CN109675590A - A kind of preparation method of titanium dioxide - Google Patents
A kind of preparation method of titanium dioxide Download PDFInfo
- Publication number
- CN109675590A CN109675590A CN201710972609.9A CN201710972609A CN109675590A CN 109675590 A CN109675590 A CN 109675590A CN 201710972609 A CN201710972609 A CN 201710972609A CN 109675590 A CN109675590 A CN 109675590A
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- CN
- China
- Prior art keywords
- titanium dioxide
- oxide
- glass
- powder
- glass powder
- 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 318
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 155
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 239000000843 powder Substances 0.000 claims abstract description 130
- 239000000075 oxide glass Substances 0.000 claims abstract description 65
- 229910003439 heavy metal oxide Inorganic materials 0.000 claims abstract description 61
- 239000002131 composite material Substances 0.000 claims abstract description 34
- 239000002994 raw material Substances 0.000 claims abstract description 29
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 25
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 21
- 239000011521 glass Substances 0.000 claims description 117
- 229910052751 metal Inorganic materials 0.000 claims description 26
- 239000002184 metal Substances 0.000 claims description 26
- 239000000428 dust Substances 0.000 claims description 23
- UZLYXNNZYFBAQO-UHFFFAOYSA-N oxygen(2-);ytterbium(3+) Chemical compound [O-2].[O-2].[O-2].[Yb+3].[Yb+3] UZLYXNNZYFBAQO-UHFFFAOYSA-N 0.000 claims description 17
- 229910003454 ytterbium oxide Inorganic materials 0.000 claims description 17
- 229940075624 ytterbium oxide Drugs 0.000 claims description 17
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 14
- 229910000464 lead oxide Inorganic materials 0.000 claims description 13
- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical compound [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 claims description 13
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 12
- VQCBHWLJZDBHOS-UHFFFAOYSA-N erbium(iii) oxide Chemical compound O=[Er]O[Er]=O VQCBHWLJZDBHOS-UHFFFAOYSA-N 0.000 claims description 10
- YBMRDBCBODYGJE-UHFFFAOYSA-N germanium oxide Inorganic materials O=[Ge]=O YBMRDBCBODYGJE-UHFFFAOYSA-N 0.000 claims description 8
- PVADDRMAFCOOPC-UHFFFAOYSA-N oxogermanium Chemical compound [Ge]=O PVADDRMAFCOOPC-UHFFFAOYSA-N 0.000 claims description 8
- 229910052714 tellurium Inorganic materials 0.000 claims description 8
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 claims description 8
- 229910052788 barium Inorganic materials 0.000 claims description 7
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims description 7
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Inorganic materials [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 claims description 7
- CSSYLTMKCUORDA-UHFFFAOYSA-N barium(2+);oxygen(2-) Chemical compound [O-2].[Ba+2] CSSYLTMKCUORDA-UHFFFAOYSA-N 0.000 claims description 7
- 229910052810 boron oxide Inorganic materials 0.000 claims description 7
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims description 7
- 229910000416 bismuth oxide Inorganic materials 0.000 claims description 6
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 claims description 6
- 239000000395 magnesium oxide Substances 0.000 claims description 6
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims description 6
- MMKQUGHLEMYQSG-UHFFFAOYSA-N oxygen(2-);praseodymium(3+) Chemical compound [O-2].[O-2].[O-2].[Pr+3].[Pr+3] MMKQUGHLEMYQSG-UHFFFAOYSA-N 0.000 claims description 6
- 229910003447 praseodymium oxide Inorganic materials 0.000 claims description 6
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims description 6
- 229910001948 sodium oxide Inorganic materials 0.000 claims description 6
- 229910003451 terbium oxide Inorganic materials 0.000 claims description 6
- SCRZPWWVSXWCMC-UHFFFAOYSA-N terbium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Tb+3].[Tb+3] SCRZPWWVSXWCMC-UHFFFAOYSA-N 0.000 claims description 6
- XHGGEBRKUWZHEK-UHFFFAOYSA-L tellurate Chemical compound [O-][Te]([O-])(=O)=O XHGGEBRKUWZHEK-UHFFFAOYSA-L 0.000 claims description 3
- 238000005352 clarification Methods 0.000 claims 2
- 229910052732 germanium Inorganic materials 0.000 claims 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 25
- 238000007146 photocatalysis Methods 0.000 abstract description 16
- 241000894006 Bacteria Species 0.000 abstract description 9
- 239000003344 environmental pollutant Substances 0.000 abstract description 5
- 231100000719 pollutant Toxicity 0.000 abstract description 5
- 230000006798 recombination Effects 0.000 abstract description 4
- 238000005215 recombination Methods 0.000 abstract description 4
- 238000005253 cladding Methods 0.000 abstract description 2
- 235000010215 titanium dioxide Nutrition 0.000 description 137
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical compound C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 description 23
- 229910003472 fullerene Inorganic materials 0.000 description 21
- 238000000137 annealing Methods 0.000 description 20
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 20
- 238000001354 calcination Methods 0.000 description 19
- 238000000034 method Methods 0.000 description 18
- 238000012360 testing method Methods 0.000 description 15
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 13
- 229940043267 rhodamine b Drugs 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 11
- 229910052697 platinum Inorganic materials 0.000 description 10
- 238000000227 grinding Methods 0.000 description 9
- 238000012545 processing Methods 0.000 description 9
- 239000000243 solution Substances 0.000 description 9
- 150000001875 compounds Chemical class 0.000 description 8
- 238000005192 partition Methods 0.000 description 8
- 230000008569 process Effects 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 239000004411 aluminium Substances 0.000 description 7
- 229910052782 aluminium Inorganic materials 0.000 description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 7
- 230000000640 hydroxylating effect Effects 0.000 description 7
- 238000002156 mixing Methods 0.000 description 7
- 238000000465 moulding Methods 0.000 description 7
- -1 terbium ion Chemical class 0.000 description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 239000011449 brick Substances 0.000 description 6
- 238000004140 cleaning Methods 0.000 description 6
- 230000005284 excitation Effects 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000000155 melt Substances 0.000 description 5
- 239000002957 persistent organic pollutant Substances 0.000 description 5
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 5
- 229910052724 xenon Inorganic materials 0.000 description 5
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 4
- 230000000844 anti-bacterial effect Effects 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 238000000354 decomposition reaction Methods 0.000 description 4
- 239000008187 granular material Substances 0.000 description 4
- 230000005283 ground state Effects 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 229910052761 rare earth metal Inorganic materials 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000000725 suspension Substances 0.000 description 4
- 239000010936 titanium Substances 0.000 description 4
- 229910052719 titanium Inorganic materials 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910052691 Erbium Inorganic materials 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 229910052771 Terbium Inorganic materials 0.000 description 3
- 238000002835 absorbance Methods 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 239000011941 photocatalyst Substances 0.000 description 3
- WCWKKSOQLQEJTE-UHFFFAOYSA-N praseodymium(3+) Chemical compound [Pr+3] WCWKKSOQLQEJTE-UHFFFAOYSA-N 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 230000007704 transition Effects 0.000 description 3
- 230000005472 transition radiation Effects 0.000 description 3
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical group CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 229910052769 Ytterbium Inorganic materials 0.000 description 2
- HGWOWDFNMKCVLG-UHFFFAOYSA-N [O--].[O--].[Ti+4].[Ti+4] Chemical compound [O--].[O--].[Ti+4].[Ti+4] HGWOWDFNMKCVLG-UHFFFAOYSA-N 0.000 description 2
- 239000008346 aqueous phase Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000003115 biocidal effect Effects 0.000 description 2
- 239000013590 bulk material Substances 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 239000000839 emulsion Substances 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 238000007496 glass forming Methods 0.000 description 2
- 230000031700 light absorption Effects 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 150000003254 radicals Chemical class 0.000 description 2
- 238000006479 redox reaction Methods 0.000 description 2
- 239000013049 sediment Substances 0.000 description 2
- 238000004088 simulation Methods 0.000 description 2
- 238000007619 statistical method Methods 0.000 description 2
- VDZOOKBUILJEDG-UHFFFAOYSA-M tetrabutylammonium hydroxide Chemical compound [OH-].CCCC[N+](CCCC)(CCCC)CCCC VDZOOKBUILJEDG-UHFFFAOYSA-M 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 241000790917 Dioxys <bee> Species 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 238000010220 Pearson correlation analysis Methods 0.000 description 1
- 241000227425 Pieris rapae crucivora Species 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 230000003373 anti-fouling effect Effects 0.000 description 1
- 230000000845 anti-microbial effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 238000000295 emission spectrum Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000001023 inorganic pigment Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000320 mechanical mixture Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 230000002335 preservative effect Effects 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 230000004043 responsiveness Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000005368 silicate glass Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
Classifications
-
- 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/057—Selenium or tellurium; Compounds thereof
- B01J27/0576—Tellurium; 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- 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
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/18—Arsenic, antimony or bismuth
-
- 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/38—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of titanium, zirconium or hafnium
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C12/00—Powdered glass; Bead compositions
-
- 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
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Glass Compositions (AREA)
- Catalysts (AREA)
Abstract
The present invention relates to a kind of preparation methods of titanium dioxide, it is characterized in that, by industrial titanium dioxide: the mass ratio of heavy metal oxide glass powder=(40-60): (40-60) prepares composite titanium dioxide powder and is uniformly mixed the composite titanium dioxide powder;Wherein, the raw material of the heavy metal oxide glass powder includes the sensitized fluorescence agent of heavy metallic oxide and quality for the 1-2% of the heavy metallic oxide gross mass.The invention enables titanium dioxide, and cladding shell to be used as to be fixed on heavy metal oxide glass powder surface, both it ensure that titanium dioxide can adequately be contacted with bacterium or pollutant, the recombination rate for reducing titanium dioxide photoproduction electrons and holes again improves the photocatalysis performance of titanium dioxide.
Description
Technical field
The present invention relates to field of chemical raw material preparation more particularly to a kind of preparation methods of titanium dioxide.
Background technique
Titanium dioxide is a kind of at present in the common white inorganic pigment of industrial circle, with whiteness is high, covering power is good,
Glossiness is high, mechanical strength is good, chemical the features such as stablizing with macroscopic property, thus is widely used in coating, plastics, makes
The numerous areas such as paper, printing ink, chemical fibre, rubber, cosmetics.In addition, from the photocatalytic effect of titanium dioxide in 1979 by day
Since two scholars' discoveries of this Fujishima and Honda, using the photocatalytic activity of titanium dioxide carry out it is antifouling, antibacterial, remove
The technology of smelly, air cleaning, water pollution processing and environmental pollution improvement etc. is also rapidly developed.
After by the excitation of the light of ultraviolet wavelength, the electronics in valence band is excited titanium dioxide, crosses forbidden band and enters conduction band,
Corresponding hole is generated in valence band simultaneously.These light induced electrons and photohole move to the different positions of titanium dioxide surface
It sets, and the oxygen and water that can and contact with titanium dioxide surface react, generates the peroxy radical or hydroxyl with high activity
Base free radical.These free radicals can decompose the organic compounds such as the organic microbials such as bacterium or formaldehyde.Therefore, have both high whiteness
With the titanium dioxide of highlight catalytic active, can be used for preparing has antibacterial and the new coating of self-cleaning function, chemical fibre, modeling
Expect the multiple material and product of profile and paper, ink etc..
For example, the patent of Publication No. CN105885557A discloses a kind of antibiosis and self-cleaning coating for wall surface, black is utilized
The photocatalytic effect of nano-titanium dioxide and rutile type nano titanic oxide, so that there is coating for wall surface significant photocatalysis to kill
Bacterium self-cleaning function.The patent of Publication No. CN106188770A discloses a kind of antimicrobial preservative film, and the patent is with polyvinyl resin
For base-material, antibacterial agent nano-titanium dioxide is added, the plastic fresh-keeping membrane for being particularly suitable for food packaging is manufactured with this.
Although titanium dioxide have ideal photocatalytic activity, however, its be applied to bactericidal, automatically cleaning,
When the related fieldss such as decomposing pollutant, there are still following deficiencies: in order to guarantee that titanium dioxide can be carried out with bacterium or pollutant
It comes into full contact with, the titanium dioxide for needing to guarantee to be applied to antibiotic self-cleaning field has high specific surface area.The prior art is usual
Increase its specific surface area by the titanium dioxide that prepared sizes are nanometer scale.However, due to nanometer scale titanium dioxide
Granularity is smaller, and the recombination rate in light induced electron and hole is then higher.After light induced electron and hole are quickly compound, the energy that absorbs
Amount is discharged in the form of luminous energy or thermal energy again, causes light induced electron and hole that can not be captured by bacterium or organic pollutant, and lead to
Cross the effect for participating in redox reaction and giving full play to antibacterial and decomposing organic matter.
In addition, in order to solve the titanium dioxide technical problem lower to the responsiveness of visible light and natural light, existing skill
Art, as sensitized fluorescence agent, is added in titanium dioxide using rare earth element composition.Specific rare earth element composition can incite somebody to action
Visible light and infrared light are converted into ultraviolet light, imitate so as to improve titanium dioxide to longer wavelengths of visible light and utilizing for infrared light
Rate, to improve the photocatalytic activity of titanium dioxide.However the intensity and efficiency of rare earth element luminescent transition in titanium dioxide
It is not ideal enough, cause rare earth element composition adulterate titanium dioxide in visible light and infrared light utilization ratio it is still inadequate
It is ideal.
Summary of the invention
To overcome defect and deficiency existing in the prior art, the invention discloses a kind of preparation methods of titanium dioxide.
The invention is realized by the following technical scheme:
A kind of preparation method of titanium dioxide, it is characterised in that: by industrial titanium dioxide: heavy metal oxide glass powder=
(40-60): the mass ratio of (40-60) prepares composite titanium dioxide powder and is uniformly mixed the composite titanium dioxide powder;
Wherein, the raw material of the heavy metal oxide glass powder includes heavy metallic oxide and quality is the total matter of the heavy metallic oxide
The sensitized fluorescence agent of the 1-2% of amount.
Further, the heavy metal oxide glass powder is in germanate-tellurite glasses powder or barium bismuthate glass powder
Any one.
Further, the germanate-tellurite glasses powder is prepared using following steps:
(1) lead oxide: boron oxide: vanadic anhydride: germanium oxide: tellurium oxide=(10-12): (10-14): (10-14) is pressed:
(20-25): the mass ratio of (40-45) weighs the heavy metallic oxide, and addition quality is the heavy metallic oxide gross mass
1-2% sensitized fluorescence agent, ground and mixed is uniform, obtain glass dust raw material;
(2) glass dust raw material is melted 2-4 hours under the conditions of 650-850 DEG C of temperature, obtains glass metal;
(3) glass metal is formed in a mold, and annealed 1-2 hours under the conditions of 200-240 DEG C of temperature, obtained clear
Clear glass body;
(4) clear glass is cooled to room temperature, crushes, grinds, obtain heavy metal oxide glass powder.
Further, the barium bismuthate glass powder is prepared using following steps:
(1) lead oxide: magnesia: sodium oxide molybdena: barium monoxide: bismuth oxide=(8-10): (6-10): (6-10): (25- is pressed
30): the mass ratio of (45-50) weighs the heavy metallic oxide, and addition quality is the 1- of the heavy metallic oxide gross mass
2% sensitized fluorescence agent, ground and mixed is uniform, obtains glass dust raw material;
(2) glass dust raw material is melted 2-4 hours under the conditions of 850-1050 DEG C of temperature, obtains glass metal;
(3) glass metal is formed in a mold, and annealed 1-2 hours under the conditions of 220-260 DEG C of temperature, obtained clear
Clear glass body;
(4) clear glass is cooled to room temperature, crushes, grinds, obtain heavy metal oxide glass powder.
Further, the sensitized fluorescence agent is the composition or praseodymium oxide of terbium oxide and ytterbium oxide and the group of ytterbium oxide
Close any one in the composition of object or erbium oxide and ytterbium oxide.
Further, the granularity of the heavy metal oxide glass powder is 100-150 microns.
Further, the refractive index of the heavy metal oxide glass powder is 1.9-2.3.
Compared with prior art, the present invention the advantage is that:
1. the present invention is by mixing industrial titanium dioxide and heavy metal oxide glass powder, so that titanium dioxide conduct
Cladding shell is fixed on heavy metal oxide glass powder surface, both ensure that titanium dioxide can be filled with bacterium or pollutant
The contact divided, and the recombination rate of titanium dioxide photoproduction electrons and holes is reduced, improve the photocatalysis performance of titanium dioxide;
2. the present invention prepares titanium dioxide using the heavy metal oxide glass powder comprising sensitized fluorescence agent and industrial titanium dioxide
The composite granule of titanium, since the higher heavy metal oxide glass powder of refractive index has strong covalency and strictly asymmetric
Property, therefore sensitized fluorescence agent has higher luminescent transition radiation intensity and efficiency in heavy metal oxide glass powder, facilitates
Efficiently titanium dioxide is helped to will be seen that light and infrared light are converted into natural light, so that the light for further improving titanium dioxide is urged
Change performance.
Detailed description of the invention
Fig. 1 present invention prepares the structural schematic diagram of titanium dioxide;
A kind of first usage state diagram of Equipment for Heating Processing of Fig. 2;
A kind of second usage state diagram of Equipment for Heating Processing of Fig. 3.
Specific embodiment
The present invention provides a kind of preparation methods of titanium dioxide: by industrial titanium dioxide: heavy metal oxide glass powder=
(40-60): the mass ratio of (40-60) prepares composite titanium dioxide powder and is uniformly mixed the composite titanium dioxide powder;
Wherein, the raw material of the heavy metal oxide glass powder includes heavy metallic oxide and quality is the total matter of the heavy metallic oxide
The sensitized fluorescence agent of the 1-2% of amount.
Industrial titanium dioxide granularity is nanometer scale (usually less than 200nm), and heavy metal oxide glass powder is as a kind of
It is crushed by glass material, the powder of grinding and acquisition, granularity is micron dimension (the specific granularity of heavy metal oxide glass powder
Size can be adjusted by grinding technics and time), it is preferred that the granularity of the heavy metal oxide glass powder is 100-
150 microns.As shown in Fig. 1, it is kernel that endothecium structure 1, which is heavy metal oxide glass powder, and layer structure 2 is outside titanium dioxide
Shell.By mechanical mixture, titanium dioxide may make to be fixed on heavy metal oxide glass powder surface, is formed with heavy metallic oxide
Glass powder is kernel, and titanium dioxide is the double-layer structure of shell.
The titanium dioxide of double-layer structure both can fully be contacted with bacterium or pollutant, at the same avoid light induced electron and
Hole it is quick compound, so as to promote light induced electron and hole mobile to titanium dioxide granule surface respectively, and sufficiently and carefully
Bacterium or organic pollutant carry out redox reaction.Therefore, the titanium dioxide of the method for the invention preparation has preferably light
Catalytic performance.
The sensitized fluorescence agent can absorb infrared light and visible light, and infrared light and visible light are converted to ultraviolet light.By
There is strong covalency and stringent asymmetry in the higher heavy metal oxide glass powder of refractive index, therefore described
Sensitized fluorescence agent has higher luminescent transition radiation intensity and efficiency in the heavy metal oxide glass powder, facilitates efficiently
Ground will be seen that light and infrared light is converted into natural light, help titanium dioxide to efficiently use natural light, to further mention
The high photocatalysis performance of titanium dioxide.
The addition of sensitized fluorescence agent can promote heavy metal oxide glass powder that there is good Ultraluminescence transmitting to influence.Tool
Body, by the addition of sensitized fluorescence agent, heavy metal oxide glass powder can effectively inhale visible light and/or infrared light
It receives, and converts a short wavelength UV photon for the more than two longer-wave photons absorbed.Therefore, the sensitized fluorescence is added
The capable of emitting effective short wave ultraviolet light of the heavy metal oxide glass powder of agent, thus promote titanium dioxide in light-catalyzed reaction, it is right
The absorption and use efficiency of visible light and infrared light.
In one of embodiment of the invention, the sensitized fluorescence agent is the composition of terbium oxide and ytterbium oxide,
Or praseodymium oxide and ytterbium oxide composition or erbium oxide and ytterbium oxide composition in any one.
Inventor can be obviously improved the light of titanium dioxide it was unexpectedly observed that using above-mentioned composition as sensitized fluorescence agent
Catalytic efficiency.It is not limited to any theory, it has been recognised by the inventors that any one in terbium ion, praseodymium ion and erbium ion can be by can
Light-exposed excitation, energy level is from ground state transition to excitation state.Ytterbium ion can be excited by near infrared light, energy level from ground state transition to
Excitation state.Then, the ytterbium ion of excitation state is fallen after rise to ground state, while discharging photon energy, and by photon energy pass to terbium from
Any one in son, praseodymium ion and erbium ion.Any one in terbium ion, praseodymium ion and erbium ion is absorbing photon energy
Transit to higher excitation state again afterwards, and release wavelength is less than or equal to the ultraviolet light of 380nm during falling to ground state.
Therefore, the composition of the composition or praseodymium oxide of terbium oxide and ytterbium oxide and the composition or erbium oxide of ytterbium oxide and ytterbium oxide
In any one can will be seen that light and infrared light are converted into ultraviolet light by energy transmission, to promote titanium dioxide to can
Light-exposed and infrared light producing level.
In one of embodiment of the invention, the heavy metal oxide glass powder is selected from germanate-tellurite glasses powder
Or any one in barium bismuthate glass powder.
Tellurate glass has the advantages that softening temperature is extremely low, however because having unique trigonal biyramid structure, it is mechanical
Intensity and chemical stability all need to be further increased.By the addition of germanium oxide, improve the object of tellurate glass with can dramatically
Physicochemical performance.And improve glass forming ability, optical property and the viscosity of tellurium oxide glass.
Bismuthate glass has ideal viscosity and glass forming ability, can further improve bismuth by the addition of barium monoxide
The refractive index of silicate glass.
In one of embodiment of the invention, the germanate-tellurite glasses powder is prepared using following steps:
(1) lead oxide: boron oxide: vanadic anhydride: germanium oxide: tellurium oxide=(10-12): (10-14): (10-14) is pressed:
(20-25): the mass ratio of (40-45) weighs the heavy metallic oxide, and addition quality is the heavy metallic oxide gross mass
1-2% sensitized fluorescence agent, ground and mixed is uniform, obtain glass dust raw material;
(2) glass dust raw material is melted 2-4 hours under the conditions of 650-850 DEG C of temperature, obtains glass metal;
(3) glass metal is formed in a mold, and annealed 1-2 hours under the conditions of 200-240 DEG C of temperature, obtained clear
Clear glass body;
(4) clear glass is cooled to room temperature, crushes, grinds, obtain heavy metal oxide glass powder.
In one of embodiment of the invention, the barium bismuthate glass powder is prepared using following steps:
(1) lead oxide: magnesia: sodium oxide molybdena: barium monoxide: bismuth oxide=(8-10): (6-10): (6-10): (25- is pressed
30): the mass ratio of (45-50) weighs the heavy metallic oxide, and addition quality is the 1- of the heavy metallic oxide gross mass
2% sensitized fluorescence agent, ground and mixed is uniform, obtains glass dust raw material;
(2) glass dust raw material is melted 2-4 hours under the conditions of 850-1050 DEG C of temperature, obtains glass metal;
(3) glass metal is formed in a mold, and annealed 1-2 hours under the conditions of 220-260 DEG C of temperature, obtained clear
Clear glass body;
(4) clear glass is cooled to room temperature, crushes, grinds, obtain heavy metal oxide glass powder.
The industrial titanium dioxide that the present invention uses can be by prior arts such as hydro-thermal method, sol-gal process, sulfuric acid process, chloridisings
It obtains, or is directly purchased by commercial sources.In order to inhibit the compound of light induced electron and hole, promote light induced electron and hole with
Bacterium or organic pollutant carry out being sufficiently oxidized reduction reaction, to further increase beneficial effects of the present invention, are using
Before this method prepares titanium dioxide, fullerene also can be used, processing is modified to the industrial titanium dioxide.
In one of embodiment of the invention, before preparing composite titanium dioxide powder, using fullerene pair
Industrial titanium dioxide is modified processing.Graphite can be used as carbon source in the fullerene that the embodiment of the present invention uses, and is put by electric arc
The prior arts such as point method, oxidation-reduction method, chemical vapour deposition technique, plasma method obtain, or are directly adopted by commercial sources
Purchase.Inventor is it was unexpectedly observed that by mixing the fullerene water solution of certain concentration and ratio and tio_2 suspension
Stirring is closed, the photocatalysis performance of titanium dioxide is remarkably improved.It can be not limited to any theory, it has been recognised by the inventors that due to fullerene
With special carrier properties, electronics at room temperature, which is much higher than other with hole concentration, charge migration rate, is partly led
Body material.Therefore, fullerene can reduce the recombination rate of light induced electron and hole in titanium dioxide, to further improve two
The photocatalytic activity of titanium oxide.
In one of embodiment of the invention, the fullerene can be hydroxylating fullerene.Hydroxylating fowler
Alkene has preferably solubility and dispersibility in water-based system.Therefore, hydroxylating fullerene is configured to aqueous solution, and with two
After titanium oxide suspension mixing, the hydroxylating fullerene can more rapidly, equably contact with each other with titanium dioxide granule, thus
It improves the effect of fullerene modification and improves the photocatalytic activity of titanium dioxide.
Technical solution of the present invention is described below in conjunction with specific embodiment, it should be noted that the present invention makes
The devices such as weighing, mixing, stirring and equipment are device and equipment commonly used in the art, are able to achieve the purpose of the present invention i.e.
Can, the invention does not limit this.
Embodiment 1
By lead oxide: boron oxide: vanadic anhydride: germanium oxide: tellurium oxide=10:10:10:25:45 mass ratio weighs
Glass dust raw material, addition quality is 1% terbium oxide of above-mentioned five kinds of oxide gross masses and quality is above-mentioned five kinds of oxides
1% ytterbium oxide of gross mass, ground and mixed are uniform;The glass dust raw material is put into platinum crucible, is sent by preheating
Muffle furnace melts 2 hours under the conditions of 850 DEG C of temperature, obtains glass metal;The glass metal is poured into aluminium sheet die for molding,
And it is sent into another Muffle furnace by preheating, it anneals 2 hours under the conditions of 240 DEG C of temperature, obtains clear glass;Close Muffle
The power supply of furnace cools to the clear glass with the furnace room temperature.The clear glass is crushed, grinding, obtains granularity about
For 100-150 microns of heavy metal oxide glass powder.By industrial titanium dioxide: heavy metal oxide glass powder=40:60 matter
Composite titanium dioxide powder is uniformly mixed by amount than preparing composite titanium dioxide powder.
Embodiment 2
By lead oxide: boron oxide: vanadic anhydride: germanium oxide: tellurium oxide=12:12:12:22:42 mass ratio weighs
Glass dust raw material, addition quality is 1% praseodymium oxide of above-mentioned five kinds of oxide gross masses and quality is above-mentioned five kinds of oxides
1% ytterbium oxide of gross mass, ground and mixed are uniform;The glass dust raw material is put into platinum crucible, is sent by preheating
Muffle furnace melts 4 hours under the conditions of 650 DEG C of temperature, obtains glass metal;The glass metal is poured into aluminium sheet die for molding,
And it is sent into another Muffle furnace by preheating, it anneals 1 hour under the conditions of 220 DEG C of temperature, obtains clear glass;Close Muffle
The power supply of furnace cools to the clear glass with the furnace room temperature.The clear glass is crushed, grinding, obtains granularity about
For 100-150 microns of heavy metal oxide glass powder.By industrial titanium dioxide: heavy metal oxide glass powder=60:40 matter
Composite titanium dioxide powder is uniformly mixed by amount than preparing composite titanium dioxide powder.
Embodiment 3
By lead oxide: boron oxide: vanadic anhydride: germanium oxide: tellurium oxide=12:14:14:20:40 mass ratio weighs
Glass dust raw material, addition quality is 1% erbium oxide of above-mentioned five kinds of oxide gross masses and quality is above-mentioned five kinds of oxides
1% ytterbium oxide of gross mass, ground and mixed are uniform;The glass dust raw material is put into platinum crucible, is sent by preheating
Muffle furnace melts 3 hours under the conditions of 700 DEG C of temperature, obtains glass metal;The glass metal is poured into aluminium sheet die for molding,
And it is sent into another Muffle furnace by preheating, it anneals 1 hour under the conditions of 220 DEG C of temperature, obtains clear glass;Close Muffle
The power supply of furnace cools to the clear glass with the furnace room temperature.The clear glass is crushed, grinding, obtains granularity about
For 100-150 microns of heavy metal oxide glass powder.By industrial titanium dioxide: heavy metal oxide glass powder=60:40 matter
Composite titanium dioxide powder is uniformly mixed by amount than preparing composite titanium dioxide powder.
Embodiment 4
By lead oxide: magnesia: sodium oxide molybdena: barium monoxide: bismuth oxide=8:6:6:30:35 mass ratio weighs glass powder original
Material, addition quality is 0.5% terbium oxide of above-mentioned five kinds of oxide gross masses and quality is above-mentioned five kinds of oxide gross masses
0.5% ytterbium oxide, ground and mixed is uniform;The glass dust raw material is put into platinum crucible, is sent into the Muffle by preheating
Furnace melts 4 hours under the conditions of 850 DEG C of temperature, obtains glass metal;The glass metal is poured into aluminium sheet die for molding, and is sent
Enter another Muffle furnace by preheating, anneal 2 hours under the conditions of 220 DEG C of temperature, obtains clear glass;Close Muffle furnace
Power supply cools to the clear glass with the furnace room temperature.The clear glass is crushed, grinding, obtaining granularity is about
100-150 microns of heavy metal oxide glass powder.By industrial titanium dioxide: heavy metal oxide glass powder=40:60 quality
Than preparing composite titanium dioxide powder, composite titanium dioxide powder is uniformly mixed.
Embodiment 5
By lead oxide: magnesia: sodium oxide molybdena: barium monoxide: bismuth oxide=10:10:10:25:45 mass ratio weighs glass
Powder raw material, addition quality is 0.5% praseodymium oxide of above-mentioned five kinds of oxide gross masses and quality is that above-mentioned five kinds of oxides are total
0.5% ytterbium oxide of quality, ground and mixed are uniform;The glass dust raw material is put into platinum crucible, is sent by preheating
Muffle furnace melts 2 hours under the conditions of 1050 DEG C of temperature, obtains glass metal;The glass metal is poured into aluminium sheet die for molding,
And it is sent into another Muffle furnace by preheating, it anneals 1 hour under the conditions of 260 DEG C of temperature, obtains clear glass;Close Muffle
The power supply of furnace cools to the clear glass with the furnace room temperature.The clear glass is crushed, grinding, obtains granularity about
For 100-150 microns of heavy metal oxide glass powder.By industrial titanium dioxide: heavy metal oxide glass powder=60:40 matter
Composite titanium dioxide powder is uniformly mixed by amount than preparing composite titanium dioxide powder.
Embodiment 6
By fullerene: deionized water=0.4:1000 mass ratio prepares fullerene water solution;By industrial titanium dioxide: go from
The quality of sub- water=40:60 is than preparing titanium dioxide suspension;In the ratio of 1:10 by the fullerene water solution and titanium dioxide
Titanium suspension is mixed and stirred for uniformly, obtaining titanium dioxide emulsion;The titanium dioxide emulsion is filtered, is washed,
It is dry, obtain the industrial titanium dioxide Jing Guo modification.Using the commercial titanium manufactured in the present embodiment handled through fullerene modification
White powder prepares composite titanium dioxide powder in ratio described in embodiment 1 and step.
Embodiment 7
By fullerene: tetrabutylammonium hydroxide: sodium hydroxide: deionized water: ortho-xylene=0.1:0.3:4.6:18:77
Mass ratio prepare mixed solution I, the mixed solution I stir 60 hours under the conditions of 60 DEG C of temperature, separation aqueous phase solution;
By aqueous phase solution: ethyl acetate: ethylene glycol=8:32:60 volume ratio prepares mixed solution I I, and it is molten to be slowly stirred the mixing
Liquid II obtains sediment;The sediment is filtered, washed, is dried, hydroxylating fullerene is obtained.It is prepared using the present embodiment
Hydroxylating fullerene, the industrial titanium white handled through hydroxylating fullerene modification is prepared in ratio described in embodiment 6 and step
Powder, and composite titanium dioxide powder is prepared in ratio described in embodiment 1 and step.
Comparative example 1
Using the industrial titanium dioxide without any processing as a comparison case 1.
Comparative example 2
By industrial titanium dioxide: silica glass powder=40:60 mass ratio prepares composite titanium dioxide powder, by compound two
Titanium oxide powder is uniformly mixed.Wherein, the silica glass powder is by purchasing commercially available silica glass, and is ground
After obtain.
Comparative example 3
By lead oxide: boron oxide: vanadic anhydride: germanium oxide: tellurium oxide=10:10:10:25:45 mass ratio weighs
Glass dust raw material, ground and mixed are uniform;The glass dust raw material is put into platinum crucible, is sent into the Muffle furnace by preheating,
It is melted 2 hours under the conditions of 850 DEG C of temperature, obtains glass metal;The glass metal is poured into aluminium sheet die for molding, and is sent into another
It by the Muffle furnace of preheating, anneals 2 hours under the conditions of 240 DEG C of temperature, obtains clear glass;The power supply of Muffle furnace is closed,
Cool to the clear glass with the furnace room temperature.The clear glass is crushed, grinding, obtaining granularity is about 100-150
The heavy metal oxide glass powder of micron.By industrial titanium dioxide: heavy metal oxide glass powder=40:60 mass ratio is prepared multiple
Titanium dioxide powder is closed, composite titanium dioxide powder is uniformly mixed.
Comparative example 4
By lead oxide: magnesia: sodium oxide molybdena: barium monoxide: bismuth oxide=10:10:10:25:45 mass ratio weighs glass
Powder raw material, ground and mixed are uniform;The glass dust raw material is put into platinum crucible, the Muffle furnace by preheating is sent into, 1050
It is melted 2 hours under the conditions of DEG C temperature, obtains glass metal;The glass metal is poured into aluminium sheet die for molding, and is sent into another warp
The Muffle furnace for crossing preheating, anneals 1 hour under the conditions of 260 DEG C of temperature, obtains clear glass;The power supply of Muffle furnace is closed, it will
The clear glass cools to room temperature with the furnace.The clear glass is crushed, grinding, obtaining granularity is about 100-150 micro-
The heavy metal oxide glass powder of rice.By industrial titanium dioxide: heavy metal oxide glass powder=60:40 mass ratio is prepared compound
Composite titanium dioxide powder is uniformly mixed by titanium dioxide powder.
Photocatalysis performance is tested under ultraviolet light
Using the photocatalysis performance of following steps test titanium dioxide:
1. weighing the rhodamine B solution that 150ml concentration is 25mg/L is sent into photocatalyst reaction vessel;
2. being slowly added to prepared by the 0.3g embodiment of the present invention or comparative example two from the upper opening of photocatalyst reaction vessel
Titanium oxide, ultrasonic vibration make titanium dioxide be uniformly dispersed;
3. being protected from light absorption 2h;
4. carrying out rotary irradiation to photocatalyst reaction vessel using ultraviolet mercury lamp as light source;
5. at regular intervals, pipetting rhodamine B supernatant using liquid-transfering gun, rhodamine B is tested using spectrophotometer
The absorbance of maximum wavelength.
Pass through formula η=(At/A0) × 100% calculates the resolution ratio of rhodamine B, and wherein η is the resolution ratio of rhodamine B,
A0For the absorbance of initial rhodamine B, AtFor the absorbance of the rhodamine B after a period of time illumination.
Photocatalysis performance under natural light irradiation is simulated to test
Lamp is simulated using xenon lamp, tests identical equipment, parameter using with photocatalysis performance under ultraviolet light
Photocatalysis performance under simulation natural light irradiation is carried out with step.
Heavy metal oxide glass powder refraction index test
Using the heavy metal oxide glass of 2010 prism-coupled instrument of Metricon measurement 1-4 of embodiment of the present invention preparation
The refractive index of powder.It is n that heavy metal oxide glass without crushing, which is abutted against refractive index,pMaster prism lower part.It will enter
It penetrates light and imports tested glass, rotatable communication platform, when incidence angle θ is close to critical angle θcWhen, it will be all-trans in the bottom of prism
It penetrates, at this time θc=arcsin (n/np)。θcIt easily can accurately be measured with detector, it is right when detected intensity declines suddenly
The angle answered is critical angle.The refractive index n of prismpIt is known that θcIt is obtained by measurement, so as to find out the refractive index n of glass.This
Invention uses He-Ne laser and the wavelength of 633nm to test the embodiment of the present invention or right for the near infrared laser of 1550nm
The glass powder of ratio is before crushing as the refractive index of bulk material.
Statistical analysis
The test result provided in photocatalysis performance of the present invention test, absorption spectrum test and emission spectrum test is equal
Retrial of attaching most importance to test after average value.Statistical analysis is carried out using SPSS13.0 software, finally by Pearson correlation analysis
Relevance.P<0.05 is considered as difference, and statistically significant (P>0.05: difference is not significant;P < 0.05: significant difference;P < 0.01:
Difference highly significant).
Test result comparison
Table 1 lists the titanium dioxide of 1-7 of the embodiment of the present invention and comparative example 1-2 preparation in different time ultraviolet light
Under rhodamine B resolution ratio.As shown in Table 1, the titanium dioxide of 1-7 of embodiment of the present invention preparation is under ultraviolet light to sieve
The capacity of decomposition of red bright B is higher than the titanium dioxide of comparative example 1-2 preparation.The test result shows by using of the present invention
Heavy metal oxide glass powder and the mixing of industrial titanium dioxide, can get compound with excellent photocatalysis performance under ultraviolet light
Titanium dioxide powder.It is significantly higher than the industrial titanium dioxide without any processing to the capacity of decomposition of organic pollutant, also above
The composite titanium dioxide powder prepared using the simple glasses powder such as such as silica glass powder.In addition, the test knot of embodiment 6 and 7
Fruit shows using fullerene, it is preferred that after being modified processing to industrial titanium dioxide using hydroxylated fullerene, then uses
The method of the invention prepares titanium dioxide, can further improve its photocatalysis performance.
1 embodiment of the present invention of table and comparative example prepare rhodamine B of the titanium dioxide under ultraviolet light point
Solution rate
Table 2 lists the titanium dioxide of 1-7 of the embodiment of the present invention and comparative example 3-4 preparation under the irradiation of different time xenon lamp
Rhodamine B resolution ratio.As shown in Table 2, the titanium dioxide of 1-7 of embodiment of the present invention preparation is in the xenon for simulating natural light
Under the irradiation of light, the titanium dioxide of comparative example 3-4 preparation is higher than to the capacity of decomposition of rhodamine B.The test result shows logical
The addition of sensitized fluorescence agent is crossed, the present invention can get the dioxide composite titanium valve under natural light with excellent photocatalysis performance
Body.It, significantly greater than with same process, however and is not added with sensitized fluorescence agent and obtains to the capacity of decomposition of organic pollutant
Titanium dioxide powder.The reason of above-mentioned phenomenon occurs is that sensitized fluorescence agent is including ultraviolet, visible and infrared multi-wavelength
Under xenon source irradiation, the photon that can be more than 380nm to wavelength is absorbed, and has launched purple by energy transfer mechanism
Outer light, thus promote titanium dioxide to visible and infrared light absorption and utilization, therefore, 1-7 of embodiment of the present invention preparation
Titanium dioxide can more quickly and efficiently decompose rhodamine B under the xenon lamp irradiation of simulation natural light.In addition, of the invention
Photocatalytic activity is higher than the titanium dioxide of 1-3 of embodiment of the present invention preparation under the natural light of the titanium dioxide of embodiment 4-5 preparation.
The test result of embodiment 6 and 7 again shows that, using fullerene, it is preferred that using hydroxylated fullerene to industrial titanium dioxide
After being modified processing, then the method for the invention is used to prepare titanium dioxide, can further improve its photocatalysis performance.
The rhodamine B of 2 embodiment of the present invention of table and the titanium dioxide of comparative example preparation under natural light irradiation
Resolution ratio
Seen from table 3, bulk material of the heavy metal oxide glass powder that prepared by 1-5 of the embodiment of the present invention before crushing
Refractive index is between 1.9-2.3.The refractive index of the Common oxides glass such as silica alumina is usually between 1.4-1.7.By
There is strong covalency and stringent asymmetry, therefore sensitized fluorescence in the higher heavy metal oxide glass powder of refractive index
Agent has higher luminescent transition radiation intensity and efficiency in heavy metal oxide glass powder, helps efficiently to help titanium dioxide
Titanium will be seen that light and infrared light are converted into natural light, to further improve the photocatalysis performance of titanium dioxide.In addition, this hair
The refractive index of the barium bismuthate glass of bright embodiment 4-5 preparation is higher than the germanate-tellurite glasses powder of 4-5 of embodiment of the present invention preparation.
3 1-4 of the embodiment of the present invention of table prepares the refractive index of heavy metal oxide glass powder
It is complete technical solution of the invention above, however, in order to further increase titanium dioxide prepared by the present invention
Photocatalytic activity can be used following method and apparatus and be heat-treated to titanium dioxide prepared by the present invention.
Specifically, by industrial titanium dioxide: the mass ratio of heavy metal oxide glass powder=(40-60): (40-60) is prepared
Composite titanium dioxide powder and by the composite titanium dioxide powder after mixing, can be as follows to the compound dioxy
Change titanium valve body to be heat-treated:
(1) composite titanium dioxide powder is calcined 2-4 hours under the conditions of 360-420 DEG C of temperature;
(2) composite titanium dioxide powder is annealed 1-2 hours under the conditions of 200-240 DEG C of temperature.
The calcine technology can further improve the bond strength between industrial titanium dioxide and heavy metal oxide glass powder,
It fully ensures that titanium dioxide is fixed on glass powder surface, is formed using glass powder as kernel, titanium dioxide is the double-layer structure of shell
Stability.
The annealing process can eliminate the internal stress that heavy metal oxide glass powder generates in calcination process, to fill
Dividing ensure that the mechanical strength of the composite granule will not be reduced because of calcine technology, and avoid titanium dioxide because of glass powder
There are problems that internal stress in grain and be easy to fall off.
It is carried out in addition, the equipment such as resistance furnace in the prior art, Muffle furnace can be used in the calcining and annealing process.So
And in order to further increase technical effect of the invention, it improves the present invention and prepares two in titanium dioxide composite titanium dioxide powder
Binding force between titanium oxide and heavy metal oxide glass powder can carry out calcining and lehr attendant by following annealing devices
Skill.
A kind of annealing device, including calcination section 1, annealing portion 2 and sample lifting platform 3.The calcination section 1 includes outer shell
Body 11, the internal layer refractory brick 12 inside the outer shell 11, at least two silicon inside internal layer refractory brick 12
What carbon heating rod 13 and the encirclement of internal layer refractory brick 12 were formed is used to accommodate the calcination section inner cavity 14 to calcining sample.The calcination section
1 lower part is equipped with sample liftway 15.
The annealing portion 2 is located at the lower section of the calcination section 1, including outer shell 21, is located in the outer shell 21
The internal layer refractory brick 22 in portion, at least two silicon carbide heating rod 23 inside internal layer refractory brick 22 and internal layer refractory brick 22 wrap
Enclose to be formed for accommodating annealing portion inner cavity 24 to calcining sample.The calcination section 1, annealing portion 2 are gone up and down by the sample
Channel 15 is interconnected.
The sample lifting platform 3 includes the first fire rated partition 31 and the second fire rated partition 32, first fire rated partition 31
It is connected with each other with the second fire rated partition 32 by least two connecting rod 33.The lower part of second fire rated partition 32 is equipped with bottom
Seat 34.The top of second fire rated partition 32 is equipped with sample stage 35, and platinum crucible 36 is placed on the top of the sample stage 35.Institute
Stating sample lifting platform 3 can be moved up and down in the calcination section 1 and annealing portion 2 by the sample liftway 15.
As shown in Fig. 2, when a kind of annealing device provided by the invention is in the first working condition, the sample liter
Drop platform 3 is located inside the calcination section 1, and second fire rated partition 32 is located in the sample liftway 15, the platinum
Crucible 36 is located in the calcination section inner cavity 14.
As shown in Fig. 3, when a kind of annealing device provided by the invention is in the second working condition, the sample liter
Drop platform 3 is located inside the annealing portion 2, and first fire rated partition 31 is located at the bottom of the sample liftway 15, described
Platinum crucible 36 is located in annealing portion inner cavity 24.
A kind of annealing device provided by the invention further includes 4 (not shown) of sample lifting platform driving device, described
Lifting platform driving device 4 is electrically connected with the sample lifting platform 3, for driving and controlling the sample lifting platform 3 described
Moving up and down in calcination section 1 and annealing portion 2.
After calcining, there are internal stress inside glass powder, cause to be easy cracking, stripping in the titanium dioxide on glass powder surface
It falls.Annealing is to solve the effective means of above-mentioned technical problem, however, titanium dioxide to be transferred to the mistake of annealing furnace from calcining furnace
Cheng Zhong, titanium dioxide will be exposed in indoor environment, lead to sharp temperature drop, even if the temperature decrease in sample transfer process
It is very of short duration, however, this temperature decrease phenomenon still can cause certain shadow to the binding force of titanium dioxide and glass powder
It rings.Therefore, in order to further increase technical effect of the invention, it is of the present invention that above-mentioned annealing device progress can be used
Calcining and annealing process, so that titanium dioxide prepared by the present invention be avoided to occur during shifting from calcining furnace to annealing furnace
Temperature decrease, further improve the present invention and prepare titanium dioxide and heavy metal oxygen in titanium dioxide composite titanium dioxide powder
Binding force between compound glass powder.
Embodiments described above is only a part of the embodiments of the present invention, instead of all the embodiments.This field is general
Logical technical staff without making creative work, based on the present invention every other embodiment obtained, belongs to
In the scope of protection of the invention.
Claims (7)
1. a kind of preparation method of titanium dioxide, it is characterised in that: by industrial titanium dioxide: heavy metal oxide glass powder=(40-
60): the mass ratio of (40-60) prepares composite titanium dioxide powder and is uniformly mixed the composite titanium dioxide powder;Wherein,
The raw material of the heavy metal oxide glass powder includes heavy metallic oxide and quality is the heavy metallic oxide gross mass
The sensitized fluorescence agent of 1-2%.
2. the preparation method of titanium dioxide according to claim 1, which is characterized in that the heavy metal oxide glass powder
Any one in germanate-tellurite glasses powder or barium bismuthate glass powder.
3. the preparation method of titanium dioxide according to claim 2, which is characterized in that prepare the germanium using following steps
Tellurate glass powder:
(1) lead oxide: boron oxide: vanadic anhydride: germanium oxide: tellurium oxide=(10-12): (10-14): (10-14): (20- is pressed
25): the mass ratio of (40-45) weighs the heavy metallic oxide, and addition quality is the 1- of the heavy metallic oxide gross mass
2% sensitized fluorescence agent, ground and mixed is uniform, obtains glass dust raw material;
(2) glass dust raw material is melted 2-4 hours under the conditions of 650-850 DEG C of temperature, obtains glass metal;
(3) glass metal is formed in a mold, and annealed 1-2 hours under the conditions of 200-240 DEG C of temperature, obtain clarification glass
Glass body;
(4) clear glass is cooled to room temperature, crushes, grinds, obtain heavy metal oxide glass powder.
4. the preparation method of titanium dioxide according to claim 2, which is characterized in that prepare the barium using following steps
Bismuthate glass powder:
(1) lead oxide: magnesia: sodium oxide molybdena: barium monoxide: bismuth oxide=(8-10): (6-10): (6-10): (25-30) is pressed:
The mass ratio of (45-50) weighs the heavy metallic oxide, and addition quality is the 1-2% of the heavy metallic oxide gross mass
Sensitized fluorescence agent, ground and mixed is uniform, obtains glass dust raw material;
(2) glass dust raw material is melted 2-4 hours under the conditions of 850-1050 DEG C of temperature, obtains glass metal;
(3) glass metal is formed in a mold, and annealed 1-2 hours under the conditions of 220-260 DEG C of temperature, obtain clarification glass
Glass body;
(4) clear glass is cooled to room temperature, crushes, grinds, obtain heavy metal oxide glass powder.
5. the preparation method of titanium dioxide as claimed in any of claims 1 to 4, which is characterized in that the fluorescence
Sensitizer is the group of the composition or praseodymium oxide of terbium oxide and ytterbium oxide and the composition or erbium oxide of ytterbium oxide and ytterbium oxide
Close any one in object.
6. the preparation method of titanium dioxide as claimed in any of claims 1 to 4, which is characterized in that the huge sum of money
The granularity for belonging to oxide glass powder is 100-150 microns.
7. the preparation method of titanium dioxide as claimed in any of claims 1 to 6, which is characterized in that the huge sum of money
The refractive index for belonging to oxide glass powder is 1.9-2.3.
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