claims abstract description 17
- 239000011164 primary particle Substances 0.000 claims abstract description 17
- 239000002184 metal Substances 0.000 claims abstract description 16
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 11
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000003223 protective agent Substances 0.000 claims description 16
- 229920003169 water-soluble polymer Polymers 0.000 claims description 11
- -1 lanthanoid metals Chemical class 0.000 claims description 9
- 239000006104 solid solution Substances 0.000 claims description 7
- 239000002202 Polyethylene glycol Substances 0.000 claims description 5
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 5
- 229920001223 polyethylene glycol Polymers 0.000 claims description 5
- 229920000642 polymer Polymers 0.000 claims description 5
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 5
- 229910052723 transition metal Inorganic materials 0.000 claims description 3
- 150000003624 transition metals Chemical class 0.000 claims description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 2
- 229920002845 Poly(methacrylic acid) Polymers 0.000 claims description 2
- 229920002873 Polyethylenimine Polymers 0.000 claims description 2
- 229920002125 Sokalan® Polymers 0.000 claims description 2
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 2
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- 229910052783 alkali metal Inorganic materials 0.000 claims description 2
- 150000001340 alkali metals Chemical class 0.000 claims description 2
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims description 2
- 150000001342 alkaline earth metals Chemical class 0.000 claims description 2
- 150000001805 chlorine compounds Chemical class 0.000 claims description 2
- 150000004679 hydroxides Chemical class 0.000 claims description 2
- 229910052747 lanthanoid Inorganic materials 0.000 claims description 2
- 150000002739 metals Chemical class 0.000 claims description 2
- 150000002823 nitrates Chemical class 0.000 claims description 2
- 229920000729 poly(L-lysine) polymer Polymers 0.000 claims description 2
- 229920002432 poly(vinyl methyl ether) polymer Polymers 0.000 claims description 2
- 229920002401 polyacrylamide Polymers 0.000 claims description 2
- 239000004584 polyacrylic acid Substances 0.000 claims description 2
- 229920001451 polypropylene glycol Polymers 0.000 claims description 2
- 229920000523 polyvinylpolypyrrolidone Polymers 0.000 claims description 2
- 239000001253 polyvinylpolypyrrolidone Substances 0.000 claims description 2
- 235000013809 polyvinylpolypyrrolidone Nutrition 0.000 claims description 2
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 2
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 2
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 2
- 150000003467 sulfuric acid derivatives Chemical class 0.000 claims description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims 2
- 229910021193 La 2 O 3 Inorganic materials 0.000 claims 1
- 235000014655 lactic acid Nutrition 0.000 claims 1
- 239000004310 lactic acid Substances 0.000 claims 1
- 239000000463 material Substances 0.000 claims 1
- 239000000243 solution Substances 0.000 abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 abstract description 4
- 229910002651 NO3 Inorganic materials 0.000 abstract description 2
- 150000002500 ions Chemical class 0.000 abstract description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 abstract 1
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 description 36
- 229910052684 Cerium Inorganic materials 0.000 description 16
- 239000002105 nanoparticle Substances 0.000 description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 12
- 229910021645 metal ion Inorganic materials 0.000 description 11
- 239000002131 composite material Substances 0.000 description 10
- 239000013078 crystal Substances 0.000 description 10
- 229910052726 zirconium Inorganic materials 0.000 description 10
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 9
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 8
- UJVRJBAUJYZFIX-UHFFFAOYSA-N nitric acid;oxozirconium Chemical compound [Zr]=O.O[N+]([O-])=O.O[N+]([O-])=O UJVRJBAUJYZFIX-UHFFFAOYSA-N 0.000 description 7
- 239000003999 initiator Substances 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 230000002776 aggregation Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 229910000420 cerium oxide Inorganic materials 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 3
- 238000006116 polymerization reaction Methods 0.000 description 3
- 229920006316 polyvinylpyrrolidine Polymers 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 238000010532 solid phase synthesis reaction Methods 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 2
- 230000001678 irradiating effect Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- QDZRBIRIPNZRSG-UHFFFAOYSA-N titanium nitrate Chemical compound [O-][N+](=O)O[Ti](O[N+]([O-])=O)(O[N+]([O-])=O)O[N+]([O-])=O QDZRBIRIPNZRSG-UHFFFAOYSA-N 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- XURCIPRUUASYLR-UHFFFAOYSA-N Omeprazole sulfide Chemical compound N=1C2=CC(OC)=CC=C2NC=1SCC1=NC=C(C)C(OC)=C1C XURCIPRUUASYLR-UHFFFAOYSA-N 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000003426 co-catalyst Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 229920001432 poly(L-lactide) Polymers 0.000 description 1
- 125000006239 protecting group Chemical group 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 239000008247 solid mixture Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000002076 thermal analysis method Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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Abstract
【解決手段】常温かつ常圧下にて、硝酸塩、水酸化物などの金属酸化物の金属元素が水溶液中にイオン状態で存在する金属酸化物の原料に対して、モノエタノールアミン、ジエタノールアミンなどの水溶性アミン類を添加することにより、水溶液のpHを4以上として金属酸化物粒子を生成する。さらに、金属酸化物粒子が生成された水溶液を、pHが1以上4以下に調製した後、超音波を照射することで、当該水溶液中にて金属酸化物粒子を一次粒子に単分散させる。
【選択図】図1
Description
硝酸セリウム5gを入れたルツボを800℃で5時間焼成することにより、酸化セリウムを合成した。
ジエタノールアミンをセリウムイオンに対して、0.5モル当量とした以外は、実施例1と同様の方法で合成物を得た。
ジエタノールアミンをセリウムイオンに対して、10モル当量とした以外は、実施例1と同様の方法で合成物を得た。
Claims (12)
- 一次粒子径がナノメートルオーダである金属酸化物粒子を製造する金属酸化物粒子の製造方法であって、
常温かつ常圧下にて、前記金属酸化物の金属元素が水溶液中にイオン状態で存在する前記金属酸化物の原料に対して、水溶性アミン類を添加することにより、前記金属酸化物粒子を生成することを特徴とする金属酸化物粒子の製造方法。 - 前記水溶液のpHを、前記水溶性アミン類の添加により4以上とすることを特徴とする請求項1に記載の金属酸化物粒子の製造方法。
- 前記水溶性アミン類の添加量を、前記金属酸化物の原料のモル数に対して、1モル当量以上5モル当量以下であることを特徴とする請求項1または2に記載の製造方法。
- 前記水溶性アミン類として、モノエタノールアミン、ジエタノールアミン、トリエタノールアミン、モノプロパノールアミン、ジプロパノールアミン、トリプロパノールアミンから選ばれる1種以上を用いることを特徴とする請求項1ないし3のいずれか1つに記載の金属酸化物粒子の製造方法。
- 前記金属酸化物粒子の金属元素種が、アルカリ金属類、アルカリ土類金属類、遷移金属類、ランタノイド金属類、典型金属類から選ばれる1種の酸化物粒子、あるいは、2種以上の固溶酸化物粒子であることを特徴とする請求項1ないし4のいずれか1つに記載の金属酸化物粒子の製造方法。
- 前記金属酸化物粒子が、CeO2、ZrO2、TiO2、Fe2O3、Al2O3、In2O3、CaO、MgO、MnO2、CoO、NiO、La2O3から選ばれる1種の酸化物粒子、あるいは、2種以上の固溶酸化物粒子であることを特徴とする請求項1ないし5のいずれか1つに記載の金属酸化物粒子の製造方法。
- 前記金属酸化物の原料として、硝酸塩、水酸化物、塩化物、硫酸塩から選ばれるものを用いることを特徴とする請求項1ないし6のいずれか1つに記載の金属酸化物粒子の製造方法。
- 前記金属酸化物粒子が生成された水溶液を、pHが1以上4以下に調製した後、超音波を照射することで、当該水溶液中にて前記金属酸化物粒子を一次粒子に単分散させることを特徴する請求項1ないし7のいずれか1つに記載の金属酸化物粒子の製造方法。
- 前記金属酸化物粒子中に、有機成分が5〜40%含まれることを特徴とする請求項1ないし8のいずれか1つに記載の金属酸化物粒子の製造方法。
- 前記有機成分が水溶性アミン類であることを特徴とする請求項9に記載の金属酸化物粒子の製造方法。
- 前記有機成分が水溶性アミン類以外に高分子保護剤を含むことを特徴とする請求項10に記載の金属酸化物粒子の製造方法。
- 前記高分子保護剤がポリビニルピロリドン、ポリビニルポリピロリドン、ポリエチレングリコール、ポリエチレンイミン、ポリビニルアルコール、ポリアクリルアミド、ポリアクリル酸、ポリメタクリル酸、ポリイタコン酸、ポリエチレンオキシド、ポリビニルメチルエーテル、ポリプロピレングリコール、ポリ−L−乳酸、ポリ−L−リシンから選ばれる1種以上の水溶性高分子保護剤からなることを特徴とする請求項11に記載の金属酸化物粒子の製造方法。
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Cited By (6)
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JP2010110719A (ja) * | 2008-11-07 | 2010-05-20 | Toyota Central R&D Labs Inc | 金属化合物のコロイド溶液およびその製造方法 |
US7922994B2 (en) | 2007-12-25 | 2011-04-12 | Denso Corporation | Method for preparing metal oxide particles with a controlled size |
JP2014034495A (ja) * | 2012-08-09 | 2014-02-24 | Kawamura Institute Of Chemical Research | 金属酸化物ナノ構造体及びその製造方法 |
KR101575326B1 (ko) | 2013-12-17 | 2015-12-08 | 디토테크놀로지 주식회사 | 환원성이 있는 폴리올 용매에 의한 구상 알루미나 미립자의 제조방법 |
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Cited By (7)
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US7922994B2 (en) | 2007-12-25 | 2011-04-12 | Denso Corporation | Method for preparing metal oxide particles with a controlled size |
JP2010110719A (ja) * | 2008-11-07 | 2010-05-20 | Toyota Central R&D Labs Inc | 金属化合物のコロイド溶液およびその製造方法 |
JP2014034495A (ja) * | 2012-08-09 | 2014-02-24 | Kawamura Institute Of Chemical Research | 金属酸化物ナノ構造体及びその製造方法 |
KR101575326B1 (ko) | 2013-12-17 | 2015-12-08 | 디토테크놀로지 주식회사 | 환원성이 있는 폴리올 용매에 의한 구상 알루미나 미립자의 제조방법 |
KR20200031361A (ko) * | 2018-09-14 | 2020-03-24 | 주식회사 엘지화학 | 산화니켈 나노 입자의 제조 방법 |
KR102509269B1 (ko) | 2018-09-14 | 2023-03-10 | 주식회사 엘지화학 | 산화니켈 나노 입자의 제조 방법 |
CN109160539A (zh) * | 2018-11-12 | 2019-01-08 | 青岛科技大学 | 一种纳米二氧化钛及其制备方法 |
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