CN112871168A - Preparation method of one-dimensional magnetic nano photocatalyst - Google Patents
Preparation method of one-dimensional magnetic nano photocatalyst Download PDFInfo
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 23
- 230000001699 photocatalysis Effects 0.000 claims abstract description 23
- 239000002105 nanoparticle Substances 0.000 claims abstract description 19
- 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 claims abstract description 13
- 229960000907 methylthioninium chloride Drugs 0.000 claims abstract description 13
- 239000002243 precursor Substances 0.000 claims abstract description 10
- 230000009471 action Effects 0.000 claims abstract description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000002131 composite material Substances 0.000 claims abstract description 5
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 5
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 4
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 4
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 4
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 4
- 239000010703 silicon Substances 0.000 claims abstract description 4
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 4
- 239000010936 titanium Substances 0.000 claims abstract description 4
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 4
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 4
- 238000011065 in-situ storage Methods 0.000 claims abstract 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical group OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 8
- 238000007146 photocatalysis Methods 0.000 claims description 8
- 239000004408 titanium dioxide Substances 0.000 claims description 8
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 7
- 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 description 7
- 238000005406 washing Methods 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 3
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 2
- 230000000593 degrading effect Effects 0.000 claims description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 claims 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000000758 substrate Substances 0.000 claims 1
- 239000003054 catalyst Substances 0.000 abstract description 5
- 230000015556 catabolic process Effects 0.000 abstract description 4
- 238000006731 degradation reaction Methods 0.000 abstract description 4
- 230000003197 catalytic effect Effects 0.000 abstract description 3
- 240000007594 Oryza sativa Species 0.000 abstract 1
- 235000007164 Oryza sativa Nutrition 0.000 abstract 1
- 238000002474 experimental method Methods 0.000 abstract 1
- 239000011943 nanocatalyst Substances 0.000 abstract 1
- 235000009566 rice Nutrition 0.000 abstract 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 18
- 238000001878 scanning electron micrograph Methods 0.000 description 11
- 238000006243 chemical reaction Methods 0.000 description 10
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- 239000002122 magnetic nanoparticle Substances 0.000 description 8
- 239000000203 mixture Substances 0.000 description 7
- 238000001816 cooling Methods 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- 238000002156 mixing Methods 0.000 description 5
- 238000001338 self-assembly Methods 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000010335 hydrothermal treatment Methods 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 230000005389 magnetism Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- CDVAIHNNWWJFJW-UHFFFAOYSA-N 3,5-diethoxycarbonyl-1,4-dihydrocollidine Chemical compound CCOC(=O)C1=C(C)NC(C)=C(C(=O)OCC)C1C CDVAIHNNWWJFJW-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000008034 disappearance Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000007885 magnetic separation Methods 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229940031182 nanoparticles iron oxide Drugs 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- 238000004729 solvothermal method Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000007039 two-step reaction Methods 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
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- 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
- B01J23/74—Iron group metals
- B01J23/745—Iron
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- 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
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Abstract
The invention provides a preparation method of a one-dimensional magnetic nano photocatalyst, which comprises the following steps: (1) preparation of uniform size by solvothermal methodFe (b) of3O4Nanoparticles; (2) regulation of Fe by magnetic field3O4The nano particles are self-assembled under the action of magnetic force lines, and simultaneously, the titanium source and the silicon source are subjected to room temperature hydrolysis reaction and coated in situ on the surfaces thereof to form TiO2/SiO2Thereby preparing a one-dimensional magnetic nano precursor; (3) and (3) carrying out hydrothermal reaction on the nano precursor in the step (2) to finally obtain the one-dimensional magnetic nano photocatalyst with photocatalytic activity. The invention also provides an application of the one-dimensional magnetic rice catalyst, and methylene blue light catalytic degradation experiments prove that the prepared novel composite nano catalyst has good photocatalytic effect.
Description
Technical Field
The invention belongs to the technical field of inorganic nano materials, and particularly discloses a preparation method of a one-dimensional magnetic nano photocatalyst.
Background
Magnetic nanoparticles, such as iron, cobalt, nickel nanoparticles, iron oxide nanoparticles, etc., are widely noted in the fields of optics, electronics, magnetism, etc. due to their unique surface effects, quantum size effects, and magnetic properties. Magnetic nanoparticles can be assembled by means of "dipole-dipole" interaction between the particles under the action of magnetic force lines, but the force disappears along with the disappearance of the magnetic field, so that the magnetic nanoparticles need to be fixed in a proper way to form a stable one-dimensional magnetic nanomaterial.
In recent years, various materials such as polymers and inorganic substances have been used to coat magnetic nanoparticles to prepare one-dimensional magnetic nanomaterials. Wherein, the titanium dioxide is an inorganic functional material with stable chemical property and resistance to photochemistry and acid-base corrosion. How to coat titanium dioxide on the surface of ferroferric oxide nanoparticles can not only utilize the advantage of magnetism, but also solve the problem that the titanium dioxide is difficult to recover; the photocatalytic activity of titanium dioxide can also be utilized to be applied to the field of photocatalysis.
Disclosure of Invention
The invention aims to provide a preparation method of a stable one-dimensional titanium dioxide coated magnetic nano photocatalyst, which specifically comprises the following steps of:
1. preparation of uniform-sized Fe by solvothermal method3O4Nanoparticles;
2. by regulation of magnetic fieldFe3O4The nano particles are self-assembled under the action of magnetic force lines, and simultaneously, a titanium source and a silicon source are subjected to room temperature hydrolysis reaction to be coated on the surfaces of the nano particles to form TiO2/SiO2Thereby preparing a one-dimensional magnetic nano precursor;
3. and carrying out hydrothermal reaction on the one-dimensional nano precursor to finally obtain the one-dimensional magnetic nano photocatalyst with photocatalytic activity.
Preferably, the raw material of the step (1) is anhydrous ferric chloride, and the solvent is ethylene glycol; fe3O4The size of the nanoparticles is 40-120 nm;
preferably, in the step (2), the silicon source is tetraethyl orthosilicate, and the titanium source is tetrabutyl titanate with a ratio of 1: 9-4: 1;
preferably, the hydrothermal reaction temperature in the step (3) is 160-200 ℃, and the time is 6-18 h.
The invention also aims to provide application of the one-dimensional magnetic nano photocatalyst. The photocatalysis of the titanium dioxide of the catalyst under the condition of normal temperature illumination is researched by using methylene blue light for catalytic degradation.
Compared with the prior art, the invention has the advantages that:
1. under the action of magnetic force lines, the magnetic nano particles are firstly coated at room temperature to form a titanium dioxide/silicon dioxide composite oxide shell, and then hydrothermal treatment is carried out, so that the one-dimensional magnetic nano photocatalyst with photocatalytic activity is obtained.
2. The one-dimensional magnetic nano photocatalyst prepared by the invention can be used for degrading methylene blue by the catalyst. The novel composite photocatalyst not only has TiO2Has photocatalytic activity of, and has Fe3O4The magnetic property of the nano particles has good photocatalysis effect and is beneficial to recycling of samples.
Drawings
FIG. 1 is an SEM image of magnetic nanoparticles prepared according to the present invention.
FIG. 2 is an SEM image of a one-dimensional magnetic nano-photocatalyst in example 1 of the present invention.
FIG. 3 is an SEM image of a one-dimensional magnetic nano-photocatalyst in example 2 of the present invention.
FIG. 4 is an SEM image of a one-dimensional magnetic nano-photocatalyst in example 3 of the present invention.
FIG. 5 is an SEM image of a one-dimensional magnetic nano-photocatalyst in example 4 of the present invention.
FIG. 6 is an SEM image of a one-dimensional magnetic nano-photocatalyst in example 5 of the present invention.
Fig. 7 is an ultraviolet-visible absorption curve of the methylene blue solution under the irradiation of an ultraviolet lamp by the one-dimensional magnetic nano photocatalyst according to example 3 of the present invention, which changes with time.
FIG. 8 is a graph of the rate of methylene blue degradation for different photocatalytic samples of examples 1 and 3 of the present invention.
Detailed Description
The present invention is further illustrated below by means of specific embodiments, but the embodiments of the present invention are not limited thereto.
Fe3O4Preparing nano particles: firstly, 0.98g of ferric acetylacetonate and 0.30g of sodium citrate are weighed and dissolved in 30mL of glycol; then 1.8g of urea is added, the mixture is evenly dissolved by ultrasonic waves and then transferred to a 50mL reaction kettle, and the reaction kettle is placed in an oven for reaction for 12 hours at 200 ℃. Cooling to room temperature after the reaction is finished, washing for many times by deionized water and ethanol, separating by a magnet, and drying in vacuum at 60 ℃ to obtain Fe3O4And (3) nanoparticles. FIG. 1 shows Fe prepared by the present invention3O4SEM image of magnetic nanoparticles.
Example 1
2mg of self-made Fe3O4Adding the nano particles into 10mL of ethanol, and uniformly dispersing by ultrasonic; sequentially adding 150 mu L of tetrabutyl titanate, 225 mu L of ethyl orthosilicate and 600 mu L of ammonia water, fully shaking and mixing uniformly; the solution was then placed about 5cm above a magnet for self-assembly overnight. Washing with ethanol and water in sequence, and separating with a magnet to obtain the one-dimensional magnetic nano precursor. 5mL of deionized water was added, and the mixture was transferred to a reaction kettle and reacted at 160 ℃ for 12 hours. Cooling to room temperature, and separating by a magnet to obtain the one-dimensional magnetic nano photocatalyst with photocatalytic activity. FIG. 2 shows example 1 of the present inventionSEM image of medium-dimensional magnetic nano photocatalyst.
2mg of catalyst is added into 30mL of methylene blue solution with the concentration of 10mg/L, and the mixture is ultrasonically dispersed to form uniform solution which is irradiated under a 300W high-pressure mercury lamp for different reaction times. The reaction solution was taken out, and the photocatalyst was removed by magnetic separation. And testing the change of the absorption curve of methylene blue in the supernatant through UV-Vis, wherein the wavelength range is 200-800 nm.
Example 2
2mg of self-made Fe3O4Adding nanoparticles into 10mL of ethanol, ultrasonically dispersing uniformly, adding 187.5 mu L of tetrabutyl titanate and 187.5 mu L of ethyl orthosilicate, and fully shaking and uniformly mixing; the solution was then placed about 5cm above a magnet for self-assembly overnight. Washing with ethanol and water in sequence, and separating with a magnet to obtain the one-dimensional magnetic nano precursor. 5mL of deionized water was added, and the mixture was transferred to a reaction kettle and reacted at 160 ℃ for 16 hours. Cooling to room temperature, and separating by a magnet to obtain the one-dimensional magnetic nano photocatalyst with photocatalytic activity. FIG. 3 is an SEM image of a one-dimensional magnetic nano-photocatalyst in example 2 of the present invention. The photocatalytic degradation of methylene blue was performed as in example 1.
Example 3
2mg of self-made Fe3O4Adding the nano particles into 10mL of ethanol, and uniformly dispersing by ultrasonic; adding 225 μ L tetrabutyl titanate and 150 μ L ethyl orthosilicate, and fully shaking and mixing uniformly; the solution was then placed about 5cm above a magnet for self-assembly overnight. Washing with ethanol and water in sequence, and separating with a magnet to obtain the one-dimensional magnetic nano precursor. 5mL of deionized water was added, and the mixture was transferred to a reaction kettle and reacted at 180 ℃ for 18 hours. Cooling to room temperature, and separating by a magnet to obtain the one-dimensional magnetic nano photocatalyst with photocatalytic activity. FIG. 4 is an SEM image of a one-dimensional magnetic nano-photocatalyst in example 3 of the present invention. The photocatalytic degradation of methylene blue was performed as in example 1. FIG. 7 is a graph of the UV-Vis absorption of a methylene blue solution under UV lamp illumination over time for a sample of the present invention.
Example 4
2mg of self-made Fe3O4Nanoparticles, adding 10mL ethanolIn the middle, the ultrasonic dispersion is uniform; adding 281 mu L tetrabutyl titanate and 94 mu L ethyl orthosilicate, fully shaking and mixing uniformly; the solution was then placed about 5cm above a magnet for self-assembly overnight. Washing with ethanol and water in sequence, and separating with a magnet to obtain the one-dimensional magnetic nano precursor. 5mL of deionized water was added, and the mixture was transferred to a reaction vessel and reacted at 180 ℃ for 12 hours. And cooling to room temperature, and separating by using a magnet to obtain the one-dimensional magnetic nano photocatalyst with photocatalytic activity. FIG. 5 is an SEM image of a one-dimensional magnetic nano-photocatalyst in example 4 of the present invention. Photocatalytic degradation of methylene blue was performed as in example 1.
Example 5
2mg of self-made Fe3O4Adding the nano particles into 10mL of ethanol, and uniformly dispersing by ultrasonic; adding 337.5 μ L tetrabutyl titanate and 37.5 μ L ethyl orthosilicate, and sufficiently shaking and mixing uniformly; the solution was then placed about 5cm above a magnet for self-assembly overnight. 5mL of deionized water was added, and the mixture was transferred to a reaction kettle and reacted at 160 ℃ for 18 hours. And cooling to room temperature, and separating by using a magnet to obtain the one-dimensional magnetic nano photocatalyst with photocatalytic activity. FIG. 6 is an SEM image of a one-dimensional magnetic nano-photocatalyst in example 5 of the present invention. The photocatalytic degradation of methylene blue was performed as in example 1.
The invention adopts Fe3O4Under the action of magnetic force lines, the magnetic nano particles are successfully coated with TiO on the surface of the assembly through two-step reaction of room-temperature hydrolysis and high-temperature hydrothermal treatment2/SiO2Compounding oxide shell to prepare the one-dimensional magnetic nanometer photocatalysis composite material. The catalyst can realize the blue light catalytic degradation of methylene, can be repeatedly recycled, and has a good prospect in the field of photocatalysis.
In light of the foregoing description of the preferred embodiment of the present invention, many modifications and variations will be apparent to those skilled in the art without departing from the spirit and scope of the invention. The technical scope of the present invention is not limited to the content of the specification, and must be determined by determining the technical scope thereof according to the scope of the claims.
Claims (5)
1. A preparation method of a one-dimensional magnetic nano photocatalyst has the following characteristics that:
(1) production of Fe by the solution thermal method3O4Nanoparticles;
(2) regulation of Fe by magnetic field3O4The nano particles are self-assembled under the action of magnetic force lines, and simultaneously, the titanium source and the silicon source are subjected to room temperature hydrolysis reaction and coated in situ on the surfaces thereof to form TiO2/SiO2Washing and separating the composite oxide shell to obtain a one-dimensional magnetic nano precursor;
(3) and carrying out hydrothermal reaction on the one-dimensional magnetic nano precursor to finally obtain the one-dimensional magnetic nano photocatalyst with photocatalytic activity.
2. The preparation method of one-dimensional magnetic nano photocatalysis according to claim 1, wherein the raw material in step (1) is anhydrous ferric chloride, and the solvent is ethylene glycol; the size of the obtained nano particles is 40-120 nm.
3. The preparation method of one-dimensional magnetic nano photocatalysis according to claim 1, wherein the raw materials in the step (2) are tetraethoxysilane and tetrabutyl titanate with a ratio of 1: 9-4: 1.
4. The method as claimed in claim 1, wherein the hydrothermal reaction is carried out at 160-200 ℃ for 6-18 h.
5. The application of the one-dimensional magnetic nano photocatalyst is characterized in that the prepared novel one-dimensional magnetic nano photocatalyst is added into a model substrate solution, and the photocatalytic performance of the photocatalyst is researched by degrading methylene blue through photocatalysis by utilizing the photocatalytic action of titanium dioxide.
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