CN113600158A - Preparation method of nano titanium dioxide photocatalyst - Google Patents
Preparation method of nano titanium dioxide photocatalyst Download PDFInfo
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- CN113600158A CN113600158A CN202110747980.1A CN202110747980A CN113600158A CN 113600158 A CN113600158 A CN 113600158A CN 202110747980 A CN202110747980 A CN 202110747980A CN 113600158 A CN113600158 A CN 113600158A
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 87
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000011259 mixed solution Substances 0.000 claims abstract description 58
- 239000004094 surface-active agent Substances 0.000 claims abstract description 49
- 150000003608 titanium Chemical class 0.000 claims abstract description 47
- 239000007788 liquid Substances 0.000 claims abstract description 41
- 239000007787 solid Substances 0.000 claims abstract description 32
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 31
- 150000000703 Cerium Chemical class 0.000 claims abstract description 27
- 239000000203 mixture Substances 0.000 claims abstract description 24
- 150000003839 salts Chemical class 0.000 claims abstract description 24
- 238000001354 calcination Methods 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000005406 washing Methods 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 16
- 238000003756 stirring Methods 0.000 claims abstract description 15
- 238000000926 separation method Methods 0.000 claims abstract description 6
- 239000007789 gas Substances 0.000 claims description 55
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 47
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 36
- 229910052757 nitrogen Inorganic materials 0.000 claims description 17
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 16
- 239000004408 titanium dioxide Substances 0.000 claims description 16
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims description 15
- -1 polyethylene Polymers 0.000 claims description 15
- 239000004698 Polyethylene Substances 0.000 claims description 9
- 229920000573 polyethylene Polymers 0.000 claims description 9
- 229920002523 polyethylene Glycol 1000 Polymers 0.000 claims description 9
- 229940113116 polyethylene glycol 1000 Drugs 0.000 claims description 9
- 229920002582 Polyethylene Glycol 600 Polymers 0.000 claims description 8
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 8
- 235000021355 Stearic acid Nutrition 0.000 claims description 8
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 8
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 8
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 claims description 8
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims description 8
- 229940057847 polyethylene glycol 600 Drugs 0.000 claims description 8
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims description 8
- 239000008117 stearic acid Substances 0.000 claims description 8
- 229910000348 titanium sulfate Inorganic materials 0.000 claims description 8
- 229910000349 titanium oxysulfate Inorganic materials 0.000 claims description 7
- 229940083575 sodium dodecyl sulfate Drugs 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 4
- 239000002245 particle Substances 0.000 abstract description 35
- 238000009826 distribution Methods 0.000 abstract description 13
- 238000006243 chemical reaction Methods 0.000 abstract description 10
- 230000000694 effects Effects 0.000 abstract description 4
- 239000003054 catalyst Substances 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 11
- 238000003917 TEM image Methods 0.000 description 10
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 10
- 230000015556 catabolic process Effects 0.000 description 9
- 238000006731 degradation reaction Methods 0.000 description 9
- 229910021645 metal ion Inorganic materials 0.000 description 9
- 229910021529 ammonia Inorganic materials 0.000 description 8
- 230000003197 catalytic effect Effects 0.000 description 8
- 238000002835 absorbance Methods 0.000 description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 7
- 238000001914 filtration Methods 0.000 description 6
- 230000001699 photocatalysis Effects 0.000 description 6
- 239000012716 precipitator Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 230000005540 biological transmission Effects 0.000 description 5
- 239000006185 dispersion Substances 0.000 description 5
- 229910052742 iron Inorganic materials 0.000 description 5
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 5
- 229940012189 methyl orange Drugs 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 150000002500 ions Chemical class 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 4
- 229910052684 Cerium Inorganic materials 0.000 description 3
- 238000000862 absorption spectrum Methods 0.000 description 3
- 150000002505 iron Chemical class 0.000 description 3
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 3
- 230000036632 reaction speed Effects 0.000 description 3
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 2
- 238000000975 co-precipitation Methods 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 238000003541 multi-stage reaction Methods 0.000 description 2
- 229910052755 nonmetal Inorganic materials 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 230000008094 contradictory effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-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
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/83—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with rare earths or actinides
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
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- B01J35/39—Photocatalytic properties
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/03—Precipitation; Co-precipitation
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Abstract
The invention discloses a preparation method of a nano titanium dioxide photocatalyst, and relates to the technical field of catalysts. The preparation method of the nano titanium dioxide photocatalyst comprises the following steps: s10, dissolving soluble ferric salt, soluble cerium salt, soluble titanium salt and a surfactant in water to obtain a mixed solution; s20, under the condition of stirring, introducing gas containing ammonia gas into the mixed solution, and reacting to obtain a solid-liquid mixture; and S30, carrying out solid-liquid separation on the solid-liquid mixture to obtain a solid, washing, drying and calcining the solid to obtain the nano titanium dioxide photocatalyst. The method is simple and easy to operate, gas-liquid interface reaction is adopted for control, and the prepared double-ion doped nano titanium dioxide has small particle size and narrow distribution and has better activity under visible light.
Description
Technical Field
The invention relates to the technical field of catalysts, in particular to a preparation method of a nano titanium dioxide photocatalyst.
Background
The nano titanium dioxide has the advantages of good catalytic activity, stability, no pollution to the environment, low manufacturing cost and the like, and is considered to be one of the most effective photocatalysts. However, titanium dioxide has some defects, and because the band gap of titanium dioxide is wide and the energy of a valence band is 3.2eV, only when the surface of titanium dioxide is irradiated by ultraviolet light with the wavelength of 387.5nm or less, electrons can be excited from the valence band to the conduction band to form photogenerated electron-hole, and thus the catalytic effect is achieved. The content of ultraviolet light in sunlight is less than 5%, and if an ultraviolet light source is added, the energy consumption is increased, which limits the application of the titanium dioxide photocatalyst to a great extent.
Although there are many reports that the catalytic effect of titanium dioxide under visible light is improved by doping metal ions, non-metal ions and the like, the existing multi-ion doped titanium dioxide is complex in preparation process, can be prepared by multi-step reaction, needs high-temperature hydrothermal reaction in the reaction process, has high requirements on equipment, and is poor in photocatalytic effect of the prepared product.
Disclosure of Invention
The invention mainly aims to provide a preparation method of a nano titanium dioxide photocatalyst, and aims to provide a simple preparation method of the photocatalyst.
In order to achieve the purpose, the invention provides a preparation method of a nano titanium dioxide photocatalyst, which comprises the following steps:
s10, dissolving soluble ferric salt, soluble cerium salt, soluble titanium salt and a surfactant in water to obtain a mixed solution;
s20, under the condition of stirring, introducing gas containing ammonia gas into the mixed solution, and reacting to obtain a solid-liquid mixture;
and S30, carrying out solid-liquid separation on the solid-liquid mixture to obtain a solid, washing, drying and calcining the solid to obtain the nano titanium dioxide photocatalyst.
Alternatively, in step S10,
the soluble ferric salt comprises ferric nitrate; and/or the presence of a gas in the gas,
the soluble cerium salt comprises cerium nitrate; and/or the presence of a gas in the gas,
the soluble titanium salt comprises any one of titanium sulfate and titanyl sulfate; and/or the presence of a gas in the gas,
the surfactant comprises at least one of sodium dodecyl sulfate, polyethylene glycol-600, polyethylene glycol-1000, polyethylene glycol-2000, sodium polyacrylate and stearic acid.
Alternatively, in step S10,
the mass of the soluble ferric salt is 0.5-3% of that of the soluble titanium salt; and/or the presence of a gas in the gas,
the mass of the soluble cerium salt is 0.5-3% of that of the soluble titanium salt; and/or the presence of a gas in the gas,
in the mixed solution, the mass fraction of the soluble titanium salt is 10-50%; and/or the presence of a gas in the gas,
in the mixed solution, the mass of the surfactant is a, the sum of the mass of the surfactant, the soluble ferric salt, the soluble cerium salt and the soluble titanium salt is b, and a/b is 0.5-5%.
Optionally, in step S20, the gas further includes nitrogen.
Optionally, the volume fraction of nitrogen in the gas is between 10% and 90%.
Optionally, step S20 includes:
and placing the mixed solution in a closed container, introducing gas containing ammonia gas to the surface of the mixed solution in the closed container under the conditions of pressurization and stirring, and reacting to obtain a solid-liquid mixture.
Optionally, the pressure for pressurizing is 0.3-1 MPa.
Alternatively, in step S30, washing is performed with an aqueous solution of a surfactant.
Optionally, in step S30, the drying condition is vacuum drying at 60-120 ℃ for 2-6 h.
Optionally, in step S30, the calcination condition is calcination at 400-650 ℃ for 1-4 h.
The technical scheme of the invention provides a preparation method of a nano titanium dioxide photocatalyst, which adopts a gas-liquid coprecipitation method, takes ammonia gas as a precipitator, and reacts with metal ions, namely iron ions, cerium ions and titanium ions in a mixed solution after the ammonia gas is diffused on the surface of the mixed solution to generate TiO (OH) doped with iron and cerium2And (3) carrying out solid-liquid separation, washing, drying and calcining on the precipitate to obtain the diion-doped nano titanium dioxide. The method is simple and easy to operate, gas-liquid interface reaction is adopted for control, the gas precipitator reacts with metal ions after being dissolved and diffused on the surface of the solution, the reaction speed of the precipitator and the metal ions is controlled by adjusting the gas, the chemical uniformity is higher, and the prepared double-ion doped nano titanium dioxide has small particle size, narrow distribution and better activity under visible light.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the structures shown in the drawings without creative efforts.
FIG. 1 is a schematic flow chart of an embodiment of a method for preparing a nano titanium dioxide photocatalyst according to the present invention;
FIG. 2 is a TEM image of the nano-titania photocatalyst obtained in example 1 of the present invention;
FIG. 3 is a TEM image of the nano-titania photocatalyst obtained in example 2 of the present invention;
FIG. 4 is a TEM image of the nano-titania photocatalyst obtained in example 3 of the present invention;
FIG. 5 is a TEM image of the nano-titania photocatalyst obtained in example 4 of the present invention;
FIG. 6 is a TEM image of the nano-titania photocatalyst obtained in example 5 of the present invention;
FIG. 7 shows UV absorption spectra of the nano-titania photocatalysts obtained in examples 1 to 5 and comparative example 1 of the present invention;
fig. 8 is a graph of the degradation of methyl orange by the nano titanium dioxide photocatalyst obtained in examples 1 to 5 and comparative example 1 of the present invention.
The implementation, functional features and advantages of the objects of the present invention will be further explained with reference to the accompanying drawings.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that, if directional indications (such as upper, lower, left, right, front, rear, outer and inner … …) are involved in the embodiment of the present invention, the directional indications are only used to explain the relative position relationship between the components, the motion situation, etc. in a specific posture (as shown in the drawing), and if the specific posture is changed, the directional indications are changed accordingly.
In addition, if there is a description of "first", "second", etc. in an embodiment of the present invention, the description of "first", "second", etc. is for descriptive purposes only and is not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In addition, the meaning of "and/or" appearing throughout includes three juxtapositions, exemplified by "A and/or B" including either A or B or both A and B. In addition, technical solutions between various embodiments may be combined with each other, but must be realized by a person skilled in the art, and when the technical solutions are contradictory or cannot be realized, such a combination should not be considered to exist, and is not within the protection scope of the present invention.
Although there are many reports that the catalytic effect of titanium dioxide under visible light is improved by doping metal ions, non-metal ions and the like, the existing multi-ion doped titanium dioxide is complex in preparation process, can be prepared by multi-step reaction, needs high-temperature hydrothermal reaction in the reaction process, has high requirements on equipment, and is poor in photocatalytic effect of the prepared product.
In view of the above, the invention provides a preparation method of a nano titanium dioxide photocatalyst, and aims to provide a simple preparation method of a photocatalyst, and the photocatalyst prepared by the method has a good photocatalytic effect. In the attached drawings, fig. 1 is a schematic flow chart of an embodiment of a preparation method of a nano titanium dioxide photocatalyst provided by the invention; FIG. 2 is a TEM image of the nano-titania photocatalyst obtained in example 1 of the present invention; FIG. 3 is a TEM image of the nano-titania photocatalyst obtained in example 2 of the present invention; FIG. 4 is a TEM image of the nano-titania photocatalyst obtained in example 3 of the present invention; FIG. 5 is a TEM image of the nano-titania photocatalyst obtained in example 4 of the present invention; FIG. 6 is a TEM image of the nano-titania photocatalyst obtained in example 5 of the present invention; FIG. 7 shows UV absorption spectra of the nano-titania photocatalysts obtained in examples 1 to 5 and comparative example 1 of the present invention; fig. 8 is a graph of the degradation of methyl orange by the nano titanium dioxide photocatalyst obtained in examples 1 to 5 and comparative example 1 of the present invention.
Referring to fig. 1, the method for preparing a nano titanium dioxide photocatalyst provided by the present invention is characterized by comprising the following steps:
s10, dissolving soluble ferric salt, soluble cerium salt, soluble titanium salt and surfactant in water to obtain a mixed solution.
In this step, the iron salt, cerium salt and titanium salt which participate in the reaction are dissolved in water to perform the subsequent gas-liquid reaction, and the types of the soluble iron salt, the soluble cerium salt and the soluble titanium salt are not limited in the present invention.
The soluble titanium salt preferably comprises any one of titanium sulfate and titanyl sulfate, the titanium sulfate and titanyl sulfate are easily dissolved in water, the aqueous solution is easily hydrolyzed, and the subsequent ammonia gas is conveniently introduced to generate TiO (OH)2And (4) precipitating.
In the embodiment of the present invention, the addition of the surfactant makes the precipitate not easy to agglomerate, which is beneficial for forming the precipitate with smaller particles and uniform particle size, and the kind of the surfactant is not limited in the present invention, and preferably, the surfactant includes at least one of sodium dodecyl sulfate, polyethylene glycol-600, polyethylene glycol-1000, polyethylene glycol-2000, sodium polyacrylate, and stearic acid. At least one of the substances is used as a surfactant, so that the nano titanium dioxide photocatalyst with uniform particle size is formed.
It is understood that, in the above polyethylene glycol-600, polyethylene glycol-1000 and polyethylene glycol-2000, the number following the polyethylene glycol represents the average molecular weight.
The invention is not limited to the mixture ratio of each component in the mixed solution, and preferably, the mass of the soluble ferric salt is 0.5-3% of that of the soluble titanium salt; the adding mass of the soluble cerium salt is 0.5-3% of that of the soluble titanium salt; in the mixed solution, the mass fraction of the soluble titanium salt is 10-50%; in the mixed solution, the mass of the surfactant is a, the sum of the mass of the surfactant, the soluble ferric salt, the soluble cerium salt and the soluble titanium salt is b, and a/b is 0.5-5%. Experiments show that the obtained nano titanium dioxide photocatalyst has high catalytic activity in the proportion.
It can be understood that the addition amount ranges of the soluble iron salt, the soluble cerium salt, the soluble titanium salt and the surfactant can simultaneously satisfy one of the conditions, preferably, the conditions are simultaneously satisfied, and the obtained nano titanium dioxide photocatalyst has the highest catalytic activity.
And S20, under the condition of stirring, introducing gas containing ammonia gas into the mixed solution, and reacting to obtain a solid-liquid mixture.
In this step, ammonia gas is introduced into the mixed solution to perform a gas-liquid reaction, and in order to uniformly generate titanium dioxide, it is preferable that the gas further includes nitrogen gas, and the nitrogen gas is used as a carrier gas, which can dilute the ammonia gas and prevent the precipitate from being rapidly generated due to an excessively high ammonia gas concentration, thereby affecting the particle size.
More preferably, the volume fraction of nitrogen in the gas is between 10% and 90%. Under the above addition amount, the nanometer titanium dioxide photocatalyst with moderate and uniform particle size can be obtained.
The method of introducing the nitrogen-containing gas into the mixed liquid is not limited in the present invention, and the nitrogen-containing gas may be introduced by extending the gas-guide tube into the mixed liquid, or, in an embodiment of the present invention, the nitrogen-containing gas is introduced into the surface of the mixed liquid, specifically, step S20 includes:
and placing the mixed solution in a closed container, introducing gas containing ammonia gas to the surface of the mixed solution in the closed container under the conditions of pressurization and stirring, and reacting to obtain a solid-liquid mixture.
And in addition, under the condition of pressurized stirring, ammonia molecules are rapidly diffused into the mixed solution to participate in the reaction, the reaction speed of the ammonia and metal ions is regulated and controlled, and the obtained nano titanium dioxide photocatalyst has higher chemical uniformity.
Preferably, the pressurizing pressure is 0.3 to 1 MPa. For example, the photocatalyst may be 0.3MPa, 0.4MPa, 0.5MPa, 0.6MPa, 0.7MPa, 0.8MPa, 0.9MPa, 1MPa or the like, and experiments have shown that the obtained photocatalyst has good photocatalytic effect and high catalytic activity under the above-mentioned pressure.
And S30, carrying out solid-liquid separation on the solid-liquid mixture to obtain a solid, washing, drying and calcining the solid to obtain the nano titanium dioxide photocatalyst.
In the step, the obtained double-ion doped nano TiO (OH)2And separating from the solid-liquid mixed solution, washing, drying and calcining to obtain the nano titanium dioxide photocatalyst.
Preferably, the washing is carried out using an aqueous solution containing a surfactant. When washing, the nano TiO (OH) doped with double ions is easy to be mixed2The surface surfactant is washed away, thereby causing the double-ion doped nano TiO (OH)2Agglomeration, in the present example, washing with an aqueous solution of a surfactant, enables the diion-doped nano TiO (OH)2The surface of (2) always has the surfactant, and agglomeration cannot occur.
The surfactant can be at least one of sodium dodecyl sulfate, polyethylene glycol-600, polyethylene glycol-1000, polyethylene glycol-2000, sodium polyacrylate and stearic acid, and the surfactant can be decomposed by heating in the subsequent calcining step without affecting the purity of the double-ion doped nano titanium dioxide.
Preferably, the drying condition is vacuum drying at 60-120 ℃ for 2-6 h. Vacuum drying nanometer TiO (OH) capable of preventing double ions from being doped2React with substances in the air under heating to cause deterioration.
Preferably, the calcination condition is calcination at 400-650 ℃ for 1-4 h. The calcination is to make TiO (OH)2And (3) dehydrating to generate titanium dioxide, wherein the generated double-ion doped nano titanium dioxide has uniform particle size and good activity under the calcining condition.
The technical scheme of the invention provides a preparation method of a nano titanium dioxide photocatalyst, which adopts a gas-liquid coprecipitation method, takes ammonia gas as a precipitator, and reacts with metal ions, namely iron ions, cerium ions and titanium ions in a mixed solution after the ammonia gas is diffused on the surface of the mixed solution to generate TiO (OH) doped with iron and cerium2Precipitating, and solidifying the precipitateAnd (3) carrying out liquid separation, washing, drying and calcining to obtain the diionic doped nano titanium dioxide. The method is simple, easy to operate and low in cost, and adopts gas-liquid interface reaction for control, the gas precipitator reacts with metal ions after being dissolved and diffused on the surface of the solution, the reaction speed of the precipitator and the metal ions is controlled by adjusting the gas, the chemical uniformity is higher, and the prepared double-ion doped nano titanium dioxide has small particle size, narrow distribution and better activity under visible light.
An embodiment of the preparation method of the nano titanium dioxide photocatalyst provided by the invention is given as follows:
(1) dissolving ferric nitrate, cerium nitrate, soluble titanium salt (titanium sulfate or titanyl sulfate) and a surfactant (at least one of sodium dodecyl sulfate, polyethylene glycol-600, polyethylene glycol-1000, polyethylene glycol-2000, sodium polyacrylate and stearic acid) in water to obtain a mixed solution, wherein the mass of the soluble ferric salt is 0.5-3% of that of the soluble titanium salt, the mass of the soluble cerium salt is 0.5-3% of that of the soluble titanium salt, the mass fraction of the soluble titanium salt in the mixed solution is 10-50%, the mass of the surfactant in the mixed solution is a, the sum of the mass of the surfactant, the soluble ferric salt, the soluble cerium salt and the soluble titanium salt is b, and the a/b is 0.5-5%;
(2) placing the mixed solution in a closed container, introducing a gas containing ammonia and nitrogen to the surface of the mixed solution in the closed container under the conditions of pressurization of 0.3-1 MPa and stirring, and reacting to obtain a solid-liquid mixture, wherein the volume fraction of nitrogen in the gas is 10% -90%;
(3) and filtering the solid-liquid mixture to obtain a solid, washing the solid with a water solution of a surfactant, drying the solid in vacuum at the temperature of 60-120 ℃ for 2-6 hours, and calcining the solid at the temperature of 400-650 ℃ for 1-4 hours to obtain the nano titanium dioxide photocatalyst.
The technical solutions of the present invention are further described in detail with reference to the following specific examples, which should be understood as merely illustrative and not limitative.
Example 1
(1) Dissolving ferric nitrate, cerous nitrate, titanium sulfate and a surfactant (sodium dodecyl sulfate) in water to obtain a mixed solution, wherein the mass of a soluble ferric salt is 0.5% of the mass of a soluble titanium salt, the mass of a soluble cerium salt is 0.5% of the mass of the soluble titanium salt, the mass fraction of the soluble titanium salt in the mixed solution is 10%, the mass of the surfactant in the mixed solution is a, the sum of the masses of the surfactant, the soluble ferric salt, the soluble cerium salt and the soluble titanium salt is b, and a/b is 0.5%;
(2) placing the mixed solution in a closed container, introducing gas containing ammonia and nitrogen to the surface of the mixed solution in the closed container under the conditions of pressurization of 0.3MPa and stirring, and reacting to obtain a solid-liquid mixture, wherein the volume fraction of nitrogen in the gas is 10%;
(3) filtering the solid-liquid mixture to obtain a solid, washing the solid with a water solution of a surfactant, drying the solid in vacuum at 60 ℃ for 6 hours, and calcining the solid at 400 ℃ for 4 hours to obtain the nano titanium dioxide photocatalyst.
Through particle size test, the average particle size of the nano titanium dioxide photocatalyst is 28nm, and the dispersion of the particle size distribution is 0.43, which shows that the nano titanium dioxide photocatalyst has uniform particle size distribution.
The nano titanium dioxide photocatalyst is subjected to a transmission electron microscope to obtain a graph 2, and the particle size of the nano titanium dioxide photocatalyst is within 50nm and is uniform.
Example 2
(1) Dissolving ferric nitrate, cerium nitrate, titanyl sulfate and a surfactant (sodium dodecyl sulfate, polyethylene glycol-600) in water to obtain a mixed solution, wherein the mass of a soluble ferric salt is 3% of the mass of a soluble titanium salt, the mass of a soluble cerium salt is 3% of the mass of the soluble titanium salt, the mass fraction of the soluble titanium salt in the mixed solution is 50%, the mass of the surfactant in the mixed solution is a, the sum of the masses of the surfactant, the soluble ferric salt, the soluble cerium salt and the soluble titanium salt is b, and a/b is 5%;
(2) placing the mixed solution in a closed container, introducing gas containing ammonia and nitrogen to the surface of the mixed solution in the closed container under the conditions of pressurization of 1MPa and stirring, and reacting to obtain a solid-liquid mixture, wherein the volume fraction of nitrogen in the gas is 90%;
(3) filtering the solid-liquid mixture to obtain a solid, washing the solid with a water solution of a surfactant, drying the solid in vacuum at 120 ℃ for 2h, and calcining the solid at 650 ℃ for 1h to obtain the nano titanium dioxide photocatalyst.
Through particle size test, the average particle size of the nano titanium dioxide photocatalyst is 32nm, and the dispersion of the particle size distribution is 0.56, which shows that the nano titanium dioxide photocatalyst has uniform particle size distribution.
The nano titanium dioxide photocatalyst is subjected to a transmission electron microscope to obtain a graph 3, and it can be seen that the particle size of the nano titanium dioxide photocatalyst is within 50nm and is uniform.
Example 3
(1) Dissolving ferric nitrate, cerium nitrate, titanium sulfate and a surfactant (polyethylene glycol-1000, polyethylene glycol-2000, sodium polyacrylate and stearic acid) in water to obtain a mixed solution, wherein the mass of a soluble ferric salt is 1.7% of that of a soluble titanium salt, the mass of a soluble cerium salt is 1.8% of that of the soluble titanium salt, the mass fraction of the soluble titanium salt in the mixed solution is 30%, the mass of the surfactant in the mixed solution is a, the sum of the masses of the surfactant, the soluble ferric salt, the soluble cerium salt and the soluble titanium salt is b, and the a/b is 2.8%;
(2) placing the mixed solution in a closed container, introducing gas containing ammonia and nitrogen to the surface of the mixed solution in the closed container under the conditions of pressurization of 0.7MPa and stirring, and reacting to obtain a solid-liquid mixture, wherein the volume fraction of nitrogen in the gas is 50%;
(3) filtering the solid-liquid mixture to obtain a solid, washing the solid with a water solution of a surfactant, drying the solid in vacuum at 90 ℃ for 4 hours, and calcining the solid at 525 ℃ for 2.5 hours to obtain the nano titanium dioxide photocatalyst.
Through particle size test, the average particle size of the nano titanium dioxide photocatalyst is 26nm, and the dispersion of the particle size distribution is 0.49, which shows that the nano titanium dioxide photocatalyst has uniform particle size distribution.
The nano titanium dioxide photocatalyst is subjected to a transmission electron microscope to obtain a graph shown in figure 4, and the particle size of the nano titanium dioxide photocatalyst is within 50nm and is uniform.
Example 4
(1) Dissolving ferric nitrate, cerium nitrate, titanyl sulfate and a surfactant (sodium dodecyl sulfate, polyethylene glycol-600, polyethylene glycol-1000, polyethylene glycol-2000, sodium polyacrylate and stearic acid) in water to obtain a mixed solution, wherein the mass of a soluble ferric salt is 1.8% of that of a soluble titanium salt, the mass of a soluble cerium salt is 1.7% of that of the soluble titanium salt, the mass fraction of the soluble titanium salt in the mixed solution is 40%, the mass of the surfactant in the mixed solution is a, the sum of the masses of the surfactant, the soluble ferric salt, the soluble cerium salt and the soluble titanium salt is b, and a/b is 2.7%;
(2) placing the mixed solution in a closed container, introducing gas containing ammonia and nitrogen to the surface of the mixed solution in the closed container under the conditions of pressurization of 0.8MPa and stirring, and reacting to obtain a solid-liquid mixture, wherein the volume fraction of nitrogen in the gas is 70%;
(3) filtering the solid-liquid mixture to obtain a solid, washing the solid with a water solution of a surfactant, drying the solid in vacuum at 100 ℃ for 3h, and calcining the solid at 500 ℃ for 2h to obtain the nano titanium dioxide photocatalyst.
Through particle size test, the average particle size of the nano titanium dioxide photocatalyst is 30nm, and the dispersion of the particle size distribution is 0.62, which shows that the nano titanium dioxide photocatalyst has uniform particle size distribution.
The nano titanium dioxide photocatalyst is subjected to a transmission electron microscope to obtain a graph 5, and the particle size of the nano titanium dioxide photocatalyst is within 50nm and is uniform.
Example 5
(1) Dissolving ferric nitrate, cerium nitrate, titanium sulfate and a surfactant (polyethylene glycol-1000, polyethylene glycol-2000, sodium polyacrylate and stearic acid) in water to obtain a mixed solution, wherein the mass of a soluble ferric salt is 2% of that of a soluble titanium salt, the mass of a soluble cerium salt is 1% of that of the soluble titanium salt, the mass fraction of the soluble titanium salt in the mixed solution is 20%, the mass of the surfactant in the mixed solution is a, the sum of the masses of the surfactant, the soluble ferric salt, the soluble cerium salt and the soluble titanium salt is b, and a/b is 3%;
(2) placing the mixed solution in a closed container, introducing gas containing ammonia and nitrogen to the surface of the mixed solution in the closed container under the conditions of pressurization of 0.5MPa and stirring, and reacting to obtain a solid-liquid mixture, wherein the volume fraction of nitrogen in the gas is 30%;
(3) filtering the solid-liquid mixture to obtain a solid, washing the solid with a water solution of a surfactant, drying the solid in vacuum at 80 ℃ for 3h, and calcining the solid at 600 ℃ for 2h to obtain the nano titanium dioxide photocatalyst.
Through particle size test, the average particle size of the nano titanium dioxide photocatalyst is 34nm, and the dispersion of the particle size distribution is 0.58, which shows that the nano titanium dioxide photocatalyst has uniform particle size distribution.
A transmission electron microscope is carried out on the nano titanium dioxide photocatalyst to obtain a graph 6, and it can be seen that the particle size of the nano titanium dioxide photocatalyst is within 50nm and is uniform.
The ultraviolet absorption spectrum of the nano-titania photocatalyst obtained in examples 1 to 5 of the present invention and comparative example 1 was measured using a commercially available titania P25 as comparative example 1, and fig. 7 was obtained.
Referring to fig. 7, it can be seen that the titanium dioxide of comparative example 1 has a large absorbance under the ultraviolet light below 400nm, and the absorbance under the visible light between 400nm and 780nm is almost zero, which indicates that the photocatalytic activity of comparative example 1 under the visible light is almost zero; the nano titanium dioxide photocatalyst of the embodiments 1 to 5 has better absorbance under ultraviolet light and visible light, which shows that the photocatalyst has photocatalytic activity.
The nano titanium dioxide photocatalysts obtained in examples 1 to 5 and comparative example 1 were tested as follows:
taking 100mL of methyl orange solution with the concentration of 10mg/L, repeating for 6 times, respectively adding the titanium dioxide of the invention in the embodiments 1-5 and the comparative example 1 into the beaker, respectively adding the titanium dioxide of the invention in the final solution with the concentration of 1.8g/L, stirring at constant temperature for 30min, performing ultrasound for 30min, then respectively placing under visible light (xenon lamp simulated sunlight) for irradiation, continuously performing magnetic stirring in the irradiation process, sampling and centrifuging at intervals, taking the centrifuged supernatant for testing absorbance, comparing the absorbance with the absorbance of the original methyl orange solution, and obtaining a degradation graph, wherein the ratio of the difference value to the absorbance of the original solution is the degradation rate of the methyl orange solution, and the graph is shown in figure 8.
As can be seen from FIG. 8, under the irradiation of visible light, the degradation rate of the titanium dioxide of the comparative example on methyl orange is very small, and the degradation rate reaches up to 12% after 120min of illumination, while the Fe and Ce double-ion doped TiO of the embodiment of the invention2The photocatalyst is a photocatalyst, the degradation rate of the methyl orange is almost linearly increased along with the degradation time, and the degradation rate reaches about 72% after the irradiation of light for 3 hours, so that the nano titanium dioxide photocatalyst prepared by the embodiment of the invention has obvious advantages in photocatalytic degradation of the methyl orange under visible light.
In conclusion, the nano titanium dioxide photocatalyst prepared by the embodiment of the invention has small particle size, uniform distribution and better catalytic activity under visible light, is controlled by adopting gas-liquid interface reaction, and has the advantages of simple preparation method, easy operation, low cost and wide application prospect.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention, and all modifications and equivalents of the present invention, which are made by the contents of the present specification and the accompanying drawings, or directly/indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (10)
1. A preparation method of a nanometer titanium dioxide photocatalyst is characterized by comprising the following steps:
s10, dissolving soluble ferric salt, soluble cerium salt, soluble titanium salt and a surfactant in water to obtain a mixed solution;
s20, under the condition of stirring, introducing gas containing ammonia gas into the mixed solution, and reacting to obtain a solid-liquid mixture;
and S30, carrying out solid-liquid separation on the solid-liquid mixture to obtain a solid, washing, drying and calcining the solid to obtain the nano titanium dioxide photocatalyst.
2. The method for preparing nano titanium dioxide photocatalyst as claimed in claim 1, wherein in step S10,
the soluble ferric salt comprises ferric nitrate; and/or the presence of a gas in the gas,
the soluble cerium salt comprises cerium nitrate; and/or the presence of a gas in the gas,
the soluble titanium salt comprises any one of titanium sulfate and titanyl sulfate; and/or the presence of a gas in the gas,
the surfactant comprises at least one of sodium dodecyl sulfate, polyethylene glycol-600, polyethylene glycol-1000, polyethylene glycol-2000, sodium polyacrylate and stearic acid.
3. The method for preparing nano titanium dioxide photocatalyst as claimed in claim 1, wherein in step S10,
the mass of the soluble ferric salt is 0.5-3% of that of the soluble titanium salt; and/or the presence of a gas in the gas,
the mass of the soluble cerium salt is 0.5-3% of that of the soluble titanium salt; and/or the presence of a gas in the gas,
in the mixed solution, the mass fraction of the soluble titanium salt is 10-50%; and/or the presence of a gas in the gas,
in the mixed solution, the mass of the surfactant is a, the sum of the mass of the surfactant, the soluble ferric salt, the soluble cerium salt and the soluble titanium salt is b, and a/b is 0.5-5%.
4. The method of claim 1, wherein in step S20, the gas further comprises nitrogen.
5. The method of claim 4, wherein the volume fraction of nitrogen in the gas is 10% to 90%.
6. The method for preparing a nano titanium dioxide photocatalyst as claimed in claim 1, wherein the step S20 includes:
and placing the mixed solution in a closed container, introducing gas containing ammonia gas to the surface of the mixed solution in the closed container under the conditions of pressurization and stirring, and reacting to obtain a solid-liquid mixture.
7. The method for preparing the nano titanium dioxide photocatalyst according to claim 6, wherein the pressure for pressurization is 0.3 to 1 MPa.
8. The method of claim 1, wherein in step S30, the nano titanium dioxide photocatalyst is washed with an aqueous solution of a surfactant.
9. The method for preparing the nano titanium dioxide photocatalyst according to claim 1, wherein in step S30, the drying condition is vacuum drying at 60 to 120 ℃ for 2 to 6 hours.
10. The method for preparing the nano titanium dioxide photocatalyst according to claim 1, wherein in step S30, the calcination is performed at 400 to 650 ℃ for 1 to 4 hours.
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