CN108339542A - A kind of preparation method of blue titanium dioxide - Google Patents
A kind of preparation method of blue titanium dioxide Download PDFInfo
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- CN108339542A CN108339542A CN201810186766.1A CN201810186766A CN108339542A CN 108339542 A CN108339542 A CN 108339542A CN 201810186766 A CN201810186766 A CN 201810186766A CN 108339542 A CN108339542 A CN 108339542A
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- titanium dioxide
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- eutectics
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 125
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 150000003839 salts Chemical class 0.000 claims abstract description 23
- 239000010936 titanium Substances 0.000 claims abstract description 18
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 14
- 150000002894 organic compounds Chemical class 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims description 22
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 12
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical group [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 230000005496 eutectics Effects 0.000 claims description 8
- DTQVDTLACAAQTR-UHFFFAOYSA-N Trifluoroacetic acid Chemical compound OC(=O)C(F)(F)F DTQVDTLACAAQTR-UHFFFAOYSA-N 0.000 claims description 7
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 6
- 239000011780 sodium chloride Substances 0.000 claims description 6
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- STSCVKRWJPWALQ-UHFFFAOYSA-N TRIFLUOROACETIC ACID ETHYL ESTER Chemical compound CCOC(=O)C(F)(F)F STSCVKRWJPWALQ-UHFFFAOYSA-N 0.000 claims description 3
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L magnesium chloride Substances [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 3
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Inorganic materials [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 3
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims description 3
- RHQDFWAXVIIEBN-UHFFFAOYSA-N Trifluoroethanol Chemical compound OCC(F)(F)F RHQDFWAXVIIEBN-UHFFFAOYSA-N 0.000 claims description 2
- 239000013078 crystal Substances 0.000 claims description 2
- PBWZKZYHONABLN-UHFFFAOYSA-N difluoroacetic acid Chemical compound OC(=O)C(F)F PBWZKZYHONABLN-UHFFFAOYSA-N 0.000 claims description 2
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims 2
- QEWYKACRFQMRMB-UHFFFAOYSA-N fluoroacetic acid Chemical compound OC(=O)CF QEWYKACRFQMRMB-UHFFFAOYSA-N 0.000 claims 2
- VUYQBMXVCZBVHP-UHFFFAOYSA-N 1,1-difluoroethanol Chemical compound CC(O)(F)F VUYQBMXVCZBVHP-UHFFFAOYSA-N 0.000 claims 1
- GGDYAKVUZMZKRV-UHFFFAOYSA-N 2-fluoroethanol Chemical compound OCCF GGDYAKVUZMZKRV-UHFFFAOYSA-N 0.000 claims 1
- 150000002148 esters Chemical class 0.000 claims 1
- 125000004494 ethyl ester group Chemical group 0.000 claims 1
- PYLWMHQQBFSUBP-UHFFFAOYSA-N monofluorobenzene Chemical compound FC1=CC=CC=C1 PYLWMHQQBFSUBP-UHFFFAOYSA-N 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 9
- 239000011261 inert gas Substances 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract 1
- 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 11
- 229940043267 rhodamine b Drugs 0.000 description 11
- 238000002156 mixing Methods 0.000 description 8
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 8
- 238000003837 high-temperature calcination Methods 0.000 description 7
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 description 4
- 230000008859 change Effects 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 238000001362 electron spin resonance spectrum Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 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
- 239000002994 raw material Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 239000011775 sodium fluoride Substances 0.000 description 2
- 235000013024 sodium fluoride Nutrition 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 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
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 206010070834 Sensitisation Diseases 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 229910010455 TiO2 (B) Inorganic materials 0.000 description 1
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 229910052987 metal hydride Inorganic materials 0.000 description 1
- 150000004681 metal hydrides Chemical class 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000000985 reflectance spectrum Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000008313 sensitization Effects 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000010671 solid-state reaction Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- YONPGGFAJWQGJC-UHFFFAOYSA-K titanium(iii) chloride Chemical compound Cl[Ti](Cl)Cl YONPGGFAJWQGJC-UHFFFAOYSA-K 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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Hydrology & Water Resources (AREA)
- Water Supply & Treatment (AREA)
- Environmental & Geological Engineering (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Toxicology (AREA)
- Catalysts (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The present invention relates to a kind of preparation methods of blue titanium dioxide, belong to chemistry and materials science field.The present invention is to mix titanium source with fluorinated organic compound, is then calcined in fuse salt high temperature, one-step method, which is made, has highly stable blue titanium dioxide.The method of the present invention is simple, does not need inert gas shielding, and yield is high, is suitble to large-scale industrial production.
Description
Technical field
The invention belongs to inorganic nano catalysis material technical field, more particularly to a kind of preparation side of blue titanium dioxide
Method.
Background technology
The semi-conducting material that titanium dioxide is stablized as a kind of function admirable, chemical property, is widely used in photocatalysis
Agent, gas sensor, solar cell have wide application in the energy and field of environment protection.Titanium dioxide typically exhibits white,
Its energy gap is 3.2eV, is only capable of being excited by the ultraviolet light in sunlight, light conversion efficiency is relatively low.Therefore, titanium dioxide is expanded
The photoresponse range of titanium becomes the hot spot of current titanic oxide material area research to visible-range.
Currently, the technology for expanding TiO 2 visible light response includes metal/non-metal doping, dye sensitization and Ti3+
Auto-dope method introduces Lacking oxygen by outstanding processing inside titanium dioxide, titanium dioxide can be made to be changed into other colors,
The method of use includes high temperature hydrogenation, metal powder reduction, NaHB4Reduction, vacuum reduction etc..For example, patent CN103962117A
A kind of titanium dioxide process of Color tunable is disclosed, metal hydride is mixed with titanium dioxide, is protected in inert gas
Under shield, color is made from light gray through the blue most adjustable titanium dioxide of Zhongdao black through high temperature solid state reaction.It has reported at present
Preparation blue titanium dioxide method it is complicated for operation, not only need high temperature and pressure and inert gas shielding, but also obtain blue
Titanium dioxide is unstable, and color is easy to take off after placing a period of time in air, to lose the responding ability to visible light.
Patent CN103553124A discloses the titanium tetrachloride that certain mol proportion is added using titanium trichloride as raw material, while with sodium fluoride
For stabilizer, the blue titanium dioxide nano particle stablized by solvent structure, fluorine ion therein can be with Ti3+Knot
It closes, makes Ti3+It is not easy by the dioxygen oxidation in air into Ti4+.But the presence of NaF can aggravate the condensation of titanium tetrachloride, it is difficult to control
The pattern of TiO2 processed, and fluorine ion is only combined on surface with the Ti atoms of plane of crystal, and photocatalytic activity is often resulted in
It reduces.
The present invention calcines preparation process using simple fuse salt, prepares blue titanium dioxide using various titanium sources, even
The titanium dioxide of white can be changed into blue titanium dioxide, this method is easy to operate, of low cost, has extensive commodity
Change prospect of production.
Invention content
It is of high cost, complicated for operation, steady it is an object of the invention to solve blue titanium dioxide preparation method in the prior art
The technical problem of qualitative difference provides a kind of easy to operate, low-cost blue titanium dioxide preparation method.
A kind of preparation method of blue titanium dioxide of the present invention, be by titanium source and fluorinated organic compound by a certain percentage
Then mixing is calcined in fuse salt high temperature, one-step method, which is made, has highly stable blue titanium dioxide.
A kind of preparation method of blue titanium dioxide of the present invention, including following steps：
(1) titanium source and fluorinated organic compound are mixed in a certain ratio uniformly, obtain mixture；
(2) said mixture and fuse salt are ground uniformly, is subsequently placed in the calcining of Muffle furnace high temperature；
(3) it after cooling, is washed with water, removes fuse salt, obtain blue titanium dioxide.
The optimal technical scheme of the present invention is that the titanium source is tetra-n-butyl titanate, tetraisopropyl titanate, tetrachloro
Change titanium or white titania powder.
Another optimal technical scheme of the present invention is that the fluorinated organic compound is trifluoroacetic acid or trifluoro second
Alcohol.
Another another optimal technical scheme of the present invention is that the molar ratio of titanium source and organic fluorocompound is 1：0.1~1：20.
Another another optimal technical scheme of the present invention is that the fuse salt is LiCl/KCl eutectics, LiNO3/KNO3Altogether
Crystalline substance, KCl/NaCl eutectics, AlCl3/ NaCl eutectics or MgCl2/ KCl eutectics.
Another another optimal technical scheme of the present invention is that calcination temperature is 200~700 DEG C, and calcination time is 0.5~10
Hour.
Another another optimal technical scheme of the present invention is that white titania titanium source can be anatase, rutile, plate
The mixture of one or more of titanium ore or TiO2 (B).
Beneficial effects of the present invention：
(1) preparation method of the invention is simple, of low cost, is suitable for all titanium dioxide raw materials, convenient for industrialization
Production.
(2) blue titanium dioxide prepared by preparation method of the invention has good visible light-responded performance, visible
Under light irradiation, the rate of photocatalytic degradation rhodamine B is superior to commodity titanium dioxide P25.
Description of the drawings
Fig. 1 are the photos in kind of the blue titanium dioxide prepared by the embodiment of the present invention 1.
Fig. 2 are the ultraviolet-visible diffuse reflectance spectrums of the blue titanium dioxide prepared by the embodiment of the present invention 1.
Fig. 3 are the electron paramagnetic resonance spectrum figures of the blue titanium dioxide prepared by the embodiment of the present invention 2.
Fig. 4 are the x-ray photoelectron spectroscopy figures of the blue titanium dioxide prepared by the embodiment of the present invention 3.
Fig. 5 are the blue titanium dioxide and quotient prepared by the embodiment of the present invention 1, embodiment 2, embodiment 3 and embodiment 4
The photocatalytic activity of product titanium dioxide P25 rhodamine B degradations compares.
The present invention is further illustrated with reference to the accompanying drawings and embodiments, but it is to be noted that following embodiment
It is to be not to be construed as the limitation to the claimed range of the present invention for the invention will be further described.
Specific implementation mode
Embodiment 1
(1) by 5mL tetra-n-butyl titanates and 6.1mL trifluoroacetic acids in molar ratio 1：3 mixing, obtain mixture；
(2) said mixture is added in 2.48g LiCl and 3.1g KCl fuse salts and is ground uniformly, be subsequently placed in horse
Not in stove, 400 DEG C of high-temperature calcination 6h (see Fig. 1)；
(3) after cooling, be washed with water, remove fuse salt, obtain blue titanium dioxide, crystallite dimension be about 25nm (see
Fig. 2).The efficiency of its photocatalytic degradation rhodamine B is than commodity titanium dioxide P25 high (see Fig. 5).
Embodiment 2
(1) by 5mL tetra-n-butyl titanates and 12.2mL trifluoroacetic acids in molar ratio 1：6 mixing, obtain mixture；
(2) said mixture is added in 2.48g LiCl and 3.1g KCl fuse salts and is ground uniformly, be subsequently placed in horse
Not in stove, 500 DEG C of high-temperature calcination 6h；
(3) it after cooling, is washed with water, removes fuse salt, obtain blue titanium dioxide, electron paramagnetic resonance spectrum figure is shown
Contain a large amount of Ti in blue titanium dioxide3+(see Fig. 3) illustrates that the preparation method of the present invention can obtain the blue two of high stable
Titanium oxide.The efficiency of its photocatalytic degradation rhodamine B is compared with commodity titanium dioxide P25 high (see Fig. 5).
Embodiment 3
(1) by 5mL tetra-n-butyl titanates and 12.2mL trifluoroacetic acids in molar ratio 1：6 mixing, obtain mixture；
(2) said mixture is added to 3.57g LiNO3With 5.76g KNO3It grinds uniformly, is subsequently placed in fuse salt
In Muffle furnace, 600 DEG C of high-temperature calcination 3h；
(3) it after cooling, is washed with water, removes fuse salt, obtain blue titanium dioxide, x-ray photoelectron energy figure is shown
Contain Ti in blue titanium dioxide3+(see Fig. 4) illustrates that the preparation method of the present invention can obtain the blue dioxy having good stability
Change titanium.The efficiency of its photocatalytic degradation rhodamine B is better than commodity titanium dioxide P25 (see Fig. 5).
Embodiment 4
(1) by 5mL tetra-n-butyl titanates and 12.2mL trifluoroethanols in molar ratio 1：6 mixing, obtain mixture；
(2) said mixture is added to 11g AlCl3It is uniform with being ground in 1g NaCl fuse salts, it is subsequently placed in Muffle
In stove, 200 DEG C of high-temperature calcination 5h；
(3) it after cooling, is washed with water, removes fuse salt, obtain blue titanium dioxide, photocatalytic degradation rhodamine B
Efficiency is better than commodity titanium dioxide P25 (see Fig. 5).
Embodiment 5
(1) by 5mL tetra-n-butyl titanates and 12.2mL Trifluoroacetic Acid Ethyl Esters in molar ratio 1：6 mixing, obtain mixture；
(2) said mixture is added to 11g AlCl3It is uniform with being ground in 1g NaCl fuse salts, it is subsequently placed in Muffle
In stove, 700 DEG C of high-temperature calcination 5h；
(3) it after cooling, is washed with water, removes fuse salt, obtain blue titanium dioxide, photocatalytic degradation rhodamine B
Efficiency is better than commodity titanium dioxide P25.
Embodiment 6
(1) by 5mL tetra-n-butyl titanates and 12.2mL difluoroacetic acids in molar ratio 1：6 mixing, obtain mixture；
(2) said mixture is added in 2.48g LiCl and 3.1g KCl fuse salts and is ground uniformly, be subsequently placed in horse
Not in stove, 400 DEG C of high-temperature calcination 1h；
(3) it after cooling, is washed with water, removes fuse salt, obtain blue titanium dioxide, photocatalytic degradation rhodamine B
Efficiency is better than commodity titanium dioxide P25.
Embodiment 7
(1) by 5mL tetra-n-butyl titanates and 12.2mL ethyl difluoros in molar ratio 1：6 mixing, obtain mixture；
(2) said mixture is added in 2.48g LiCl and 3.1g KCl fuse salts and is ground uniformly, be subsequently placed in horse
Not in stove, 400 DEG C of high-temperature calcination 1h；
(3) it after cooling, is washed with water, removes fuse salt, obtain blue titanium dioxide, photocatalytic degradation rhodamine B
Efficiency is better than commodity titanium dioxide P25.
Blue TiO2 prepared by the present invention is compared with commodity titanium dioxide P25 visible light catalysis activities：
Experiment condition：20mg photochemical catalysts, 20mL rhodamine B solutions (concentration 20mg/L), optical source wavelength λ>420nm, light
According to time 100min.
| Sample | Rhodamine B degradation rate |
| Commodity P25 | 69% |
| Embodiment 1 | 98% |
| Embodiment 2 | 95% |
| Embodiment 3 | 97% |
| Embodiment 4 | 96% |
| Embodiment 5 | 93% |
| Embodiment 6 | 91% |
| Embodiment 7 | 98% |
Claims (7)
1. a kind of preparation method of blue titanium dioxide, it is characterised in that carry out as follows：
(1) titanium source is uniformly mixed with fluorinated organic compound, obtains mixture；
(2) said mixture and fuse salt are ground uniformly, is subsequently placed in the calcining of Muffle furnace high temperature；
(3) it after cooling, is washed with water, removes fuse salt, obtain blue titanium dioxide.
2. preparation method according to claim 1, it is characterized in that：The titanium source includes tetra-n-butyl titanate, metatitanic acid four
The mixture of one or more of ethyl ester, titanium tetrachloride, white titania powder, metatitanic acid.
3. preparation method according to claim 1, it is characterized in that：The fluorinated organic compound be selected from trifluoroacetic acid,
Difluoroacetic acid, fluoroacetic acid, trifluoroethanol, difluoroethanol, fluoroethanol, Trifluoroacetic Acid Ethyl Ester, ethyl difluoro, fluoroacetic acid second
The mixture of one or more of ester, fluorobenzene.
4. preparation method according to claim 1, it is characterized in that：The ratio of the titanium source and fluorinated organic compound is
Molar ratio 1：0.1~1：20.
5. preparation method according to claim 1, it is characterized in that：The fuse salt is selected from LiCl/KCl eutectics, LiNO3/
KNO3Eutectic, KCl/NaCl eutectics, AlCl3/ NaCl eutectics, MgCl2One kind in/KCl eutectics.
6. preparation method according to claim 1, it is characterized in that：Calcination temperature is 200~700 DEG C, calcination time 0.5
~10 hours.
7. white titania powder according to claim 2, it is characterized in that：The white titania powder crystal form
Including anatase, rutile, brockite and TiO2One or more of (B) mixture.
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Cited By (2)
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| CN111170362A (en) * | 2018-11-12 | 2020-05-19 | 中国科学院物理研究所 | Preparation method of blue titanium dioxide particles |
| CN113262812A (en) * | 2021-05-11 | 2021-08-17 | 赵海涛 | Color-controllable zeolite modification method |
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| CN102631949A (en) * | 2011-02-12 | 2012-08-15 | 首都师范大学 | Modified visible-light responsive titania doped photocatalyst and production method and uses thereof |
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|---|---|---|---|---|
| CN111170362A (en) * | 2018-11-12 | 2020-05-19 | 中国科学院物理研究所 | Preparation method of blue titanium dioxide particles |
| CN111170362B (en) * | 2018-11-12 | 2021-03-23 | 中国科学院物理研究所 | Preparation method of blue titanium dioxide particles |
| CN113262812A (en) * | 2021-05-11 | 2021-08-17 | 赵海涛 | Color-controllable zeolite modification method |
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