JP2006131458A - 酸化チタン粒子粉末及び光触媒 - Google Patents
酸化チタン粒子粉末及び光触媒 Download PDFInfo
- Publication number
- JP2006131458A JP2006131458A JP2004322635A JP2004322635A JP2006131458A JP 2006131458 A JP2006131458 A JP 2006131458A JP 2004322635 A JP2004322635 A JP 2004322635A JP 2004322635 A JP2004322635 A JP 2004322635A JP 2006131458 A JP2006131458 A JP 2006131458A
- Authority
- JP
- Japan
- Prior art keywords
- titanium oxide
- oxide particle
- particle powder
- particles
- nanostructure
- 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.)
- Granted
Links
- 239000002245 particle Substances 0.000 title claims abstract description 122
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 82
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 239000000843 powder Substances 0.000 title claims abstract description 70
- 239000011941 photocatalyst Substances 0.000 title claims description 10
- 239000011164 primary particle Substances 0.000 claims abstract description 40
- 239000002086 nanomaterial Substances 0.000 claims abstract description 35
- 239000010409 thin film Substances 0.000 claims abstract description 11
- 239000000203 mixture Substances 0.000 claims abstract description 5
- 239000012634 fragment Substances 0.000 claims abstract description 4
- 229910017053 inorganic salt Inorganic materials 0.000 abstract description 18
- 239000000243 solution Substances 0.000 abstract description 15
- 239000002105 nanoparticle Substances 0.000 abstract description 13
- 239000002994 raw material Substances 0.000 abstract description 10
- 150000003839 salts Chemical class 0.000 abstract description 5
- 238000005406 washing Methods 0.000 abstract description 5
- 239000012495 reaction gas Substances 0.000 abstract description 3
- 238000005507 spraying Methods 0.000 abstract description 3
- 239000007864 aqueous solution Substances 0.000 abstract description 2
- 230000009849 deactivation Effects 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 26
- 239000013078 crystal Substances 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 12
- 238000010438 heat treatment Methods 0.000 description 11
- 230000001699 photocatalysis Effects 0.000 description 9
- 239000002904 solvent Substances 0.000 description 8
- 239000006185 dispersion Substances 0.000 description 7
- 230000003197 catalytic effect Effects 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 238000005245 sintering Methods 0.000 description 6
- 238000011156 evaluation Methods 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 238000000746 purification Methods 0.000 description 5
- 235000002639 sodium chloride Nutrition 0.000 description 5
- 238000005118 spray pyrolysis Methods 0.000 description 5
- 238000003917 TEM image Methods 0.000 description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 238000001704 evaporation Methods 0.000 description 4
- 230000008020 evaporation Effects 0.000 description 4
- 239000010419 fine particle Substances 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- CXKWCBBOMKCUKX-UHFFFAOYSA-M methylene blue Chemical compound [Cl-].C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 CXKWCBBOMKCUKX-UHFFFAOYSA-M 0.000 description 4
- 229960000907 methylthioninium chloride Drugs 0.000 description 4
- 238000013032 photocatalytic reaction Methods 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- 238000005979 thermal decomposition reaction Methods 0.000 description 4
- 239000010936 titanium Substances 0.000 description 4
- 229910052719 titanium Inorganic materials 0.000 description 4
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 4
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 229910052938 sodium sulfate Inorganic materials 0.000 description 3
- 235000011152 sodium sulphate Nutrition 0.000 description 3
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 2
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000004332 deodorization Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000000197 pyrolysis Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000012798 spherical particle Substances 0.000 description 2
- 238000004438 BET method Methods 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000003373 anti-fouling effect Effects 0.000 description 1
- 230000003542 behavioural effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 150000003841 chloride salts Chemical class 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000004042 decolorization Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 1
- 235000019341 magnesium sulphate Nutrition 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 description 1
- 230000001443 photoexcitation Effects 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 description 1
- 229910052939 potassium sulfate Inorganic materials 0.000 description 1
- 235000011151 potassium sulphates Nutrition 0.000 description 1
- 230000003405 preventing effect Effects 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000000935 solvent evaporation Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 238000006557 surface reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000013076 target substance Substances 0.000 description 1
- 229910000348 titanium sulfate Inorganic materials 0.000 description 1
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/07—Producing by vapour phase processes, e.g. halide oxidation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/066—Zirconium or hafnium; Oxides or hydroxides thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/10—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of rare earths
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
- C01B13/14—Methods for preparing oxides or hydroxides in general
- C01B13/18—Methods for preparing oxides or hydroxides in general by thermal decomposition of compounds, e.g. of salts or hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
- C01F17/224—Oxides or hydroxides of lanthanides
- C01F17/235—Cerium oxides or hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/30—Preparation of aluminium oxide or hydroxide by thermal decomposition or by hydrolysis or oxidation of aluminium compounds
- C01F7/308—Thermal decomposition of nitrates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
- C01G23/0536—Producing by wet processes, e.g. hydrolysing titanium salts by hydrolysing chloride-containing salts
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G25/00—Compounds of zirconium
- C01G25/02—Oxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/06—Ferric oxide [Fe2O3]
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/60—Compounds characterised by their crystallite size
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
- C01P2004/34—Spheres hollow
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Nanotechnology (AREA)
- Composite Materials (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Catalysts (AREA)
Abstract
【解決手段】 30nm以下の一次粒子で構成される薄膜、球体及びその断片、或いはそれら混合物であることを特徴とするナノ構造体からなる酸化チタン粒子粉末は、ナノ構造体を構成する元素の水溶性塩と第三無機塩とを含有する原料水溶液を噴霧することによって、発生した液滴を反応ガスに同伴させて高温場に投入し、乾燥・熱分解を起こさせた後、生成した粒子を回収し、前記第三無機塩のみを水洗・除去することで得られる。
【選択図】 図1
Description
従来の噴霧熱分解法では原理上、生成粒子径は出発液滴径及び溶質濃度によって、ほぼ一義的に決定される。従って、噴霧熱分解法にてナノ粒子を製造しようとした場合、出発液滴の微小化、或いは溶質濃度の希薄化が必要となる。
液滴の微小化技術としては、超音波噴霧方式等が挙げられるが、数μmが限界であり、故に非現実的な溶質の希薄化が要求される。しかも、前記の液滴微小化技術ではいずれも極少量しか噴霧できず工業的であるとは言い難い。
一方、溶媒の蒸発速度が著しく大きい場合、溶媒及び溶質の移動が追いつかず、液滴表面に乾燥殻が生じる。内部には溶媒が閉じ込められた状態となる。さらに受熱することで、内圧が上昇し、やがて爆裂・破胞し、薄膜となる。これら両者現象を利用することで、薄膜或いは球体を作り分けることが可能となる。
即ち、薄膜状のナノ構造体では、薄膜と薄膜との間で接触面が発生するため、接触面を起点に焼結が進行する可能性があるものと考えられる。一方、球体状のナノ構造体では、球体間では基本的には接触面が小さく、また、数点しか発生しないため、焼結がより抑制できたと考えられる。
その結果、光励起に寄与する酸化チタン粒子の数も増加するとともに、一次粒子がナノサイズであることによって、高い活性を有するので、電子と正孔の表面反応速度が大きくなる。
従って、浄化対象物を短期間で、効率よく吸着・分解することができるものと本発明者は推定している。
但し、β=装置に起因する機械幅を補正した真の回折ピークの半値幅(ラジアン単位)。
K=シェラー定数(=0.9)。
λ=X線の波長(Cu Kα線 0.1542nm)。
θ=回折角(各結晶面の回折ピークに対応)。
酸化チタン粒子粉末の液相挙動は、「HELOS SYSTEM PARTICLE SIZE ANALYZER(以下、「へロス」とよぶ。)」 (JEOL製)を使用した。分散媒は純水を使用し、試料濃度を10%に調整し、超音波を300s照射した後、測定を行った。
水に四塩化チタン、硫酸ナトリウムをそれぞれ0.15mol/L、0.3mol/Lずつ溶解させて原料溶液を調製した。ここに得た原料溶液を二流体ノズルにより噴霧し、空気に同伴させ、加熱炉に供給した。加熱炉を出た粒子はバグフィルターにより捕集し、回収した粒子は超音波洗浄及び遠心分離により洗浄後、乾燥させた。
なお、加熱炉には抵抗加熱方式の管状炉を用い、炉心管には内径(D)70mm、有効長さ(L)1800mmのセラミック管を用いた。炉温は700℃とした。なお、使用した空気流量は全量で40NL/minとした。
得られた酸化チタン粒子粉末の水中での分散状態を図3に示す。へロスで測定した酸化チタン粒子粉末の平均粒径は0.4μmであり、SEM観察による粒子径とがほぼ同様であることから、得られた酸化チタン粒子粉末は水中においてほぼ単分散しているものと推定できる。
水に四塩化チタン、硫酸ナトリウムをそれぞれ0.15mol/L、0.3mol/Lずつ溶解させて原料溶液を調製した。ここに得た原料溶液を二流体ノズルにより噴霧し、空気に同伴させ、加熱炉に供給した。加熱炉を出た粒子はバグフィルターにより捕集し、回収した粒子は超音波洗浄及び遠心分離により洗浄後、乾燥させた。
なお、加熱炉には抵抗加熱方式の管状炉を用い、炉心管には内径(D)70mm、有効長さ(L)1800mmのセラミック管を用いた。炉温は600℃とした。なお、使用した空気流量は全量で40NL/minとした。
BET比表面積は202m2/gであった。
得られた酸化チタン粒子粉末の水中での分散状態を図5に示す。へロスで測定した酸化チタン粒子粉末の平均粒径は0.5μmであり、SEM観察による粒子径とがほぼ同様であることから、得られた酸化チタン粒子粉末は水中において、ナノ構造体の状態でほぼ単分散しているものと推定できる。
比較例としてST−01(石原産業製)を用いた。
実施例1、2、比較例1の酸化チタン粉末の光触媒活性はメチレンブルー水溶液(MB溶液)の脱色性能で評価した。
なおメチレンブルーは使用したブラックライトのUVではほとんど分解されず、光触媒作用により分解されて青色から無色になることから、光触媒の活性評価に広く用いられている。
Claims (4)
- 平均粒子径が30nm以下の一次粒子で構成されたナノ構造体からなることを特徴とする酸化チタン粒子粉末。
- 請求項1において、ナノ構造体の形状が薄膜、球体又はその断片、或いはそれら混合物であることを特徴とする酸化チタン粒子粉末。
- 請求項1又は2記載の酸化チタン粒子粉末において、球状ナノ構造体の平均粒径が50nm〜20μmであることを特徴とする酸化チタン粒子粉末。
- 請求項1乃至3のいずれかに記載の酸化チタン粒子粉末からなる光触媒。
Priority Applications (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2004322635A JP5241994B2 (ja) | 2004-11-05 | 2004-11-05 | 酸化チタン粒子粉末及び光触媒 |
US11/258,383 US7449199B2 (en) | 2004-11-05 | 2005-10-26 | Nanostructural substance |
EP05256631A EP1657219A3 (en) | 2004-11-05 | 2005-10-26 | Nanostructural substance |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2004322635A JP5241994B2 (ja) | 2004-11-05 | 2004-11-05 | 酸化チタン粒子粉末及び光触媒 |
Publications (2)
Publication Number | Publication Date |
---|---|
JP2006131458A true JP2006131458A (ja) | 2006-05-25 |
JP5241994B2 JP5241994B2 (ja) | 2013-07-17 |
Family
ID=35954016
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP2004322635A Active JP5241994B2 (ja) | 2004-11-05 | 2004-11-05 | 酸化チタン粒子粉末及び光触媒 |
Country Status (3)
Country | Link |
---|---|
US (1) | US7449199B2 (ja) |
EP (1) | EP1657219A3 (ja) |
JP (1) | JP5241994B2 (ja) |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2014015340A (ja) * | 2012-07-06 | 2014-01-30 | Daito Kasei Kogyo Kk | 球状二酸化チタン及び表面被覆球状二酸化チタン並びにそれを含有する化粧料 |
JP2014534141A (ja) * | 2011-08-31 | 2014-12-18 | シャンハイ ワールド−プロスペクト ケミテック カンパニーリミテッド | 二酸化チタン層を担持した無機非金属鉱物の複合材料、その製造方法および応用 |
JP2016175034A (ja) * | 2015-03-20 | 2016-10-06 | 公立大学法人高知工科大学 | 酸化チタン触媒およびその製造方法 |
WO2019117075A1 (ja) * | 2017-12-11 | 2019-06-20 | 日本化薬株式会社 | 中空粒子及びその製造方法、並びに白インク |
Families Citing this family (13)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP4714568B2 (ja) | 2005-11-22 | 2011-06-29 | マツダ株式会社 | 排気ガス浄化用触媒及びその製造方法 |
JP4851190B2 (ja) | 2006-01-13 | 2012-01-11 | 戸田工業株式会社 | 排気ガス浄化用触媒 |
US7892447B2 (en) | 2006-08-11 | 2011-02-22 | Aqua Resources Corporation | Nanoplatelet metal hydroxides and methods of preparing same |
US8822030B2 (en) | 2006-08-11 | 2014-09-02 | Aqua Resources Corporation | Nanoplatelet metal hydroxides and methods of preparing same |
US20080097018A1 (en) | 2006-10-18 | 2008-04-24 | John Stratton | Depolluting coating composition |
CN100431968C (zh) * | 2006-11-09 | 2008-11-12 | 上海大学 | 中空珠状纳米氧化铈及其制备方法 |
JP5267488B2 (ja) * | 2010-03-11 | 2013-08-21 | 信越化学工業株式会社 | ポリカーボネート樹脂積層体 |
US10471409B2 (en) * | 2012-11-05 | 2019-11-12 | University Of Rochester | Methods for producing hydrogen using nanoparticle-catalyst mixtures |
CN103011303B (zh) * | 2013-01-07 | 2014-12-03 | 云南云天化股份有限公司 | 氧化铁粒子的制备方法 |
IN2013MU02425A (ja) * | 2013-07-20 | 2015-06-19 | Tata Consultancy Services Ltd | |
TWI651269B (zh) * | 2013-09-23 | 2019-02-21 | 歐洲泰奧色得有限公司 | 二氧化鈦粒子及其製備方法 |
US10047443B2 (en) * | 2014-01-28 | 2018-08-14 | University Of Rochester | Methods for producing hydrogen using nanoparticle-catalyst mixtures |
EP3339248B1 (en) * | 2014-07-02 | 2020-02-26 | Ishihara Sangyo Kaisha, Ltd. | Method for producing titanium oxide fine particles |
Citations (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH0812961A (ja) * | 1993-10-01 | 1996-01-16 | Kao Corp | 紫外線遮蔽性複合微粒子、その製造方法、及び化粧料 |
JPH11349330A (ja) * | 1998-06-02 | 1999-12-21 | Murata Mfg Co Ltd | TiO2 粉体の製造方法 |
JP2000191325A (ja) * | 1998-12-25 | 2000-07-11 | Tayca Corp | 二酸化チタンの小球状粒子から形成される球状二酸化チタン集合体およびその製造方法 |
JP2001010867A (ja) * | 1999-06-21 | 2001-01-16 | Murata Mfg Co Ltd | セラミック原料造粒粉末の製造方法 |
JP2001114519A (ja) * | 1999-08-12 | 2001-04-24 | Sumitomo Chem Co Ltd | 多孔質チタニア、それを用いた触媒およびその製造方法 |
JP2001206720A (ja) * | 2000-01-26 | 2001-07-31 | Taki Chem Co Ltd | 酸化チタンゾル及びその製造方法 |
JP2003507300A (ja) * | 1999-06-24 | 2003-02-25 | アルテア ナノマテリアルズ インコーポレイテッド | 塩化チタン水溶液から超微細二酸化チタンを製造する方法 |
JP2005139020A (ja) * | 2003-11-05 | 2005-06-02 | National Institute For Materials Science | 可視光応答型酸化チタン粉末光触媒およびその製造法 |
Family Cites Families (18)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP3167756B2 (ja) | 1991-11-13 | 2001-05-21 | 花王株式会社 | 酸化亜鉛中空微粒子、その製造方法およびその装置 |
JPH08281060A (ja) | 1995-04-10 | 1996-10-29 | Toray Ind Inc | NOx吸収体およびその製造方法 |
JP3976851B2 (ja) * | 1996-09-13 | 2007-09-19 | 古河機械金属株式会社 | 二酸化チタン微粒子の製造方法、nox浄化用光触媒粉末の製造方法、塗料の製造方法、建材の製造方法 |
US6451220B1 (en) | 1997-01-21 | 2002-09-17 | Xerox Corporation | High density magnetic recording compositions and processes thereof |
FR2765591B1 (fr) | 1997-07-01 | 2002-08-09 | Pasteur Institut | Procede de diagnostic de la maladie d'alzheimer |
US8163386B1 (en) | 1997-09-02 | 2012-04-24 | Ishihara Sangyo Kaisha, Ltd. | Fine hollow powder thin flaky titanium oxide powder obtained by pulverization of the fine hollow powder and processes for producing the same |
JP4084463B2 (ja) * | 1998-06-05 | 2008-04-30 | 道雄 松村 | 光触媒用酸化チタン粉末 |
JP2000203810A (ja) | 1999-01-14 | 2000-07-25 | Toyota Central Res & Dev Lab Inc | 中空状酸化物粉末粒子 |
JP3517698B2 (ja) | 2000-03-03 | 2004-04-12 | 独立行政法人産業技術総合研究所 | ナノ粒子分散構造体及びその積層体 |
JP4822576B2 (ja) | 2000-05-30 | 2011-11-24 | 京セラ株式会社 | 無機質中空粉体とその製造方法 |
JP3857547B2 (ja) | 2001-07-09 | 2006-12-13 | 独立行政法人科学技術振興機構 | 噴霧熱分解法による微粒子の製造方法 |
AUPR725701A0 (en) * | 2001-08-24 | 2001-09-20 | Commonwealth Scientific And Industrial Research Organisation | Functionalised nanoparticle concentrates |
JP2003112925A (ja) | 2001-10-04 | 2003-04-18 | Mitsubishi Chemicals Corp | マグネタイト結晶ナノ粒子 |
JP2003297617A (ja) | 2002-04-03 | 2003-10-17 | Sony Corp | 強磁性合金ナノ粒子の製造方法 |
WO2004056461A2 (en) * | 2002-12-17 | 2004-07-08 | E.I. Du Pont De Nemours And Company | Method of producing nanoparticles using a evaporation-condensation process with a reaction chamber plasma reactor system |
JP4462828B2 (ja) * | 2003-01-20 | 2010-05-12 | 弌倫 木島 | チタン含有酸化物超微粒子の製造方法、及びチタン含有酸化物微粒子 |
RU2344994C2 (ru) * | 2003-12-03 | 2009-01-27 | Дегусса Аг | Порошкообразный диоксид титана, полученный пламенным гидролизом |
DE102004039139A1 (de) * | 2004-08-12 | 2006-02-23 | Degussa Ag | Yttrium-Zirkon-Mischoxidpulver |
-
2004
- 2004-11-05 JP JP2004322635A patent/JP5241994B2/ja active Active
-
2005
- 2005-10-26 EP EP05256631A patent/EP1657219A3/en not_active Withdrawn
- 2005-10-26 US US11/258,383 patent/US7449199B2/en not_active Expired - Fee Related
Patent Citations (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH0812961A (ja) * | 1993-10-01 | 1996-01-16 | Kao Corp | 紫外線遮蔽性複合微粒子、その製造方法、及び化粧料 |
JPH11349330A (ja) * | 1998-06-02 | 1999-12-21 | Murata Mfg Co Ltd | TiO2 粉体の製造方法 |
JP2000191325A (ja) * | 1998-12-25 | 2000-07-11 | Tayca Corp | 二酸化チタンの小球状粒子から形成される球状二酸化チタン集合体およびその製造方法 |
JP2001010867A (ja) * | 1999-06-21 | 2001-01-16 | Murata Mfg Co Ltd | セラミック原料造粒粉末の製造方法 |
JP2003507300A (ja) * | 1999-06-24 | 2003-02-25 | アルテア ナノマテリアルズ インコーポレイテッド | 塩化チタン水溶液から超微細二酸化チタンを製造する方法 |
JP2001114519A (ja) * | 1999-08-12 | 2001-04-24 | Sumitomo Chem Co Ltd | 多孔質チタニア、それを用いた触媒およびその製造方法 |
JP2001206720A (ja) * | 2000-01-26 | 2001-07-31 | Taki Chem Co Ltd | 酸化チタンゾル及びその製造方法 |
JP2005139020A (ja) * | 2003-11-05 | 2005-06-02 | National Institute For Materials Science | 可視光応答型酸化チタン粉末光触媒およびその製造法 |
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2014534141A (ja) * | 2011-08-31 | 2014-12-18 | シャンハイ ワールド−プロスペクト ケミテック カンパニーリミテッド | 二酸化チタン層を担持した無機非金属鉱物の複合材料、その製造方法および応用 |
JP2014015340A (ja) * | 2012-07-06 | 2014-01-30 | Daito Kasei Kogyo Kk | 球状二酸化チタン及び表面被覆球状二酸化チタン並びにそれを含有する化粧料 |
JP2016175034A (ja) * | 2015-03-20 | 2016-10-06 | 公立大学法人高知工科大学 | 酸化チタン触媒およびその製造方法 |
WO2019117075A1 (ja) * | 2017-12-11 | 2019-06-20 | 日本化薬株式会社 | 中空粒子及びその製造方法、並びに白インク |
JPWO2019117075A1 (ja) * | 2017-12-11 | 2020-12-17 | 日本化薬株式会社 | 中空粒子及びその製造方法、並びに白インク |
JP7058286B2 (ja) | 2017-12-11 | 2022-04-21 | 日本化薬株式会社 | 中空粒子及びその製造方法、並びに白インク |
US11345820B2 (en) | 2017-12-11 | 2022-05-31 | Nippon Kayaku Kabushiki Kaisha | Hollow particles and production method therefor, and white ink |
Also Published As
Publication number | Publication date |
---|---|
EP1657219A3 (en) | 2009-04-01 |
EP1657219A2 (en) | 2006-05-17 |
US20060116282A1 (en) | 2006-06-01 |
JP5241994B2 (ja) | 2013-07-17 |
US7449199B2 (en) | 2008-11-11 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
JP5241994B2 (ja) | 酸化チタン粒子粉末及び光触媒 | |
Mamaghani et al. | Hydrothermal/solvothermal synthesis and treatment of TiO2 for photocatalytic degradation of air pollutants: Preparation, characterization, properties, and performance | |
Pudukudy et al. | Synthesis, characterization and photocatalytic activity of annealing dependent quasi spherical and capsule like ZnO nanostructures | |
Vieira et al. | CeO2/TiO2 nanostructures enhance adsorption and photocatalytic degradation of organic compounds in aqueous suspension | |
TWI651269B (zh) | 二氧化鈦粒子及其製備方法 | |
Xiong et al. | Tunable BiOCl hierarchical nanostructures for high-efficient photocatalysis under visible light irradiation | |
Fei et al. | Controlled preparation of MnO2 hierarchical hollow nanostructures and their application in water treatment | |
Hwangbo et al. | Facile synthesis of zirconia nanoparticles using a salt-assisted ultrasonic spray pyrolysis combined with a citrate precursor method | |
Pudukudy et al. | Simple chemical synthesis of novel ZnO nanostructures: role of counter ions | |
KR101318743B1 (ko) | 산화 텅스텐계 광촉매 및 그 제조 방법 | |
Wang et al. | 7 Preparation of | |
Ghorai | Synthesis of spherical mesoporous titania modified iron-niobate nanoclusters for photocatalytic reduction of 4-nitrophenol | |
US20100209710A1 (en) | Manufacturing method of core-shell-type ceria-polymer hybrid nanoparticles and dispersion sols of them | |
Kadota et al. | Interfacial sol–gel processing for preparation of porous titania particles using a piezoelectric inkjet nozzle | |
Melo et al. | Effect of non-ionic surfactant in the solvothermal synthesis of anatase TiO2 nanoplates with a high percentage of exposed {001} facets and its role in the photocatalytic degradation of methylene blue dye | |
CN107889471B (zh) | 一种包含TiO2的光催化颗粒及其制备方法 | |
Rosnan et al. | Synthesis and characterization of ZnO-decorated GO nanocomposite material with different ZnO loading through sol-gel method | |
KR20040036464A (ko) | 티타니아계 촉매의 제조방법 | |
Yang et al. | Dynamic growth of rhombic dodecahedral Cu 2 O crystals controlled by reaction temperature and their size-dependent photocatalytic performance | |
Atrazina et al. | Catalytic study on TiO2 photocatalyst synthesised via microemulsion method on atrazine | |
Wang et al. | Template-free fabrication of rattle-type TiO 2 hollow microspheres with superior photocatalytic performance | |
JP5062988B2 (ja) | 新規酸化チタンおよび新規酸化チタンの合成方法 | |
JP5750662B2 (ja) | 酸化セリウムナノ粒子−ゼオライト複合体、その製造方法および紫外線遮蔽材としての利用 | |
JP2024515312A (ja) | 埋め込まれたナノ粒子を含むナノチタン酸塩、ナノチタン酸、ナノTiO2の製造方法、及び金属ナノ粒子の製造方法 | |
JP4776910B2 (ja) | ナノ構造体 |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
A621 | Written request for application examination |
Free format text: JAPANESE INTERMEDIATE CODE: A621 Effective date: 20070906 |
|
A977 | Report on retrieval |
Free format text: JAPANESE INTERMEDIATE CODE: A971007 Effective date: 20090430 |
|
A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20101116 |
|
A521 | Request for written amendment filed |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20110117 |
|
A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20110525 |
|
A02 | Decision of refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A02 Effective date: 20111228 |
|
A521 | Request for written amendment filed |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20120328 |
|
A911 | Transfer to examiner for re-examination before appeal (zenchi) |
Free format text: JAPANESE INTERMEDIATE CODE: A911 Effective date: 20120516 |
|
A912 | Re-examination (zenchi) completed and case transferred to appeal board |
Free format text: JAPANESE INTERMEDIATE CODE: A912 Effective date: 20120622 |
|
A61 | First payment of annual fees (during grant procedure) |
Free format text: JAPANESE INTERMEDIATE CODE: A61 Effective date: 20130403 |
|
FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20160412 Year of fee payment: 3 |
|
R150 | Certificate of patent or registration of utility model |
Free format text: JAPANESE INTERMEDIATE CODE: R150 Ref document number: 5241994 Country of ref document: JP Free format text: JAPANESE INTERMEDIATE CODE: R150 |
|
S531 | Written request for registration of change of domicile |
Free format text: JAPANESE INTERMEDIATE CODE: R313531 |
|
R350 | Written notification of registration of transfer |
Free format text: JAPANESE INTERMEDIATE CODE: R350 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |