KR100854984B1 - 미립자 이산화티탄 및 그의 제조방법과 용도 - Google Patents
미립자 이산화티탄 및 그의 제조방법과 용도 Download PDFInfo
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 469
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 216
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 31
- 239000000843 powder Substances 0.000 claims abstract description 144
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 108
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims abstract description 38
- 238000010438 heat treatment Methods 0.000 claims abstract description 28
- 230000008859 change Effects 0.000 claims abstract description 20
- 239000011521 glass Substances 0.000 claims abstract description 17
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- 238000006243 chemical reaction Methods 0.000 claims description 50
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- 230000000996 additive effect Effects 0.000 claims description 3
- 230000004580 weight loss Effects 0.000 claims 3
- 238000006298 dechlorination reaction Methods 0.000 abstract description 19
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- 229910052801 chlorine Inorganic materials 0.000 description 22
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 21
- 238000005259 measurement Methods 0.000 description 15
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 14
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- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 12
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- -1 clothing Substances 0.000 description 10
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 9
- 239000010936 titanium Substances 0.000 description 8
- 229910010413 TiO 2 Inorganic materials 0.000 description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
- 239000003989 dielectric material Substances 0.000 description 7
- 229910001873 dinitrogen Inorganic materials 0.000 description 7
- 239000000975 dye Substances 0.000 description 7
- 238000009434 installation Methods 0.000 description 7
- 229910052760 oxygen Inorganic materials 0.000 description 7
- 239000001301 oxygen Substances 0.000 description 7
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 7
- 239000004810 polytetrafluoroethylene Substances 0.000 description 7
- 238000004458 analytical method Methods 0.000 description 6
- 238000000149 argon plasma sintering Methods 0.000 description 6
- 239000000919 ceramic Substances 0.000 description 6
- 239000013078 crystal Substances 0.000 description 6
- 238000001035 drying Methods 0.000 description 6
- 230000002776 aggregation Effects 0.000 description 5
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- 239000001257 hydrogen Substances 0.000 description 5
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- 229910052719 titanium Inorganic materials 0.000 description 4
- 238000004438 BET method Methods 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- 238000004220 aggregation Methods 0.000 description 3
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- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
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- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- KPZGRMZPZLOPBS-UHFFFAOYSA-N 1,3-dichloro-2,2-bis(chloromethyl)propane Chemical compound ClCC(CCl)(CCl)CCl KPZGRMZPZLOPBS-UHFFFAOYSA-N 0.000 description 1
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 1
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- 125000004429 atom Chemical group 0.000 description 1
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 1
- 229910002113 barium titanate Inorganic materials 0.000 description 1
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- 238000010899 nucleation Methods 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 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
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- 239000004065 semiconductor Substances 0.000 description 1
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 description 1
- 235000019982 sodium hexametaphosphate Nutrition 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 239000002352 surface water Substances 0.000 description 1
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 description 1
- 229910000348 titanium sulfate Inorganic materials 0.000 description 1
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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
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
- A61K8/29—Titanium; Compounds 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
- B01J21/063—Titanium; Oxides or hydroxides thereof
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- 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
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- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
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- C01P2006/12—Surface area
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- 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
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Abstract
Description
BET, m2/g | LOI 측정후 BET, m2/g | 900℃ -1hr의 LOI 이론치, 질량% | LOI 실험치, 질량% | LOI 이론치, *0.85 질량% | LOI 이론치, *1.5 질량% | LOI 이론치, *0.25 질량% | LOI 이론치, *2.1 질량% | 20℃,80%RH에서5시간정치전의질량을기준으로한변화율, 질량% | |
실시예1 | 107 | 6 | 4.73 | 5.00 | 4.02 | 7.09 | 1.18 | 9.92 | 2.3 |
실시예2 | 158 | 3.5 | 7.06 | 6.50 | 6.00 | 10.59 | 1.76 | 14.82 | 3.6 |
실시예3 | 12 | 5 | 0.47 | 0.37 | 0.40 | 0.70 | 0.12 | 0.98 | 0.12 |
실시예4 | 50 | 5.6 | 2.17 | 2.40 | 1.84 | 3.25 | 0.54 | 4.55 | 1.8 |
실시예5 | 30 | 5.2 | 1.27 | 1.25 | 1.08 | 1.91 | 0.32 | 2.67 | 1.0 |
실시예6 | 107 | 6.1 | 4.73 | 6.75 | 4.02 | 7.09 | 1.18 | 9.92 | 1.4 |
실시예7 | 50 | 5.2 | 2.17 | 3.14 | 1.84 | 3.25 | 0.54 | 4.55 | 0.83 |
실시예8 | 30 | 5 | 1.27 | 1.52 | 1.08 | 1.91 | 0.32 | 2.67 | 0.74 |
비교예1 | 6 | 5 | 0.20 | 0.60 | 0.17 | 0.29 | 0.05 | 0.41 | 6.0 |
비교예2 | 60 | 5.1 | 2.62 | 5.60 | 2.23 | 3.94 | 0.66 | 5.51 | 9.0 |
Claims (27)
- 2~5g의 이산화티탄 분말을 지름 10㎝의 유리제 페트리디쉬에 균일한 두께로 스프레드하고, 20℃, 상대습도 80%의 환경에서 5시간 동안 정치시킨 경우, 정치 전의 질량을 기준으로 질량의 변화율이 -5질량%~5질량%인 것을 특징으로 하는 10~200 m2/g의 BET 비표면적을 갖는 미립자 이산화티탄.
- 제1항에 있어서, 90% 누적질량 입자크기 분포 직경(이하, "D90"이라 함)이 2.2㎛ 이하인 것을 특징으로 하는 미립자 이산화티탄.
- 제1항 또는 제2항에 있어서, 하기 일반식(1)으로 표시되는 로진-람러 식에 따른 분포상수 n이 1.7~3.5인 것을 특징으로 하는 미립자 이산화티탄:R=100exp(-bDn) (1)(여기서, D는 입자 직경이고, R은 전체 입자의 질량을 기준으로 D(입자 직경)보다 큰 입자의 질량 퍼센트이며, n은 분포상수이다.)
- BET 비표면적이 α(m2/g)이고, 분말을 900℃로 유지한 전기로에서 1시간 동안 연소시킨 경우의 질량감소(이후, 작열감량이라 함)가 X(질량%)라고 하면, 상기 작열감량 X가 일반식(2)으로 표시되는 범위 내에 존재하는 것을 특징으로 하는 미 립자 이산화티탄:2.1×{α/(6×104)×18+(α-β)/(6×104)×9}×100≥X≥0.25×{α/(6×104)×18+(α-β)/(6×104)×9}×100 (2)(여기서, β는 900℃로 유지한 전기로에서 1시간 동안 분말을 연소시킨 후의 BET 비표면적 (m2/g)이다.)
- BET 비표면적이 α(m2/g)이고, 상기 분말을 900℃로 유지한 전기로에서 1시간 동안 연소시킨 경우의 질량감소(이후, 작열감량이라 함)가 X(질량%)라고 하면, 상기 작열감량 X가 일반식(2')으로 표시되는 범위 내에 존재하는 것을 특징으로 하는 미립자 이산화티탄:1.3×{α/(6×104)×18+(α-β)/(6×104)×9}×100≥X≥0.7×{α/(6×104)×18+(α-β)/(6×104)×9}×100 (2')(여기서, β는 900℃로 유지한 전기로에서 1시간 동안 분말을 연소시킨 후의 BET 비표면적 (m2/g)이다.)
- BET 비표면적이 α(m2/g)이고, 분말을 900℃로 유지한 전기로에서 1시간 동안 연소시킨 경우의 질량감소(이후, 작열감량이라 함)가 X(질량%)라고 하면, 상기 작열감량 X가 일반식(3)으로 표시되는 범위 내에 존재하는 것을 특징으로 하는 미립자 이산화티탄:1.5×{α/(6×104)×18+(α-β)/(6×104)×9}×100≥X≥0.85×{α/(6×104)×18+(α-β)/(6×104)×9}×100 (3)(여기서, β는 900℃로 유지한 전기로에서 1시간 동안 분말을 연소시킨 후의 BET 비표면적 (m2/g)이다.)
- BET 비표면적이 α(m2/g)이고, 분말을 900℃로 유지한 전기로에서 1시간 동안 연소시킨 경우의 질량감소(이후, 작열감량이라 함)가 X(질량%)라고 하면, 상기 작열감량 X가 일반식(3')으로 표시되는 범위 내에 존재하는 것을 특징으로 하는 미립자 이산화티탄:1.15×{α/(6×104)×18+(α-β)/(6×104)×9}×100≥X≥0.85×{α/(6×104)×18+(α-β)/(6×104)×9}×100 (3')(여기서, β는 900℃로 유지한 전기로에서 1시간 동안 분말을 연소시킨 후의 BET 비표면적 (m2/g)이다.)
- 제1항, 제4항 내지 제7항 중 어느 한 항에 있어서, Fe, Al 및 S의 함량이 각각 10질량ppm 이하인 것을 특징으로 하는 미립자 이산화티탄.
- 제1항, 제4항 내지 제7항 중 어느 한 항에 있어서, 상기 분체 중의 Cl의 함량이 작열감량의 50질량% 이하인 것을 특징으로 하는 미립자 이산화티탄.
- 사염화티탄 함유 가스를 산화성 가스를 사용하여 고온 산화하여 이산화티탄 분말을 제조하는 제1단계와, 가열로에서 상기 분말을 롤링하면서 수증기를 상기 이산화티탄 분말과 접촉시켜서 탈염소화를 행하는 동시에 흡착수를 증가시키는 제2단계를 포함하는 것을 특징으로 하는 미립자 이산화티탄의 제조방법.
- 제10항에 있어서, 상기 산화성 가스는 수증기인 것을 특징으로 하는 미립자 이산화티탄의 제조방법.
- 제11항에 있어서, 상기 접촉되는 수증기의 양은 사염화티탄 가스의 몰당 2~30몰인 것을 특징으로 하는 미립자 이산화티탄의 제조방법.
- 제10항 내지 제12항 중 어느 한 항에 있어서, 반응관에 공급되는 상기 사염화티탄 함유 가스 및 산화성 가스는 각각 600℃~1,100℃ 미만의 온도에서 예열되는 것을 특징으로 하는 미립자 이산화티탄의 제조방법.
- 제10항에 있어서, 상기 제2단계에서, 가열로에 이산화티탄 분말을 기준으로 1~60질량%의 비율로 수증기를 도입하여 상기 수증기와 상기 분체를 향류 접촉시키는 것을 특징으로 하는 미립자 이산화티탄의 제조방법.
- 제10항에 있어서, 상기 제2단계에서, 가열로에 이산화티탄 분말을 기준으로 1~50질량%의 비율이 되도록 수증기를 도입하여 상기 수증기와 상기 분체를 향류 접촉시키는 것을 특징으로 하는 미립자 이산화티탄의 제조방법.
- 제10항에 있어서, 상기 제2단계에서 상기 이산화티탄을 150℃~500℃에서 가열하는 것을 특징으로 하는 미립자 이산화티탄의 제조방법.
- 제10항에 있어서, 상기 제2단계에서 상기 분말의 가열로 내에서의 체류시간이 0.5시간~3시간 미만인 것을 특징으로 하는 미립자 이산화티탄의 제조방법.
- 분말을 수지포대에 패킹할 때, 액적직경이 5~500㎛인 수적을 분무하고, 봉합한 다음, 상기 포대를 보관하는 단계를 포함하는 것을 특징으로 하는 미립자 이산화티탄의 제조방법.
- 삭제
- 제1항, 제4항 내지 제7항 중 어느 한 항에 기재된 미립자 이산화티탄을 원료의 일부로서 사용하는 것을 특징으로 하는 페로브스카이트 화합물.
- 제1항, 제4항 내지 제7항 중 어느 한 항에 기재된 이산화티탄 분말을 함유하는 것을 특징으로 하는 유전체 원료.
- 제1항, 제4항 내지 제7항 중 어느 한 항에 기재된 이산화티탄 분말을 함유하는 것을 특징으로 하는 슬러리.
- 제1항, 제4항 내지 제7항 중 어느 한 항에 기재된 이산화티탄 분말을 함유하는 것을 특징으로 하는 조성물.
- 제1항, 제4항 내지 제7항 중 어느 한 항에 기재된 이산화티탄 분말을 함유하는 것을 특징으로 하는 광촉매 재료.
- 제1항, 제4항 내지 제7항 중 어느 한 항에 기재된 이산화티탄 분말을 함유하는 것을 특징으로 하는 화장료.
- 제1항, 제4항 내지 제7항 중 어느 한 항에 기재된 이산화티탄 분말을 함유하는 것을 특징으로 하는 태양전지 재료.
- 제1항, 제4항 내지 제7항 중 어느 한 항에 기재된 이산화티탄 분말을 함유하는 것을 특징으로 하는 실리콘 고무용 첨가제.
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