CN108339542B - Preparation method of blue titanium dioxide - Google Patents
Preparation method of blue titanium dioxide Download PDFInfo
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- CN108339542B CN108339542B CN201810186766.1A CN201810186766A CN108339542B CN 108339542 B CN108339542 B CN 108339542B CN 201810186766 A CN201810186766 A CN 201810186766A CN 108339542 B CN108339542 B CN 108339542B
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 139
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 64
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000000203 mixture Substances 0.000 claims abstract description 36
- 150000003839 salts Chemical class 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 16
- 239000010936 titanium Substances 0.000 claims abstract description 11
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 9
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 9
- 239000011737 fluorine Substances 0.000 claims abstract description 9
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 9
- 150000002894 organic compounds Chemical class 0.000 claims abstract description 7
- 238000001354 calcination Methods 0.000 claims description 12
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical group [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims description 12
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 10
- DTQVDTLACAAQTR-UHFFFAOYSA-N Trifluoroacetic acid Chemical compound OC(=O)C(F)(F)F DTQVDTLACAAQTR-UHFFFAOYSA-N 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 9
- 238000000227 grinding 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
- 239000011780 sodium chloride Substances 0.000 claims description 6
- 239000013078 crystal Substances 0.000 claims description 5
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 claims description 5
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium chloride Substances Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims description 4
- RHQDFWAXVIIEBN-UHFFFAOYSA-N Trifluoroethanol Chemical compound OCC(F)(F)F RHQDFWAXVIIEBN-UHFFFAOYSA-N 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
- STSCVKRWJPWALQ-UHFFFAOYSA-N TRIFLUOROACETIC ACID ETHYL ESTER Chemical compound CCOC(=O)C(F)(F)F STSCVKRWJPWALQ-UHFFFAOYSA-N 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
- GZKHDVAKKLTJPO-UHFFFAOYSA-N ethyl 2,2-difluoroacetate Chemical compound CCOC(=O)C(F)F GZKHDVAKKLTJPO-UHFFFAOYSA-N 0.000 claims description 2
- 238000003837 high-temperature calcination Methods 0.000 claims description 2
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L magnesium chloride Substances [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 2
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 2
- QEWYKACRFQMRMB-UHFFFAOYSA-N fluoroacetic acid Chemical compound OC(=O)CF QEWYKACRFQMRMB-UHFFFAOYSA-N 0.000 claims 2
- JMXKSZRRTHPKDL-UHFFFAOYSA-N titanium ethoxide Chemical compound [Ti+4].CC[O-].CC[O-].CC[O-].CC[O-] JMXKSZRRTHPKDL-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
- 229910010251 TiO2(B) Inorganic materials 0.000 claims 1
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims 1
- VCYZVXRKYPKDQB-UHFFFAOYSA-N ethyl 2-fluoroacetate Chemical compound CCOC(=O)CF VCYZVXRKYPKDQB-UHFFFAOYSA-N 0.000 claims 1
- PYLWMHQQBFSUBP-UHFFFAOYSA-N monofluorobenzene Chemical compound FC1=CC=CC=C1 PYLWMHQQBFSUBP-UHFFFAOYSA-N 0.000 claims 1
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 4
- 239000011261 inert gas Substances 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract description 2
- 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
- 230000001699 photocatalysis Effects 0.000 description 6
- 238000005406 washing Methods 0.000 description 6
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 5
- 230000000593 degrading effect Effects 0.000 description 4
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 description 4
- 238000007146 photocatalysis Methods 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000004298 light response Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000011775 sodium fluoride Substances 0.000 description 2
- 235000013024 sodium fluoride Nutrition 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
- 238000004435 EPR spectroscopy Methods 0.000 description 1
- 206010070834 Sensitisation Diseases 0.000 description 1
- 229910010455 TiO2 (B) Inorganic materials 0.000 description 1
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001362 electron spin resonance spectrum Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- -1 fluoride ions Chemical class 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 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
- 239000005416 organic matter Substances 0.000 description 1
- 238000000985 reflectance spectrum Methods 0.000 description 1
- 230000004044 response Effects 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
- 238000004729 solvothermal method Methods 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- YONPGGFAJWQGJC-UHFFFAOYSA-K titanium(iii) chloride Chemical compound Cl[Ti](Cl)Cl YONPGGFAJWQGJC-UHFFFAOYSA-K 0.000 description 1
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- 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
-
- B01J35/39—
-
- 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)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Water Supply & Treatment (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Toxicology (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention relates to a preparation method of blue titanium dioxide, belonging to the technical field of chemistry and material science. The invention mixes the titanium source and the fluorine-containing organic compound, and then calcines the mixture in the fused salt at high temperature to prepare the blue titanium dioxide with high stability by a one-step method. The method is simple, does not need inert gas protection, has high yield and is suitable for large-scale industrial production.
Description
Technical Field
The invention belongs to the technical field of inorganic nano photocatalytic materials, and particularly relates to a preparation method of blue titanium dioxide.
Background
Titanium dioxide is used as a semiconductor material with excellent performance and stable chemical properties, is widely applied to photocatalysts, gas sensors and solar cells, and has wide application in the fields of energy and environmental protection. Titanium dioxide is generally white, has a forbidden band width of 3.2eV, can be excited only by ultraviolet light in sunlight, and has low light conversion efficiency. Therefore, expanding the photoresponse range of the titanium dioxide to the visible light range becomes a hot point of research in the field of the current titanium dioxide materials.
At present, techniques for expanding the visible light response of titanium dioxide include metal/nonmetal doping, dye sensitization, and Ti3+The self-doping method can lead the titanium dioxide to be converted into other colors by introducing oxygen vacancies into the titanium dioxide through special treatment, and adopts the methods of high-temperature hydrogenation, metal powder reduction and NaHB4Reduction, vacuum reduction, and the like. For example, patent CN103962117A discloses a method for preparing titanium dioxide with adjustable color, which comprises mixing metal hydride with titanium dioxide, and carrying out high temperature solid phase reaction under the protection of inert gas to obtain titanium dioxide with adjustable color from light gray, blue and black. The method for preparing the blue titanium dioxide reported at present is complex in operation, high temperature and high pressure and inert gas protection are required, the obtained blue titanium dioxide is unstable, and the color of the obtained blue titanium dioxide is easy to fade after the blue titanium dioxide is placed in the air for a period of time, so that the response capability to visible light is lost. Patent CN103553124A discloses that stable blue titanium dioxide nanoparticles are synthesized by a solvothermal method by using titanium trichloride as a raw material, adding titanium tetrachloride in a certain molar ratio and using sodium fluoride as a stabilizer, wherein fluorine is contained in the stable blue titanium dioxide nanoparticlesThe ions may be bonded to Ti3+Bonding of Ti3+Is not easily oxidized into Ti by oxygen in the air4+. However, the presence of NaF can aggravate the condensation of titanium tetrachloride, the morphology of TiO2 is difficult to control, and fluoride ions are only bonded with Ti atoms on the crystal surface at the surface, which tends to cause reduction of photocatalytic activity.
The method adopts a simple molten salt calcination preparation process, utilizes various titanium sources to prepare the blue titanium dioxide, and can even convert the white titanium dioxide into the blue titanium dioxide.
Disclosure of Invention
The invention aims to solve the technical problems of high cost, complex operation and poor stability of a blue titanium dioxide preparation method in the prior art, and provides the blue titanium dioxide preparation method which is simple and convenient to operate and low in cost.
The invention relates to a preparation method of blue titanium dioxide, which is characterized in that a titanium source and a fluorine-containing organic compound are mixed according to a certain proportion, and then are calcined in molten salt at high temperature to prepare the highly stable blue titanium dioxide by a one-step method.
The preparation method of the blue titanium dioxide comprises the following steps:
(1) uniformly mixing a titanium source and a fluorine-containing organic compound according to a certain proportion to obtain a mixture;
(2) grinding the mixture and molten salt uniformly, and then placing the mixture in a muffle furnace for high-temperature calcination;
(3) after cooling, the mixture was washed with water to remove the molten salt, thereby obtaining blue titanium dioxide.
According to a preferred technical scheme of the invention, the titanium source is tetra-n-butyl titanate, tetra-isopropyl titanate, titanium tetrachloride or white titanium dioxide powder.
In another preferred technical scheme of the invention, the fluorine-containing organic compound is trifluoroacetic acid or trifluoroethanol.
In another preferred technical scheme, the molar ratio of the titanium source to the fluorine-containing organic matter is 1: 0.1-1: 20.
in another preferred technical scheme of the invention, the molten salt is LiCl/KCl eutectic or LiNO3/KNO3Eutectic, KCl/NaCl eutectic, AlCl3NaCl eutectic or MgCl2a/KCl eutectic crystal.
According to another preferable technical scheme, the calcining temperature is 200-700 ℃, and the calcining time is 0.5-10 hours.
In another preferred embodiment of the present invention, the white titanium dioxide source may be one or a mixture of anatase, rutile, brookite or TiO2 (B).
The invention has the beneficial effects that:
(1) the preparation method is simple, has low cost, is suitable for all titanium dioxide raw materials, and is convenient for industrial production.
(2) The blue titanium dioxide prepared by the preparation method has good visible light response performance, and the rate of photocatalytic degradation of rhodamine B is better than that of commercial titanium dioxide P25 under the irradiation of visible light.
Drawings
FIG. 1 is a photograph of a real object of blue titanium dioxide produced in example 1 of the present invention.
FIG. 2 is a UV-VIS diffuse reflectance spectrum of blue titanium dioxide prepared in example 1 of the present invention.
FIG. 3 is an electron paramagnetic resonance spectrum of blue titanium dioxide prepared in example 2 of the present invention.
FIG. 4 is an X-ray photoelectron spectrum of blue titanium dioxide produced in example 3 of the present invention.
FIG. 5 is a comparison of the photocatalytic activity of blue titanium dioxide prepared in examples 1, 2, 3 and 4 of the present invention in degrading rhodamine B with commercial titanium dioxide P25.
The present invention is further described with reference to the following drawings and examples, but it should be noted that the following examples are only for the purpose of further illustrating the present invention and should not be construed as limiting the scope of the claimed invention.
Detailed Description
Example 1
(1) 5mL of tetra-n-butyl titanate and 6.1mL of trifluoroacetic acid were mixed in a molar ratio of 1: 3, mixing to obtain a mixture;
(2) adding the mixture into 2.48g LiCl and 3.1g KCl molten salt, grinding uniformly, and then placing in a muffle furnace, and calcining at the high temperature of 400 ℃ for 6h (see figure 1);
(3) after cooling, washing with water to remove the molten salt gave blue titanium dioxide having a crystal grain size of about 25nm (see FIG. 2). The efficiency of degrading rhodamine B by photocatalysis is higher than that of the commercial titanium dioxide P25 (see figure 5).
Example 2
(1) 5mL of tetra-n-butyl titanate and 12.2mL of trifluoroacetic acid were mixed in a molar ratio of 1: 6, mixing to obtain a mixture;
(2) adding the mixture into 2.48g LiCl and 3.1g KCl molten salt, grinding uniformly, then placing in a muffle furnace, and calcining at the high temperature of 500 ℃ for 6 hours;
(3) after cooling, washing with water to remove molten salt to obtain blue titanium dioxide, wherein an electron paramagnetic resonance spectrogram shows that the blue titanium dioxide contains a large amount of Ti3+(see FIG. 3), it is demonstrated that the preparation method of the present invention can obtain blue titanium dioxide with high stability. The efficiency of degrading rhodamine B by photocatalysis is higher than that of the commercial titanium dioxide P25 (see figure 5).
Example 3
(1) 5mL of tetra-n-butyl titanate and 12.2mL of trifluoroacetic acid were mixed in a molar ratio of 1: 6, mixing to obtain a mixture;
(2) the mixture was added to 3.57g of LiNO3And 5.76g KNO3Uniformly grinding the mixture in molten salt, then placing the mixture in a muffle furnace, and calcining the mixture for 3 hours at the high temperature of 600 ℃;
(3) after cooling, the resultant was washed with water to remove the molten salt, thereby obtaining blue titanium dioxide having an X-ray photoelectron diagram showing that the blue titanium dioxide contains Ti3+(see FIG. 4), it is demonstrated that blue titanium dioxide having good stability can be obtained by the production method of the present invention. The efficiency of degrading rhodamine B by photocatalysis is better than that of the commercial titanium dioxide P25 (see figure 5).
Example 4
(1) 5mL of tetra-n-butyl titanate and 12.2mL of trifluoroethanol were mixed in a molar ratio of 1: 6, mixing to obtain a mixture;
(2) the mixture is added to 11g of AlCl3Grinding the mixture evenly with 1g of NaCl molten salt, then placing the mixture in a muffle furnace, and calcining the mixture for 5 hours at a high temperature of 200 ℃;
(3) after cooling, washing with water to remove molten salt, blue titanium dioxide was obtained, which was superior in efficiency of photocatalytic degradation of rhodamine B to commercial titanium dioxide P25 (see fig. 5).
Example 5
(1) 5mL of tetra-n-butyl titanate and 12.2mL of ethyl trifluoroacetate were mixed in a molar ratio of 1: 6, mixing to obtain a mixture;
(2) the mixture is added to 11g of AlCl3Grinding the mixture evenly with 1g of NaCl molten salt, then placing the mixture in a muffle furnace, and calcining the mixture for 5 hours at the high temperature of 700 ℃;
(3) after cooling, washing with water to remove molten salt to obtain blue titanium dioxide, wherein the efficiency of photocatalytic degradation of rhodamine B is better than that of commercial titanium dioxide P25.
Example 6
(1) 5mL of tetra-n-butyl titanate and 12.2mL of difluoroacetic acid were mixed in a molar ratio of 1: 6, mixing to obtain a mixture;
(2) adding the mixture into 2.48g LiCl and 3.1g KCl molten salt, grinding uniformly, then placing in a muffle furnace, and calcining at the high temperature of 400 ℃ for 1 h;
(3) after cooling, washing with water to remove molten salt to obtain blue titanium dioxide, wherein the efficiency of photocatalytic degradation of rhodamine B is better than that of commercial titanium dioxide P25.
Example 7
(1) 5mL of tetra-n-butyl titanate and 12.2mL of ethyl difluoroacetate were mixed in a molar ratio of 1: 6, mixing to obtain a mixture;
(2) adding the mixture into 2.48g LiCl and 3.1g KCl molten salt, grinding uniformly, then placing in a muffle furnace, and calcining at the high temperature of 400 ℃ for 1 h;
(3) after cooling, washing with water to remove molten salt to obtain blue titanium dioxide, wherein the efficiency of photocatalytic degradation of rhodamine B is better than that of commercial titanium dioxide P25.
The visible light catalytic activity of the blue TiO2 prepared by the invention is compared with that of commercial titanium dioxide P25:
the experimental conditions are as follows: 20mg of photocatalyst, 20mL of rhodamine B solution (the concentration is 20mg/L), the wavelength of a light source is more than 420nm, and the illumination time is 100 min.
| Sample (I) | Degradation rate of rhodamine B |
| Commercial product P25 | 69％ |
| Example 1 | 98％ |
| Example 2 | 95％ |
| Example 3 | 97％ |
| Example 4 | 96％ |
| Example 5 | 93％ |
| Example 6 | 91％ |
| Example 7 | 98％ |
Claims (7)
1. The preparation method of the blue titanium dioxide is characterized by comprising the following steps:
(1) uniformly mixing a titanium source and a fluorine-containing organic compound to obtain a mixture;
(2) grinding the mixture and molten salt uniformly, and then placing the mixture in a muffle furnace for high-temperature calcination;
(3) after cooling, the mixture was washed with water to remove the molten salt, thereby obtaining blue titanium dioxide.
2. The method of claim 1, wherein: the titanium source comprises one or a mixture of more of tetrabutyl titanate, tetraethyl titanate, titanium tetrachloride, white titanium dioxide powder and titanic acid.
3. The method of claim 1, wherein: the fluorine-containing organic compound is one or a mixture of more of trifluoroacetic acid, difluoroacetic acid, fluoroacetic acid, trifluoroethanol, difluoroethanol, fluoroethanol, ethyl trifluoroacetate, ethyl difluoroacetate, ethyl fluoroacetate and fluorobenzene.
4. The method of claim 1, wherein: the ratio of the titanium source to the fluorine-containing organic compound is 1: 0.1-1: 20.
5. the method of claim 1, wherein: the molten salt is selected from LiCl/KCl eutectic and LiNO3/KNO3Eutectic, KCl/NaCl eutectic, AlCl3NaCl eutectic, MgCl2One of the/KCl eutectic crystals.
6. The method of claim 1, wherein: the calcination temperature is 200-700 ℃, and the calcination time is 0.5-10 hours.
7. The method according to claim 2, wherein the method further comprises: the white titanium dioxide powder crystal form comprises anatase, rutile, brookite and TiO2(B) One or a mixture of several of them.
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| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| WO2013062306A2 (en) * | 2011-10-24 | 2013-05-02 | 포항공과대학교 산학협력단 | High purity graphene synthesis melted in water through photocatalytic reaction |
| CN107500350A (en) * | 2017-09-25 | 2017-12-22 | 首都师范大学 | A kind of anatase TiO of the crystal face of exposure 0012And preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| WO2013062306A2 (en) * | 2011-10-24 | 2013-05-02 | 포항공과대학교 산학협력단 | High purity graphene synthesis melted in water through photocatalytic reaction |
| CN107500350A (en) * | 2017-09-25 | 2017-12-22 | 首都师范大学 | A kind of anatase TiO of the crystal face of exposure 0012And preparation method thereof |
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