CN114849743A - Method for synthesizing anatase titanium dioxide based on eutectic solvent - Google Patents
Method for synthesizing anatase titanium dioxide based on eutectic solvent Download PDFInfo
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 152
- 230000005496 eutectics Effects 0.000 title claims abstract description 45
- 239000002904 solvent Substances 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 20
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 16
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 55
- 239000002245 particle Substances 0.000 claims abstract description 31
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000002156 mixing Methods 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 15
- 238000001354 calcination Methods 0.000 claims abstract description 14
- 230000032683 aging Effects 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000008367 deionised water Substances 0.000 claims abstract description 11
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 11
- 238000000227 grinding Methods 0.000 claims abstract description 11
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 11
- 239000010936 titanium Substances 0.000 claims abstract description 11
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 11
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000002243 precursor Substances 0.000 claims abstract description 10
- 150000002366 halogen compounds Chemical class 0.000 claims abstract description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 15
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 15
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical group [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 15
- JHJLBTNAGRQEKS-UHFFFAOYSA-M sodium bromide Chemical compound [Na+].[Br-] JHJLBTNAGRQEKS-UHFFFAOYSA-M 0.000 claims description 12
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 8
- 229910052739 hydrogen Inorganic materials 0.000 claims description 8
- 239000001257 hydrogen Substances 0.000 claims description 8
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 6
- FVAUCKIRQBBSSJ-UHFFFAOYSA-M sodium iodide Chemical compound [Na+].[I-] FVAUCKIRQBBSSJ-UHFFFAOYSA-M 0.000 claims description 6
- JRMUNVKIHCOMHV-UHFFFAOYSA-M tetrabutylammonium bromide Chemical compound [Br-].CCCC[N+](CCCC)(CCCC)CCCC JRMUNVKIHCOMHV-UHFFFAOYSA-M 0.000 claims description 6
- 239000001763 2-hydroxyethyl(trimethyl)azanium Substances 0.000 claims description 4
- JOOXCMJARBKPKM-UHFFFAOYSA-N 4-oxopentanoic acid Chemical compound CC(=O)CCC(O)=O JOOXCMJARBKPKM-UHFFFAOYSA-N 0.000 claims description 4
- 235000019743 Choline chloride Nutrition 0.000 claims description 4
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 4
- SGMZJAMFUVOLNK-UHFFFAOYSA-M choline chloride Chemical group [Cl-].C[N+](C)(C)CCO SGMZJAMFUVOLNK-UHFFFAOYSA-M 0.000 claims description 4
- 229960003178 choline chloride Drugs 0.000 claims description 4
- 239000011780 sodium chloride Substances 0.000 claims description 4
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims description 4
- BMYNFMYTOJXKLE-UHFFFAOYSA-N 3-azaniumyl-2-hydroxypropanoate Chemical compound NCC(O)C(O)=O BMYNFMYTOJXKLE-UHFFFAOYSA-N 0.000 claims description 2
- 239000005703 Trimethylamine hydrochloride Substances 0.000 claims description 2
- 239000004202 carbamide Substances 0.000 claims description 2
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims description 2
- 229940071870 hydroiodic acid Drugs 0.000 claims description 2
- 229940040102 levulinic acid Drugs 0.000 claims description 2
- 235000006408 oxalic acid Nutrition 0.000 claims description 2
- 239000011775 sodium fluoride Substances 0.000 claims description 2
- 235000013024 sodium fluoride Nutrition 0.000 claims description 2
- 235000009518 sodium iodide Nutrition 0.000 claims description 2
- SZYJELPVAFJOGJ-UHFFFAOYSA-N trimethylamine hydrochloride Chemical compound Cl.CN(C)C SZYJELPVAFJOGJ-UHFFFAOYSA-N 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 8
- 230000001699 photocatalysis Effects 0.000 abstract description 6
- 238000002360 preparation method Methods 0.000 abstract description 4
- 239000004065 semiconductor Substances 0.000 abstract description 4
- 238000010438 heat treatment Methods 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 229910010413 TiO 2 Inorganic materials 0.000 description 5
- 239000002608 ionic liquid Substances 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 239000002351 wastewater Substances 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 230000018109 developmental process Effects 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000004043 dyeing Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 231100000053 low toxicity Toxicity 0.000 description 2
- 229960000907 methylthioninium chloride Drugs 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000003911 water pollution Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002189 fluorescence spectrum Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000002563 ionic surfactant Substances 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 238000000696 nitrogen adsorption--desorption isotherm Methods 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000003900 soil pollution Methods 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
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- 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
- B01J27/06—Halogens; Compounds thereof
- B01J27/135—Halogens; Compounds thereof with titanium, zirconium, hafnium, germanium, tin or lead
-
- 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
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- 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
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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Abstract
The invention relates to the technical field of preparation of semiconductor photocatalytic materials, and provides a method for synthesizing anatase titanium dioxide based on a eutectic solvent, which comprises the following steps: s1, dispersing a precursor of titanium in first absolute ethyl alcohol to form solution A; s2, mixing the eutectic solvent with a halogen compound, second absolute ethyl alcohol, deionized water and nitric acid to form a solution B; s3, dropwise adding the solution B obtained in the step S2 into the solution A obtained in the step S1, and aging to obtain white titanium dioxide gel; s4, drying the titanium dioxide white gel obtained in the step S3 to obtain titanium dioxide particles; and S5, grinding the dried titanium dioxide particles and then calcining to obtain anatase titanium dioxide.
Description
Technical Field
The invention relates to the technical field of preparation of semiconductor photocatalytic materials, in particular to a method for synthesizing anatase titanium dioxide based on a eutectic solvent.
Background
With the progress of society, the rapid development of industrialization and the advancement of human civilization, the utilization of existing resources to realize the prosperity of national nationality becomes a key research object of researchers. However, in the process of development, a series of pollution problems such as air pollution, water pollution, soil pollution and the like are brought about. Among them, water resources are the most rigid demand for human life, and water pollution is a problem that is mainly focused and valued in various countries. In recent years, the discharge of wastewater from industrial production and daily life has been increasingly influential on the ecological environment, and among them, printing and dyeing wastewater is one of the most harmful species in wastewater because it contains a large amount of organic substances, which are relatively stable, chemically inactive, and poorly degradable, and seriously affect human health. Therefore, an efficient method for treating the printing and dyeing wastewater is urgently needed and becomes a research hotspot of researchers.
The application of the photocatalysis technology as a green technology in the fields of environmental improvement and energy becomes a research hotspot of researchers, and semiconductor materials widely researched comprise TiO 2 、ZnO、CdS、WO 3 、V 2 O 5 、g-C 3 N 4 Etc. among the above semiconductor photocatalytic materials, TiO 2 Due to the characteristics of good photochemistry, simple preparation, low toxicity, high catalytic activity and the like, the method has been widely researched in a plurality of fields and has made a certain progress.
TiO 2 The photocatalytic performance of the material mainly depends on the specific surface area, the particle size, the forbidden band width and the electron-hole recombination efficiency of the material. In TiO 2 In the synthesis of (2), in order to improve the photocatalytic effectResearch and development of TiO with high specific surface area 2 The material usually utilizes ionic liquid or surfactant as template agent, but because the surfactant is difficult to remove, the ionic liquid has the problems of complex synthesis, poor environmental friendliness, high price and the like, the ionic liquid is limited to TiO 2 Application in the technical field. And the eutectic solvent (DES) is taken as an ionic liquid, and is considered as a substitute of the ionic liquid due to the characteristics of negligible vapor pressure at room temperature, low toxicity and designability. The DES can be made of cheap, nontoxic and biodegradable materials, is simple to prepare, can be synthesized in one step only by heating and mechanical stirring, has an atom utilization rate of 100 percent, and is more suitable for industrial production.
Disclosure of Invention
The invention provides a method for synthesizing anatase titanium dioxide based on a eutectic solvent, which can effectively solve the problems.
The embodiment of the invention is realized by the following technical scheme:
a method for synthesizing anatase titanium dioxide based on a eutectic solvent comprises the following steps:
s1, dispersing a precursor of titanium in first absolute ethyl alcohol to form a solution A;
s2, mixing the eutectic solvent with a halogen compound, second absolute ethyl alcohol, deionized water and nitric acid to form a solution B;
s3, dropwise adding the solution B obtained in the step S2 into the solution A obtained in the step S1, and aging to obtain white titanium dioxide gel;
s4, drying the titanium dioxide white gel obtained in the step S3 to obtain titanium dioxide particles;
and S5, grinding the dried titanium dioxide particles and then calcining to obtain anatase titanium dioxide.
The technical scheme of the embodiment of the invention at least has the following advantages and beneficial effects:
1. the titanium dioxide prepared by the method is low in raw material cost and environment-friendly in synthesis, the dispersibility of the titanium dioxide can be enhanced by using the eutectic solvent as a template agent, the in-situ growth of the titanium dioxide is promoted, the prepared anatase titanium dioxide is uniform in shape and size, uniform in spatial distribution, large in specific surface area and uniform in pore size, the degradation efficiency of the anatase titanium dioxide on organic pollutants can be effectively improved, and the degradation rate of 20mg/L methylene blue for 120min can reach 88.8%;
2. according to the invention, the eutectic solvent is used as a template agent, and a halogen compound is doped under the action of the template agent to realize non-metal doping, so that the photocatalytic degradation performance of titanium dioxide is improved.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is an X-ray diffraction pattern of titanium dioxide of inventive example 3 and example 5 and a comparative example;
FIG. 2 is a nitrogen adsorption-desorption isotherm and pore size distribution diagram of titanium dioxide of example 6 of the present invention and a comparative example;
FIG. 3 is a fluorescence spectrum of titanium dioxide of examples 5 and 6 of the present invention and a comparative example;
FIG. 4 is a graph showing the ultraviolet diffuse reflection spectra of titanium dioxide of examples 3 and 4 of the present invention and a comparative example;
FIG. 5 is an X-ray photoelectron spectroscopy spectrum of titanium dioxide of example 6 of the present invention;
FIG. 6 is a graph of high resolution of Ti and Cl in example 6 of the present invention;
FIG. 7 is a scanning electron micrograph of titanium dioxide according to example 6 of the present invention;
FIG. 8 is a graph showing the degradation effects of anatase titania prepared in examples 2, 4 and 6 according to the present invention and titania prepared in a comparative example on 20mg/L methylene blue solution;
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The specific implementation mode of the invention comprises the following steps:
s1, dispersing a precursor of titanium in first absolute ethyl alcohol to form solution A;
s2, mixing the eutectic solvent with a halogen compound, second absolute ethyl alcohol, deionized water and nitric acid to form a solution B;
s3, dropwise adding the solution B obtained in the step S2 into the solution A obtained in the step S1, and aging to obtain white titanium dioxide gel;
s4, drying the titanium dioxide white gel obtained in the step S3 to obtain titanium dioxide particles;
and S5, grinding the dried titanium dioxide particles and then calcining to obtain anatase titanium dioxide.
In step S1, the precursor of titanium is tetrabutyl titanate.
In step S1, the molar ratio of the precursor of titanium: first absolute ethyl alcohol ═ 1: (20-28).
In step S2, the eutectic solvent is a combination of a hydrogen bond acceptor and a hydrogen bond donor;
the hydrogen bond receptor is choline chloride, tetrabutylammonium bromide or trimethylamine hydrochloride;
the hydrogen bond donor is one or more of urea, oxalic acid, ethylene glycol, glycerol and levulinic acid.
Wherein the molar ratio of the precursor of titanium in the step S1 to the eutectic solvent in the step S2 is 1: (1-3).
Wherein, in step S2, the halogen compound is one or more of sodium fluoride, sodium chloride, sodium bromide, sodium iodide, hydrofluoric acid, hydrochloric acid, hydrobromic acid and hydroiodic acid.
Wherein, in step S2, the pH value of the solution B is 3-4.
Wherein, in the step S3, the aging time is 3h-6 h.
Wherein, in the step S4, the drying temperature is 80-100 ℃, and the drying time is 12-24 h.
Wherein, in the step S5, the calcining temperature is 350-500 ℃, and the calcining time is 1-3 h.
Example 1
S1, dispersing 1.7mL of tetrabutyl titanate in 6.8mL of absolute ethyl alcohol to form a solution A;
s2, mixing the eutectic solvent with 2.34g of sodium chloride, 1.7mL of absolute ethyl alcohol, 1.7mL of deionized water and 0.01mL of nitric acid to form a solution B; wherein the molar ratio of the eutectic solvent to tetrabutyl titanate is 2:1, and the preparation method of the eutectic solvent comprises the steps of mixing choline chloride and ethylene glycol according to the molar ratio of 1:2, heating to 60 ℃, and stirring for reacting for 2 hours;
s3, dropwise adding the solution B to the solution A at the dropping speed of 3mL/min, and aging for 3h to obtain white gel;
s4, drying the white titanium dioxide gel in an oven at 80 ℃ for 24 hours; obtaining titanium dioxide particles;
s5, grinding the dried titanium dioxide particles, and calcining the titanium dioxide particles in a muffle furnace for 2 hours at 400 ℃ to obtain anatase titanium dioxide.
Example 2
S1, dispersing 1.7mL of tetrabutyl titanate in 6.8mL of absolute ethyl alcohol to form a solution A;
s2, mixing the eutectic solvent with 4.12g of sodium bromide, 1.7mL of absolute ethyl alcohol, 1.7mL of deionized water and 0.01mL of nitric acid to form a solution B; wherein the molar ratio of the eutectic solvent to tetrabutyl titanate is 3:1, and the eutectic solvent is prepared by mixing tetrabutylammonium bromide and ethylene glycol according to the molar ratio of 1:2, heating to 60 ℃, and stirring for reaction for 2 h;
s3, dropwise adding the solution B to the solution A at the dropping speed of 3mL/min, and aging for 3h to obtain white gel;
s4, drying the white titanium dioxide gel in an oven at 80 ℃ for 24 hours; obtaining titanium dioxide particles;
s5, grinding the dried titanium dioxide particles, and then putting the titanium dioxide particles into a muffle furnace to calcine the titanium dioxide particles for 2 hours at 400 ℃ to obtain anatase titanium dioxide.
Example 3
S1, dispersing 1.7mL of tetrabutyl titanate in 6.8mL of absolute ethyl alcohol to form a solution A;
s2, mixing the eutectic solvent with 4.12g of sodium bromide, 1.7mL of absolute ethyl alcohol, 1.7mL of deionized water and 0.01mL of nitric acid to form a solution B; wherein the molar ratio of the eutectic solvent to tetrabutyl titanate is 0.8:1, and the eutectic solvent is prepared by mixing tetrabutyl ammonium bromide and glycerol according to the molar ratio of 1:2, heating to 60 ℃, and stirring for reaction for 2 h;
s3, dropwise adding the solution B to the solution A at the dropping speed of 3mL/min, and aging for 3h to obtain white gel;
s4, drying the white titanium dioxide gel in an oven at 80 ℃ for 24 hours; obtaining titanium dioxide particles;
s5, grinding the dried titanium dioxide particles, and calcining the titanium dioxide particles in a muffle furnace for 2 hours at 400 ℃ to obtain anatase titanium dioxide.
Example 4
S1, dispersing 1.7mL of tetrabutyl titanate in 6.8mL of absolute ethyl alcohol to form a solution A;
s2, mixing the eutectic solvent with 4.12g of sodium bromide, 1.7mL of absolute ethyl alcohol, 1.7mL of deionized water and 0.01mL of nitric acid to form a solution B; wherein the molar ratio of the eutectic solvent to tetrabutyl titanate is 1.1:1, and the eutectic solvent is prepared by mixing tetrabutyl ammonium bromide and ethylene glycol according to the molar ratio of 1:2, heating to 60 ℃, and stirring for reacting for 2 h;
s3, dropwise adding the solution B to the solution A at the dropping speed of 3mL/min, and aging for 3h to obtain white gel;
s4, drying the white titanium dioxide gel in an oven at 80 ℃ for 24 hours; obtaining titanium dioxide particles;
s5, grinding the dried titanium dioxide particles, and calcining the titanium dioxide particles in a muffle furnace for 2 hours at 400 ℃ to obtain anatase titanium dioxide.
Example 5
S1, dispersing 1.7mL of tetrabutyl titanate in 6.8mL of absolute ethyl alcohol to form a solution A;
s2, mixing the eutectic solvent with 4.12g of sodium bromide, 1.7mL of absolute ethyl alcohol, 1.7mL of deionized water and 0.01mL of nitric acid to form a solution B; wherein the molar ratio of the eutectic solvent to tetrabutyl titanate is 1.6:1, and the eutectic solvent is prepared by mixing tetrabutyl ammonium bromide and glycerol according to the molar ratio of 1:2, heating to 60 ℃, and stirring for reaction for 2 h;
s3, dropwise adding the solution B to the solution A at the dropping speed of 3mL/min, and aging for 3h to obtain white gel;
s4, drying the white titanium dioxide gel in an oven at 80 ℃ for 24 hours; obtaining titanium dioxide particles;
s5, grinding the dried titanium dioxide particles, and calcining the titanium dioxide particles in a muffle furnace for 2 hours at 400 ℃ to obtain anatase titanium dioxide.
Example 6
S1, dispersing 1.7mL of tetrabutyl titanate in 6.8mL of absolute ethyl alcohol to form a solution A;
s2, mixing the eutectic solvent with 2.34g of sodium chloride, 1.7mL of absolute ethyl alcohol, 1.7mL of deionized water and 0.01mL of nitric acid to form a solution B; wherein the molar ratio of the eutectic solvent to tetrabutyl titanate is 2:1, and the eutectic solvent is prepared by mixing choline chloride and glycerol according to the molar ratio of 1:2, heating to 60 ℃, and stirring for reaction for 2 h;
s3, dropwise adding the solution B to the solution A at the dropping speed of 3mL/min, and aging for 3h to obtain white gel;
s4, drying the white titanium dioxide gel in an oven at 80 ℃ for 24 hours; obtaining titanium dioxide particles;
s5, grinding the dried titanium dioxide particles, and calcining the titanium dioxide particles in a muffle furnace for 2 hours at 400 ℃ to obtain anatase titanium dioxide.
Comparative example
S1, dispersing 1.7mL of tetrabutyl titanate in 6.8mL of absolute ethyl alcohol to form a solution A;
s2, mixing 1.7mL of absolute ethyl alcohol, 1.7mL of deionized water and 0.01mL of nitric acid to form a solution B;
s3, dropwise adding the solution B to the solution A at the dropping speed of 3mL/min, and aging for 3h to obtain white gel;
s4, drying the white titanium dioxide gel in an oven at 80 ℃ for 24 hours; obtaining titanium dioxide particles;
s5, grinding the dried titanium dioxide particles, and calcining the titanium dioxide particles in a muffle furnace for 2 hours at 400 ℃ to obtain anatase titanium dioxide.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method for synthesizing anatase titanium dioxide based on a eutectic solvent is characterized by comprising the following steps:
s1, dispersing a precursor of titanium in first absolute ethyl alcohol to form solution A;
s2, mixing the eutectic solvent with a halogen compound, second absolute ethyl alcohol, deionized water and nitric acid to form a solution B;
s3, dropwise adding the solution B obtained in the step S2 into the solution A obtained in the step S1, and aging to obtain white titanium dioxide gel;
s4, drying the titanium dioxide white gel obtained in the step S3 to obtain titanium dioxide particles;
and S5, grinding the dried titanium dioxide particles and then calcining to obtain anatase titanium dioxide.
2. The method for synthesizing anatase titania based on the eutectic solvent according to claim 1 wherein, in step S1, the precursor of titanium is tetrabutyl titanate.
3. The method for synthesizing anatase titania based on the eutectic solvent according to claim 1 wherein, in step S1, the molar ratio of the precursor of titanium: first absolute ethyl alcohol ═ 1: (20-28).
4. The method for synthesizing anatase titanium dioxide based on the eutectic solvent according to claim 1, wherein in step S2, the eutectic solvent is a combination of a hydrogen bond acceptor and a hydrogen bond donor;
the hydrogen bond receptor is choline chloride, tetrabutylammonium bromide or trimethylamine hydrochloride;
the hydrogen bond donor is one or more of urea, oxalic acid, ethylene glycol, glycerol and levulinic acid.
5. The method for synthesizing anatase titania based on the eutectic solvent according to claim 1, wherein the molar ratio of the precursor of titanium in step S1 to the eutectic solvent in step S2 is 1: (1-3).
6. The method for synthesizing anatase titanium dioxide based on the eutectic solvent according to claim 1 wherein, in step S2, the halogen compound is one or more of sodium fluoride, sodium chloride, sodium bromide, sodium iodide, hydrofluoric acid, hydrochloric acid, hydrobromic acid and hydroiodic acid.
7. The method for synthesizing anatase titania based on the eutectic solvent according to claim 1 wherein the pH of the B solution is 3 to 4 in step S2.
8. The method for synthesizing anatase titanium dioxide based on the eutectic solvent according to claim 1 wherein the aging time is 3 to 6 hours at step S3.
9. The method for synthesizing anatase titanium dioxide based on the eutectic solvent according to claim 1 wherein the drying temperature is 80 ℃ to 100 ℃ and the drying time is 12h to 24h in step S4.
10. The method for synthesizing anatase titanium dioxide based on the eutectic solvent according to claim 1 wherein the calcination temperature is 350 ℃ to 500 ℃ and the calcination time is 1h to 3h in step S5.
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