KR100674496B1 - 초미세 기공을 갖는 다공성의 나노 미립자 이산화티탄광촉매 및 안료의 제조방법 - Google Patents
초미세 기공을 갖는 다공성의 나노 미립자 이산화티탄광촉매 및 안료의 제조방법 Download PDFInfo
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- KR100674496B1 KR100674496B1 KR1020050024260A KR20050024260A KR100674496B1 KR 100674496 B1 KR100674496 B1 KR 100674496B1 KR 1020050024260 A KR1020050024260 A KR 1020050024260A KR 20050024260 A KR20050024260 A KR 20050024260A KR 100674496 B1 KR100674496 B1 KR 100674496B1
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- KR
- South Korea
- Prior art keywords
- titanium dioxide
- nano
- weight
- photocatalyst
- porous
- Prior art date
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 367
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 158
- 239000011148 porous material Substances 0.000 title claims abstract description 99
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 96
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 75
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims description 16
- 239000000049 pigment Substances 0.000 title abstract description 15
- 239000002245 particle Substances 0.000 claims abstract description 53
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000013078 crystal Substances 0.000 claims abstract description 30
- 239000000843 powder Substances 0.000 claims abstract description 20
- 239000003381 stabilizer Substances 0.000 claims abstract description 5
- 239000002002 slurry Substances 0.000 claims description 39
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 28
- 238000006386 neutralization reaction Methods 0.000 claims description 26
- 238000010304 firing Methods 0.000 claims description 25
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 claims description 25
- 239000010936 titanium Substances 0.000 claims description 20
- 239000003973 paint Substances 0.000 claims description 19
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 16
- 238000001914 filtration Methods 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 16
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 claims description 16
- 229910000348 titanium sulfate Inorganic materials 0.000 claims description 16
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 12
- 239000000706 filtrate Substances 0.000 claims description 12
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 12
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- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 8
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 8
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- 238000003756 stirring Methods 0.000 claims description 7
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- 239000011701 zinc Substances 0.000 claims description 6
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- 239000002253 acid Substances 0.000 claims description 5
- 239000012535 impurity Substances 0.000 claims description 5
- 229910052742 iron Inorganic materials 0.000 claims description 5
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 5
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- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 4
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- HDUMBHAAKGUHAR-UHFFFAOYSA-J titanium(4+);disulfate Chemical compound [Ti+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O HDUMBHAAKGUHAR-UHFFFAOYSA-J 0.000 claims description 4
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- VGIBGUSAECPPNB-UHFFFAOYSA-L nonaaluminum;magnesium;tripotassium;1,3-dioxido-2,4,5-trioxa-1,3-disilabicyclo[1.1.1]pentane;iron(2+);oxygen(2-);fluoride;hydroxide Chemical compound [OH-].[O-2].[O-2].[O-2].[O-2].[O-2].[F-].[Mg+2].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[K+].[K+].[K+].[Fe+2].O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2 VGIBGUSAECPPNB-UHFFFAOYSA-L 0.000 claims description 3
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- 125000002924 primary amino group Chemical class [H]N([H])* 0.000 claims description 3
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- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 2
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- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- UCNNJGDEJXIUCC-UHFFFAOYSA-L hydroxy(oxo)iron;iron Chemical compound [Fe].O[Fe]=O.O[Fe]=O UCNNJGDEJXIUCC-UHFFFAOYSA-L 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 238000003905 indoor air pollution Methods 0.000 description 1
- IXQWNVPHFNLUGD-UHFFFAOYSA-N iron titanium Chemical compound [Ti].[Fe] IXQWNVPHFNLUGD-UHFFFAOYSA-N 0.000 description 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 1
- YDZQQRWRVYGNER-UHFFFAOYSA-N iron;titanium;trihydrate Chemical compound O.O.O.[Ti].[Fe] YDZQQRWRVYGNER-UHFFFAOYSA-N 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- CAAULPUQFIIOTL-UHFFFAOYSA-N methyl dihydrogen phosphate Chemical compound COP(O)(O)=O CAAULPUQFIIOTL-UHFFFAOYSA-N 0.000 description 1
- 239000011859 microparticle Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen 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
- 230000000149 penetrating effect Effects 0.000 description 1
- DLYUQMMRRRQYAE-UHFFFAOYSA-N phosphorus pentoxide Inorganic materials O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 230000021715 photosynthesis, light harvesting Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 description 1
- 229910001950 potassium oxide Inorganic materials 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000002250 progressing effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 208000023504 respiratory system disease Diseases 0.000 description 1
- 208000013220 shortness of breath Diseases 0.000 description 1
- 208000008842 sick building syndrome Diseases 0.000 description 1
- UKHWJBVVWVYFEY-UHFFFAOYSA-M silver;hydroxide Chemical compound [OH-].[Ag+] UKHWJBVVWVYFEY-UHFFFAOYSA-M 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- JBQYATWDVHIOAR-UHFFFAOYSA-N tellanylidenegermanium Chemical compound [Te]=[Ge] JBQYATWDVHIOAR-UHFFFAOYSA-N 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical compound O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 description 1
- 229910001935 vanadium oxide Inorganic materials 0.000 description 1
- 239000004034 viscosity adjusting agent Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000004246 zinc acetate Substances 0.000 description 1
- UGZADUVQMDAIAO-UHFFFAOYSA-L zinc hydroxide Chemical compound [OH-].[OH-].[Zn+2] UGZADUVQMDAIAO-UHFFFAOYSA-L 0.000 description 1
- 229940007718 zinc hydroxide Drugs 0.000 description 1
- 229910021511 zinc hydroxide Inorganic materials 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
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Abstract
Description
구 분 | 실시예 2 | 실시예 3 | 실시예 4 | 실시예 5 | 실시예 6 | 실시예 7 |
비표면적 | 326 | 185 | 100 | 46 | 19 | 9 |
구 분 | 황산이온(SO3)의 함량(%) |
비교예 1 | 15 |
실시예 8 | 3.0 |
실시예 9 | 1.2 |
실시예 10 | 0.3(300ppm) |
실시예 11 | 0.07(70ppm) |
항 균 실 험 | ||
균종 | 경과시간(시간) | 세균감소율(%) |
대장균 | 초기 | 0 |
12 | 100 | |
황색포도상구균 | 초기 | 0 |
12 | 100 |
시험항목 | TiO2함량(%) | 5분 | 15분 | 30분 | 60분 |
탈취율(%) | 20 | 72.0 | 84.0 | 85.0 | 87.0 |
30 | 74.5 | 86.4 | 88.0 | 90.4 |
시험항목 | TiO2함량(%) | 6시간 | 12시간 | 24시간 |
NO제거율(%) | 30 | 75.0 | 94.0 | 98.0 |
NO2제거율(%) | 30 | 74.3 | 89.7 | 95.4 |
SO2제거율(%) | 30 | 72.2 | 87.0 | 94.0 |
실험항목 | 초기 | 30분 | 60분 | 90분 | 120분 |
탈취율(%) | 0 | 73.4 | 92.4 | 98.7 | 100 |
실험항목 | 초기 | 1분 | 10분 | 30분 | 60분 |
포름알데히드감소율(%) | 0 | 37.4 | 68.7 | 94.7 | 99.8 |
실험항목 | 초기 | 12시간 | 24시간 |
대장균 살균율(%) | 0 | 88.7 | 99.9 |
황색포도상구균 살균율(%) | 0 | 87.9 | 99.9 |
구 분 | 경과시간(분) | 블랭크 농도(ppm) | 시료농도(ppm) | 탈취율(%) |
탈취 실험 | 초기 | 500 | 500 | 0 |
30 | 494 | 9.9 | 98 | |
60 | 486 | 4.9 | 99 | |
90 | 472 | 4.7 | 99 | |
120 | 460 | 4.6 | 99 |
시 간 | 1분 | 10분 | 30분 | 60분 |
분해효율 | 30% | 75% | 95% | 100% |
실험균명 | 실험 시료 | 실험시작전 (개/㎖) | 12시간 후 (개/㎖) | 세균감소율(%) |
대장균 | 대조군 | 3.5*105 | 3.0*107 | - |
실시예 2 | 3.5*105 | <10 | <99.9% | |
황색포도상구균 | 대조군 | 1.9*105 | 9*105 | - |
실시예 2 | 1.9*105 | <10 | <99.9% |
Claims (13)
- 입자 내부에 중심 기공의 지름이 0.01 내지 5㎚의 기공을 갖는, 아나타제형의 이산화티탄으로 이루어짐을 특징으로 하는 나노 크기의 기공을 갖는 다공성의 이산화티탄 광촉매.
- 이산화티탄의 제조에 있어서,(1) 건조 분쇄된 티탄원광에 80 내지 95% 농도의 황산(H2SO4)을 중량비로 1.5 내지 3.0배 혼합하여 반응을 시켜 용해된 황산티탄용액을 만드는 용해단계;(2) 상기 용해단계에서 수득된 황산티탄용액(티타닐황산)을 침강조에서 청등화하여 불용해 잔분을 침전시켜 청등액만 여과하고, 황산티탄용액을 0 내지 -5℃의 온도범위로 냉각하여 황산티타늄용액 중에 함유되어 있는 황산제1철(FeSO4.7H2O)을 생성시켜 이것을 원심분리기를 통하여 결정을 분리한 후 여과시키는 여과단계;(3) 상기 여과단계에서 수득된 황산티탄 청등여액에 물을 중량비로 2.0 내지 3.0배수로 가하여 가수분해하면 백색유탁의 수산화티탄 미립자를 생성시키는 가수분해단계;(4) 상기 가수분해단계에서 생성되는 수산화티탄산 여액에 염기로서 암모니아수, 중탄산암모늄을 가하여 중성으로 중화시키는 중화단계;(5) 상기 중화단계에서 수득된 침전물을 물로 세척하여 수산화티탄산 슬러리에 함유된 황산, 가용성불순물 즉 철분, 기타 성분을 필터로 여과하여 제거하는 세척단계; 및(6) 상기 수득된 이산화티탄 슬러리를 50 내지 100℃의 온도에서 10 내지 30시간 동안 수열시켜 다공성의 결정상으로 전이시키는 전이단계;들을 포함하여 이루어짐을 특징으로 하는 나노 크기의 기공을 갖는 다공성의 이산화티탄 광촉매의 제조방법.
- 제 2 항에 있어서,상기 전이단계 이후에 수득된 이산화티탄 슬러리를 압착하여 수분을 제거하고, 100 내지 1,200℃의 온도로 가열하여 소성시키는 소성단계를 더 포함하여 이루어짐을 특징으로 하는 나노 크기의 기공을 갖는 다공성의 이산화티탄 광촉매의 제조방법.
- 제 2 항에 있어서,상기 중화단계 이후에 아세트산아연(zinc acetate dihydrate ; Zn(CH3COO)2ㆍ2H2O), 소듐실리케이트 용액(sodium silicate solution ; Na2OㆍnSiO2ㆍxH2O) 또는 질산은(silver nitrate ; AgNO3)를 첨가하여 금속이온을 담지시키는 담지단계를 더 포함하여 이루어짐을 특징으로 하는 나노 크기의 기공을 갖는 다공성의 이산화티탄 광촉매의 제조방법.
- 삭제
- 삭제
- 삭제
- 상기 청구항 제 2 항에 따라 수득되는 나노 크기의 기공을 갖는 수열반응 시킨 다공성의 이산화티탄 슬러리에 통상의 도료 조성물의 제조를 위하여 사용되는 수용성 바인더수지와 물을 혼합하여 이루어짐을 특징으로 하는 나노 크기의 기공을 갖는 다공성의 이산화티탄 광촉매를 포함하는 도료.
- 제 8 항에 있어서,상기 청구항 제 2 항에 따라 수득되는 나노 크기의 기공을 갖는 수열반응 시킨 다공성의 이산화티탄 슬러리 100중량부, 수용성 에멀션 아크릴 중합체 5 내지 15중량부, 수용성 우레탄 수지 1 내지 10중량부, 실리카-졸(silica-Sol) 10 내지 20중량부, 소포제 0.1 내지 0.5중량부, 폴리카르복실산형 분산제 0.1 내지 0.5중량부들을 포함하여 이루어짐을 특징으로 하는 나노 크기의 기공을 갖는 다공성의 이산화티탄 광촉매를 포함하는 도료.
- 제 9 항에 있어서,착색제로서 무기계 안료 0.1 내지 5.0중량%, pH조절제로서 제1급 아민 0.1 내지 3.0중량%, 동결안정제로서 에틸렌글리콜 3 내지 10중량%를 더 포함하여 이루어짐을 특징으로 하는 나노 크기의 기공을 갖는 다공성의 이산화티탄 광촉매를 포함하는 도료.
- 제 9 항 또는 제 10 항에 있어서,전기석, 일라이트, 도석, 석회석, 규석, 황토, 맥반석, 옥분말, 제올라이트, 활성탄, 활성점토, 코디어라이트, 알루미나 또는 이들 중 2이상의 혼합물로 이루어지는 그룹으로부터 선택되는 음이온 및 원적외선을 방출하는 광물분말이 상기 도료 총량을 기준으로 10 내지 90중량%의 양으로 더 포함되어 이루어짐을 특징으로 하는 나노 크기의 기공을 갖는 다공성의 이산화티탄 광촉매를 포함하는 도료.
- 삭제
- (1) 수용성 에멀션 아크릴 중합체 5 내지 15중량부, 수용성 우레탄 수지 1 내지 10중량부, 실리카-졸(silica-Sol) 10 내지 20중량부, 소포제 0.1 내지 0.5중량부, 폴리카르복실산형 분산제 0.1 내지 0.5중량부를 모두 혼합하고, 700rpm으로 15분간 교반하는 제1혼합단계; 및(2) 상기 청구항 제 2 항에 따라 수득되는 나노 크기의 기공을 갖는 수열반응 시킨 다공성의 이산화티탄 슬러리 100중량부를 첨가하고, 1,500 내지 2,500rpm으로 10 내지 30분간 고속 교반하는 제2혼합단계;들을 포함하여 이루어짐을 특징으로 하는 나노 크기의 기공을 갖는 다공성의 이산화티탄 광촉매를 포함하는 도료.
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Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
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KR100913622B1 (ko) | 2007-12-28 | 2009-08-26 | 포항공과대학교 산학협력단 | 수소 생성용 메조다공성 이산화티타늄 광촉매의 제조방법 |
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KR100913622B1 (ko) | 2007-12-28 | 2009-08-26 | 포항공과대학교 산학협력단 | 수소 생성용 메조다공성 이산화티타늄 광촉매의 제조방법 |
WO2011050141A3 (en) * | 2009-10-24 | 2011-09-15 | Nanoscale Corporation | Remediation of undesirable substances from enclosed spaces and monitoring of contaminants |
KR101247161B1 (ko) | 2012-12-07 | 2013-03-25 | 김윤환 | 새집증후군 제거용 나노산소 촉매제 제조방법 |
KR101328657B1 (ko) | 2012-12-07 | 2013-11-14 | 김윤환 | 새집증후군 제거용 나노산소 촉매제 |
KR101247162B1 (ko) | 2012-12-20 | 2013-03-25 | 김윤환 | 정전기 방지 cnt를 함유한 새집증후군 제거용 나노산소 촉매제 제조방법 |
CN110586930A (zh) * | 2019-10-22 | 2019-12-20 | 广东银纳科技有限公司 | 一种防腐用纳米钛材料的制备方法 |
CN110586930B (zh) * | 2019-10-22 | 2022-01-14 | 广东银纳科技有限公司 | 一种防腐用纳米钛材料的制备方法 |
KR20220132067A (ko) * | 2021-03-22 | 2022-09-30 | 한림대학교 산학협력단 | 질소-이산화티타늄 나노 결정체의 제조방법 및 이에 의해 제조된 질소-이산화티타늄 나노 결정체 |
KR102507162B1 (ko) | 2021-03-22 | 2023-03-08 | 한림대학교 산학협력단 | 질소-이산화티타늄 나노 결정체의 제조방법 및 이에 의해 제조된 질소-이산화티타늄 나노 결정체 |
KR20220142803A (ko) | 2021-04-15 | 2022-10-24 | 정용주 | 미세유리 중공구를 포함하는 항균 도료조성물 |
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