KR100633382B1 - 나노 크기의 광촉매용 아나타제형 이산화티탄 분말 및그의 제조방법 - Google Patents
나노 크기의 광촉매용 아나타제형 이산화티탄 분말 및그의 제조방법 Download PDFInfo
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- KR100633382B1 KR100633382B1 KR1020040082722A KR20040082722A KR100633382B1 KR 100633382 B1 KR100633382 B1 KR 100633382B1 KR 1020040082722 A KR1020040082722 A KR 1020040082722A KR 20040082722 A KR20040082722 A KR 20040082722A KR 100633382 B1 KR100633382 B1 KR 100633382B1
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- titanium dioxide
- titanium
- powder
- dioxide powder
- water
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- 238000004519 manufacturing process Methods 0.000 title claims description 11
- 239000011941 photocatalyst Substances 0.000 title abstract description 15
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 142
- 239000000843 powder Substances 0.000 claims abstract description 70
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 63
- 238000000034 method Methods 0.000 claims abstract description 32
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000012046 mixed solvent Substances 0.000 claims abstract description 15
- 239000002245 particle Substances 0.000 claims description 37
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical group [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims description 17
- 238000010335 hydrothermal treatment Methods 0.000 claims description 16
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 13
- 239000010936 titanium Substances 0.000 claims description 12
- 229910052719 titanium Inorganic materials 0.000 claims description 11
- 239000011148 porous material Substances 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- 238000010304 firing Methods 0.000 claims description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 239000006185 dispersion Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 2
- 230000009467 reduction Effects 0.000 claims description 2
- DNIAPMSPPWPWGF-GSVOUGTGSA-N (R)-(-)-Propylene glycol Chemical compound C[C@@H](O)CO DNIAPMSPPWPWGF-GSVOUGTGSA-N 0.000 claims 1
- 230000003301 hydrolyzing effect Effects 0.000 claims 1
- 238000010791 quenching Methods 0.000 abstract description 13
- 230000000171 quenching effect Effects 0.000 abstract description 13
- 239000007858 starting material Substances 0.000 abstract description 13
- 230000008569 process Effects 0.000 abstract description 12
- 230000000694 effects Effects 0.000 abstract description 5
- 238000007796 conventional method Methods 0.000 abstract description 4
- 230000001747 exhibiting effect Effects 0.000 abstract description 4
- 230000003287 optical effect Effects 0.000 abstract description 4
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 21
- 229960000907 methylthioninium chloride Drugs 0.000 description 21
- 239000013078 crystal Substances 0.000 description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 150000004703 alkoxides Chemical class 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 6
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 5
- BTANRVKWQNVYAZ-UHFFFAOYSA-N butan-2-ol Chemical compound CCC(C)O BTANRVKWQNVYAZ-UHFFFAOYSA-N 0.000 description 5
- 230000007062 hydrolysis Effects 0.000 description 5
- 238000006460 hydrolysis reaction Methods 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 4
- 238000000354 decomposition reaction Methods 0.000 description 4
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 4
- 238000003980 solgel method Methods 0.000 description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 238000006303 photolysis reaction Methods 0.000 description 3
- 238000004626 scanning electron microscopy Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- 229920002153 Hydroxypropyl cellulose Polymers 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 239000002537 cosmetic Substances 0.000 description 2
- 230000006837 decompression Effects 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 239000001863 hydroxypropyl cellulose Substances 0.000 description 2
- 235000010977 hydroxypropyl cellulose Nutrition 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 230000015843 photosynthesis, light reaction Effects 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000012085 test solution Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000004438 BET method Methods 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910006404 SnO 2 Inorganic materials 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 231100000460 acute oral toxicity Toxicity 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 238000004887 air purification Methods 0.000 description 1
- -1 aliphatic alcohols Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000003373 anti-fouling effect Effects 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 235000019219 chocolate Nutrition 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000001935 peptisation Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000000527 sonication Methods 0.000 description 1
- 230000001052 transient effect Effects 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
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Classifications
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- 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
-
- 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
- B01J6/00—Heat treatments such as Calcining; Fusing ; Pyrolysis
- B01J6/001—Calcining
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
Abstract
Description
구분 | 비표면적(㎡/g) | 입자직경(nm) |
실시예 1 | 116.43 | 12.47 |
실시예 2 | 90.07 | 13.23 |
실시예 3 | 81.05 | 22.76 |
실시예 4 | 101.23 | 13.78 |
실시예 5 | 87.67 | 19.82 |
실시예 6 | 54.91 | 29.35 |
실시예 7 | 42.58 | 14.58 |
실시예 8 | 54.02 | 31.10 |
Pore diameter : BET 방법을 측정하였으며, BJH 식에 의하여 계산하였다. |
Claims (9)
- 입경 1 ~ 5 ㎚인 이산화티탄 단위입자의 집합체로서 근접한 상기 이산화티탄 단위입자 간에 기공이 형성되어 있고, 이산화티탄 단위입자 집합체의 평균입경이 20 ~ 100 ㎚이며, 비표면적이 40 ~ 120 ㎡/g인 것을 특징으로 하는 광활성이 우수한 나노 크기의 아나타제형 이산화티탄 분말.
- 물과 알콜 혼합용매에 사염화티탄(TiCl4)을 분산시킨 후 30 ~ 100 ℃에서 가수분해하여 졸을 형성시키는 단계;상기 졸에 암모니아수를 가한 다음 세정 및 여과하여 비정질 티탄 겔을 형성시키는 단계; 및상기 비정질 티탄 겔을 물에 분산시킨 후 10 ~ 100 atm, 100 ~ 300 ℃에서 수열처리하고, 1 ∼ 5 atm/min의 감압속도와 5 ∼ 15 ℃/min의 감온속도로 켄칭 및 소성하여 이산화티탄 분말을 형성시키는 단계를 포함하여 이루어지는 것을 특징으로 하는 광활성이 우수한 나노 크기의 아나타제형 이산화티탄 분말의 제조방법.
- 제 2 항에 있어서, 상기 알콜은 C1 ~ C8의 지방족 알콜인 것을 특징으로 하 는 광활성이 우수한 나노 크기의 아나타제형 이산화티탄 분말의 제조방법.
- 제 2 항에 있어서, 상기 혼합용매는 물과 알콜이 1 ~ 5 : 5 ~ 1 부피비로 이루어진 것을 특징으로 하는 광활성이 우수한 나노 크기의 아나타제형 이산화티탄 분말의 제조방법.
- 제 2 항에 있어서, 상기 사염화티탄의 분산은 1 ~ 4 ℃의 혼합용매에서 수행되는 것을 특징으로 하는 광활성이 우수한 나노 크기의 아나타제형 이산화티탄 분말의 제조방법.
- 제 2 항에 있어서, 상기 사염화티탄의 분산은 비활성 가스 분위기에서 수행되는 것을 특징으로 하는 광활성이 우수한 나노 크기의 아나타제형 이산화티탄 분말의 제조방법.
- 제 2 항에 있어서, 상기 세정 및 여과는 물, 아세톤 또는 이들의 혼합물로 수행되는 것을 특징으로 하는 광활성이 우수한 나노 크기의 아나타제형 이산화티탄 분말의 제조방법.
- 삭제
- 제 2 항에 있어서, 상기 소성은 400 ~ 800 ℃, 1 ~ 4 시간 동안 수행되는 것을 특징으로 하는 광활성이 우수한 나노 크기의 아나타제형 이산화티탄 분말의 제조방법.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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KR101290400B1 (ko) | 2012-01-27 | 2013-07-26 | 군산대학교산학협력단 | 아나타제 이산화티타늄 나노 분말 제조 장치 |
KR101357053B1 (ko) * | 2011-10-20 | 2014-02-14 | 포항공과대학교 산학협력단 | 계층구조 이산화티탄 분말 제조방법 및 이를 이용한 염료감응형 태양전지 제조방법 |
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KR101804599B1 (ko) * | 2013-10-22 | 2017-12-06 | (주)엘지하우시스 | 광촉매재의 제조 방법 및 그에 의한 광촉매재 |
CN117088408B (zh) * | 2023-10-20 | 2023-12-26 | 西南石油大学 | 一种纳米二氧化钛及其制备方法与应用 |
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KR101357053B1 (ko) * | 2011-10-20 | 2014-02-14 | 포항공과대학교 산학협력단 | 계층구조 이산화티탄 분말 제조방법 및 이를 이용한 염료감응형 태양전지 제조방법 |
KR101290400B1 (ko) | 2012-01-27 | 2013-07-26 | 군산대학교산학협력단 | 아나타제 이산화티타늄 나노 분말 제조 장치 |
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