CN111617777A - Indoor visible light response catalyst, preparation method and application thereof - Google Patents
Indoor visible light response catalyst, preparation method and application thereof Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 230000004298 light response Effects 0.000 title claims abstract description 19
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 40
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000006731 degradation reaction Methods 0.000 claims abstract description 11
- 230000015556 catabolic process Effects 0.000 claims abstract description 10
- 238000003980 solgel method Methods 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 93
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 69
- 239000008367 deionised water Substances 0.000 claims description 55
- 229910021641 deionized water Inorganic materials 0.000 claims description 55
- 239000000843 powder Substances 0.000 claims description 39
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 36
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 18
- 238000005406 washing Methods 0.000 claims description 18
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 17
- 239000001257 hydrogen Substances 0.000 claims description 17
- 229910052739 hydrogen Inorganic materials 0.000 claims description 17
- 238000002156 mixing Methods 0.000 claims description 17
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 13
- 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 12
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- 238000003756 stirring Methods 0.000 claims description 10
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- 239000002253 acid Substances 0.000 claims description 9
- 238000013329 compounding Methods 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 9
- 229910017604 nitric acid Inorganic materials 0.000 claims description 9
- -1 polytetrafluoroethylene Polymers 0.000 claims description 9
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 9
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 9
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- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 9
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 9
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- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 8
- 239000012279 sodium borohydride Substances 0.000 claims description 7
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 7
- 239000002131 composite material Substances 0.000 claims description 6
- 229910052742 iron Inorganic materials 0.000 claims description 6
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 4
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 4
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 4
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 4
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims description 4
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 239000010936 titanium Substances 0.000 claims description 4
- 229910052719 titanium Inorganic materials 0.000 claims description 4
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 claims description 3
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims description 3
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 2
- 239000011668 ascorbic acid Substances 0.000 claims description 2
- 229960005070 ascorbic acid Drugs 0.000 claims description 2
- 235000010323 ascorbic acid Nutrition 0.000 claims description 2
- 239000003153 chemical reaction reagent Substances 0.000 claims description 2
- 239000003638 chemical reducing agent Substances 0.000 claims description 2
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 2
- 239000000356 contaminant Substances 0.000 claims 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 abstract description 23
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 abstract description 16
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- 230000003197 catalytic effect Effects 0.000 abstract description 11
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- 238000002198 surface plasmon resonance spectroscopy Methods 0.000 abstract description 2
- 150000002739 metals Chemical class 0.000 abstract 1
- 238000005457 optimization Methods 0.000 abstract 1
- 125000001997 phenyl group Chemical class [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 abstract 1
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 34
- 239000010931 gold Substances 0.000 description 25
- 239000007789 gas Substances 0.000 description 10
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 7
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 6
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- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 239000011358 absorbing material Substances 0.000 description 1
- 238000004887 air purification Methods 0.000 description 1
- IWLBIFVMPLUHLK-UHFFFAOYSA-N azane;formaldehyde Chemical compound N.O=C IWLBIFVMPLUHLK-UHFFFAOYSA-N 0.000 description 1
- 150000001555 benzenes Chemical class 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
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- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
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- 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
- B01J23/89—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals
- B01J23/8906—Iron and noble metals
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
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Abstract
The invention discloses an indoor visible light response catalyst, a preparation method and application thereof2Preparation of high-proportion (001) -plane Fe @ TiO with dodecahedral nano-structure2Improving the photocatalytic efficiency to make TiO2The absorption wavelength range of the material is expanded to a visible light region, the degradation efficiency of the benzene series is improved, and Au nano particles are loaded to Fe @ TiO by a sol-gel method2Preparation of Au/Fe @ TiO2Based on the local surface plasmon resonance effect of the Au nanoparticles, the degradation efficiency of ammonia and formaldehyde is improved. The proportion of the metals in the material prepared by the invention is adjustable, and the Au/Fe @ TiO @ modified material is beneficial to optimization2The reaction efficiency of the visible light catalytic material system is applied to the field of pollutant degradation, and the degradation effect can be improved by times.
Description
Technical Field
The invention relates to the technical field of indoor environment, in particular to an indoor visible light response catalyst, a preparation method and application thereof.
Background
With the rapid development of economy and the great improvement of living standard in China, the demand of newly built houses is increased rapidly, meanwhile, luxury is pursued in indoor decoration and fitment, and meanwhile, indoor air pollution caused by building materials generally exists and becomes one of the main sources of indoor air pollution. The indoor air pollution problem is more and more serious, and the indoor air pollution problem has the characteristics of low concentration and complex components. On the other hand, as society develops, more and more human activities are performed indoors. Poor indoor air quality can affect human life and work.
In the current situation of indoor air pollution in China, existing researches are mostly concentrated on a single pollution component along with the development of decoration, and researches on multi-component mixed gas are less, so that the research on indoor mixed pollutant purification is of practical significance. Among the existing indoor air purification technologies, photocatalysis is one of the most promising treatment technologies. The photocatalytic oxidation (PCO) technology based on nano materials is a new environmental protection technology developed in recent years, and utilizes the characteristic that the surface energy of a semiconductor oxide material is stimulated and activated under illumination and utilizes the light energy to effectively oxidize and decompose organic matters.
Chinese patent with publication number CN108855064A discloses a binary alloy @ TiO2Visible light catalytic material and preparation method thereof, wherein a one-step hydrothermal method is adopted to prepare the visible light catalytic material on TiO2The surface carries binary alloy nano particles, the reaction time is short, the alloy components are controllable, and TiO with various crystal phases2The surface can be loaded, the alloy components/proportion is controllable, and the visible light catalytic water can be effectively optimizedHydrogen/oxygen production and carbon dioxide photoreduction activity are decomposed; however, the reaction rate of the organic gas in an indoor environment is limited by factors such as a light source and light intensity, meanwhile, the degradable organic gas is single, the mineralization rate is low, and the use effect of the organic gas in the current indoor complex components is limited.
Disclosure of Invention
In view of the above technical problems to be solved, the present invention aims to provide a safe, broad-spectrum, durable and efficient indoor visible light response catalyst, a preparation method and an application thereof, the catalyst shows efficient and durable indoor harmful gas degradation activity, and oxidizes indoor common harmful gas into carbon dioxide and water under the induction of visible light, and has excellent catalytic activity and stability.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of an indoor visible light response catalyst comprises the following steps:
firstly, preparing Fe @ TiO by adopting hydrothermal method process2：
S1, ultrasonically dissolving 10-20g of a titanium source, 30-50ml of isopropanol, 10-30ml of deionized water and a proper amount of diethylenetriamine in a beaker at room temperature to form solution A;
s2, taking 10-30ml of ethanol, 20-40ml of deionized water, 1-5ml of nitric acid and 0.1-1g of iron source at room temperature, and carrying out ultrasonic homogenization for 5-15 minutes to form solution B;
s3, adding the solution A and the solution B into a polytetrafluoroethylene lining, mixing, performing ultrasonic homogenization, and performing continuous constant-temperature heating treatment in an oven;
s4, naturally cooling to room temperature, ultrasonically crushing, centrifuging, washing with ethanol and deionized water for three times respectively, and drying to obtain Fe @ TiO2Powder;
secondly, preparing Au/Fe @ TiO by adopting sol-gel process2：
S5, mixing the above 10-20gFe @ TiO2Adding the powder, 0.1-0.2g of chloroauric acid and 0.1-0.2g of polyvinylpyrrolidone into 30-90ml of deionized water to dissolve to prepare an aqueous solution C;
s6, adding a reducing reagent into 5-20ml of deionized water to form a solution D;
s7, rapidly adding the solution D into the solution C with high-speed stirring under an ice bath condition, and continuously stirring to obtain a light purple solution E;
s8, centrifuging the solution E, washing the solution E with deionized water for three times to obtain light purple powder, and reducing and roasting the powder in a hydrogen atmosphere at the temperature of 200-300 ℃ to obtain Au/Fe @ TiO2And (3) compounding a catalyst.
Further, the titanium source in step S1 is one of titanium tetrachloride, n-butyl titanate and isopropyl titanate, and more preferably isopropyl titanate.
Furthermore, the addition amount of the diethylenetriamine in the step S1 is 1-8 ml.
Further, the iron source in step S2 is one of ferric nitrate, ferric chloride and ferric sulfate, and more preferably ferric nitrate.
Further, the heating temperature of the oven in the step S3 is 100-200 ℃, and the heating time is 0.5-5 hours.
Further, the Fe @ TiO obtained by drying in the step S42The mass percentage of Fe in the powder is 0.5-5%. Fe @ TiO2The powder microstructure exhibited a dodecahedron of (001) exposed faces.
Further, the reducing agent in step S6 is one of hydrogen peroxide, sodium borohydride, hydrazine hydrate, and ascorbic acid, and the addition amount is 0.5-1 g.
Further, the high-speed stirring speed in the step S7 is 500-2000r/min, and the stirring duration is 0.5-3 hours. And the flow rate of the introduced hydrogen in the step S8 is controlled to be 50-200 ml/min.
Further, the Au/Fe @ TiO obtained by roasting in the step S82The mass percentage of Au in the composite catalyst is 0.05-0.2%.
An indoor visible light response catalyst prepared by any one of the preparation methods. The application of the indoor visible light response catalyst in the field of pollutant degradation can oxidize indoor common harmful gases into carbon dioxide and water.
The invention has the following beneficial effects:
the invention relates to binary metal step-by-step loaded TiO2Visible light catalytic material, innovative preparation process of preparation method thereof, and prepared Au/Fe @ TiO2The composite catalyst is a dodecahedral nano-structure with a high proportion of (001) planes, and has higher catalytic activity.
Based on Fe ion doping, the invention improves the surface hydroxyl position and the photocatalysis efficiency, so that TiO can be used2The absorption wavelength range of the light-absorbing material is expanded to a visible light region, the conversion and utilization of solar energy are increased, and the degradation efficiency of the benzene series is improved.
The invention can photosensitize TiO based on the local surface plasmon resonance effect of Au nano particles2The material has visible light catalytic activity, improves the degradation efficiency of ammonia and formaldehyde, has adjustable metal proportion in the prepared material, and is beneficial to optimizing Au/Fe @ TiO2The reaction efficiency of the visible light catalytic material system can be improved by times.
In conclusion, the invention adopts a hydrothermal method combined with a sol-gel method to prepare the TiO2Preparation of Au/Fe @ TiO by surface loading of iron and gold binary components2. Au/Fe @ TiO prepared by the invention2The invention has the indoor visible light catalytic activity, can effectively degrade the common indoor harmful gases such as benzene, ammonia formaldehyde and the like, has great market potential and wide application prospect.
Drawings
FIG. 1 shows Au/Fe @ TiO in the present invention2Degradation synthesis and action principle schematic diagram.
FIG. 2 shows Au/Fe @ TiO in the present invention2Ultraviolet-visible absorption spectrum of the composite material.
FIG. 3 shows Au/Fe @ TiO in the present invention2Transmission electron microscopy images.
Detailed Description
The invention is described in further detail below with reference to the following figures and specific examples:
example 1
Ultrasonically dissolving 10g of titanium tetrachloride, 30ml of isopropanol, 10ml of deionized water and 1ml of diethylenetriamine in a beaker at room temperature to form solution A; 10ml of ethanol and 20ml of deionized water are taken at room temperatureWater, 1ml nitric acid and 0.1g ferric chloride are subjected to ultrasonic homogenization for 5 minutes to form a solution B; adding the solution A and the solution B into a polytetrafluoroethylene lining, and uniformly mixing by ultrasonic waves; and heating the mixture in an oven at constant temperature of 100 ℃ for 0.5 hour; naturally cooling to room temperature, ultrasonically crushing, centrifuging, washing with ethanol and deionized water for three times respectively, and drying to obtain Fe @ TiO2And (3) powder.
Mixing the above 10g of Fe @ TiO2Adding the powder, 0.1g of chloroauric acid and 0.1g of polyvinylpyrrolidone into 30ml of deionized water to dissolve to prepare an aqueous solution C; adding 0.5g hydrogen peroxide to 5ml deionized water to form solution D; under the ice bath condition, quickly adding the solution D into the solution C with high-speed stirring at 500r/min, and continuously stirring for 0.5 hour to obtain a light purple solution E; centrifuging the solution E, washing the solution E with deionized water for three times to obtain light purple powder, placing the powder in hydrogen at 200 ℃, controlling the flow of the hydrogen to be 50ml/min, and carrying out reduction roasting to obtain Au/Fe @ TiO2And (3) compounding a catalyst.
Example 2
Ultrasonically dissolving 10g of isopropyl titanate, 30ml of isopropanol, 10ml of deionized water and 1ml of diethylenetriamine in a beaker at room temperature to form solution A; taking 10ml of ethanol, 20ml of deionized water, 1ml of nitric acid and 0.1g of ferric nitrate at room temperature, and carrying out ultrasonic homogenization for 5 minutes to form a solution B; adding the solution A and the solution B into a polytetrafluoroethylene lining, and uniformly mixing by ultrasonic waves; and heating the mixture in an oven at constant temperature of 100 ℃ for 0.5 hour; naturally cooling to room temperature, ultrasonically crushing, centrifuging, washing with ethanol and deionized water for three times respectively, and drying to obtain Fe @ TiO2And (3) powder.
Mixing the above 10g of Fe @ TiO2Adding the powder, 0.1g of chloroauric acid and 0.1g of polyvinylpyrrolidone into 30ml of deionized water to dissolve to prepare an aqueous solution C; adding 0.5g of sodium borohydride to 5ml of deionized water to form a solution D; under the ice bath condition, quickly adding the solution D into the solution C with high-speed stirring at 500r/min, and continuously stirring for 0.5 hour to obtain a light purple solution E; centrifuging the solution E, washing the solution E with deionized water for three times to obtain light purple powder, placing the powder in hydrogen at 200 ℃, controlling the flow of the hydrogen to be 50ml/min, and carrying out reduction roasting to obtain Au/Fe @ TiO2And (3) compounding a catalyst.
Example 3
Ultrasonically dissolving 16g of isopropyl titanate, 42ml of isopropanol, 20ml of deionized water and 3ml of diethylenetriamine in a beaker at room temperature to form solution A; taking 20ml of ethanol, 30ml of deionized water, 2ml of nitric acid and 0.5g of ferric nitrate at room temperature, and carrying out ultrasonic homogenization for 10 minutes to form a solution B; adding the solution A and the solution B into a polytetrafluoroethylene lining, and uniformly mixing by ultrasonic waves; and heating for 2 hours in an oven at the constant temperature of 150 ℃; naturally cooling to room temperature, ultrasonically crushing, centrifuging, washing with ethanol and deionized water for three times respectively, and drying to obtain Fe @ TiO2And (3) powder.
Mixing the above 15gFe @ TiO2Adding the powder, 0.15g of chloroauric acid and 0.15g of polyvinylpyrrolidone into 60ml of deionized water to dissolve to prepare an aqueous solution C; adding 0.75g of sodium borohydride to 12ml of deionized water to form a solution D; under the ice bath condition, rapidly adding the solution D into the solution C with high-speed stirring at 1200r/min, and continuously stirring for 2 hours to obtain a light purple solution E; centrifuging the solution E, washing the solution E with deionized water for three times to obtain light purple powder, placing the powder in hydrogen at 200 ℃, controlling the flow of the hydrogen to be 120ml/min, and carrying out reduction roasting to obtain Au/Fe @ TiO2And (3) compounding a catalyst.
Example 4
Ultrasonically dissolving 20g of isopropyl titanate, 50ml of isopropanol, 30ml of deionized water and 8ml of diethylenetriamine in a beaker at room temperature to form solution A; taking 30ml of ethanol, 40ml of deionized water, 5ml of nitric acid and 1g of ferric nitrate at room temperature, and carrying out ultrasonic homogenization for 15 minutes to form a solution B; adding the solution A and the solution B into a polytetrafluoroethylene lining, and uniformly mixing by ultrasonic waves; continuously keeping the temperature in an oven at 200 ℃, and heating for 2 hours; naturally cooling to room temperature, ultrasonically crushing, centrifuging, washing with ethanol and deionized water for three times respectively, and drying to obtain Fe @ TiO2And (3) powder.
Mixing the above 20g of Fe @ TiO2Adding the powder, 0.2g of chloroauric acid and 0.2g of polyvinylpyrrolidone into 90ml of deionized water to dissolve to prepare an aqueous solution C; adding 1g of sodium borohydride into 20ml of deionized water to form a solution D; under the ice bath condition, quickly adding the solution D into the solution C along with high-speed stirring at 2000r/min, and continuously stirring for 3 hours to obtain a light purple solution E; centrifuging the solution E, and washing the solution E with deionized water for three times to obtain the productPlacing the light purple powder in hydrogen at 200 ℃, controlling the flow of the hydrogen to be 200ml/min, and reducing and roasting to obtain Au/Fe @ TiO2And (3) compounding a catalyst.
Example 5
Ultrasonically dissolving 10g of n-butyl titanate, 30ml of isopropanol, 10ml of deionized water and 1ml of diethylenetriamine in a beaker at room temperature to form solution A; taking 10ml of ethanol, 20ml of deionized water, 1ml of nitric acid and 0.1g of ferric sulfate at room temperature, and carrying out ultrasonic homogenization for 5 minutes to form a solution B; adding the solution A and the solution B into a polytetrafluoroethylene lining, and uniformly mixing by ultrasonic waves; and heating the mixture in an oven at constant temperature of 100 ℃ for 0.5 hour; naturally cooling to room temperature, ultrasonically crushing, centrifuging, washing with ethanol and deionized water for three times respectively, and drying to obtain Fe @ TiO2And (3) powder.
Adding 10g of the Fe @ TiO2 powder, 0.1g of chloroauric acid and 0.1g of polyvinylpyrrolidone into 30ml of deionized water to dissolve to prepare an aqueous solution C; adding 0.5g hydrogen peroxide to 5ml deionized water to form solution D; under the ice bath condition, quickly adding the solution D into the solution C with high-speed stirring at 500r/min, and continuously stirring for 0.5 hour to obtain a light purple solution E; centrifuging the solution E, washing the solution E with deionized water for three times to obtain light purple powder, placing the powder in hydrogen at 200 ℃, controlling the flow of the hydrogen to be 50ml/min, and carrying out reduction roasting to obtain Au/Fe @ TiO2And (3) compounding a catalyst.
Example 6
Ultrasonically dissolving 16g of isopropyl titanate, 42ml of isopropanol, 20ml of deionized water and 3ml of diethylenetriamine in a beaker at room temperature to form solution A; taking 20ml of ethanol, 30ml of deionized water, 2ml of nitric acid and 0.5g of ferric chloride at room temperature, and carrying out ultrasonic homogenization for 10 minutes to form a solution B; adding the solution A and the solution B into a polytetrafluoroethylene lining, and uniformly mixing by ultrasonic waves; and heating for 2 hours in an oven at the constant temperature of 150 ℃; naturally cooling to room temperature, ultrasonically crushing, centrifuging, washing with ethanol and deionized water for three times respectively, and drying to obtain Fe @ TiO2And (3) powder.
Mixing the above 15gFe @ TiO2Adding the powder, 0.15g of chloroauric acid and 0.15g of polyvinylpyrrolidone into 60ml of deionized water to dissolve to prepare an aqueous solution C; adding 0.75g of sodium borohydride to 12ml of deionized water to form a solution D; on the iceUnder the bath condition, rapidly adding the solution D into the solution C with high-speed stirring at 1200r/min, and continuously stirring for 2 hours to obtain a light purple solution E; centrifuging the solution E, washing the solution E with deionized water for three times to obtain light purple powder, placing the powder in hydrogen at 200 ℃, controlling the flow of the hydrogen to be 120ml/min, and carrying out reduction roasting to obtain Au/Fe @ TiO2And (3) compounding a catalyst.
Example 7
Ultrasonically dissolving 16g of isopropyl titanate, 42ml of isopropanol, 20ml of deionized water and 3ml of diethylenetriamine in a beaker at room temperature to form solution A; taking 20ml of ethanol, 30ml of deionized water, 2ml of nitric acid and 0.5g of ferric sulfate at room temperature, and carrying out ultrasonic homogenization for 10 minutes to form a solution B; adding the solution A and the solution B into the polytetrafluoroethylene lining, and uniformly mixing by ultrasonic treatment. And heating for 2 hours in an oven at the constant temperature of 150 ℃; naturally cooling to room temperature, ultrasonically crushing, centrifuging, washing with ethanol and deionized water for three times respectively, and drying to obtain Fe @ TiO2And (3) powder.
Mixing the above 15gFe @ TiO2Adding the powder, 0.15g of chloroauric acid and 0.15g of polyvinylpyrrolidone into 60ml of deionized water to dissolve to prepare an aqueous solution C; adding 0.75g of sodium borohydride to 12ml of deionized water to form a solution D; under the ice bath condition, rapidly adding the solution D into the solution C with high-speed stirring at 1200r/min, and continuously stirring for 2 hours to obtain a light purple solution E; centrifuging the solution E, washing the solution E with deionized water for three times to obtain light purple powder, placing the powder in hydrogen at 200 ℃, controlling the flow of the hydrogen to be 120ml/min, and carrying out reduction roasting to obtain Au/Fe @ TiO2And (3) compounding a catalyst.
Indoor visible light response catalyst performance comparison test:
the test was carried out by taking 0.1g of each of the 7 room visible-light-responsive catalysts prepared in the above examples as a solution in 1L of deionized water as an experimental group and 1 equivalent of water as a control group.
1) Respectively coating 5ml of indoor visible light response catalyst aqueous solution and water prepared in 7 examples on 50 x 50cm glass, naturally airing, and placing in a container with the thickness of 1m3A climate chamber, formaldehyde, benzene and ammonia are respectively introduced into the climate chamber through a formaldehyde generator, a benzene generator and an ammonia generator,starting the LED lamp and fan in the cabin, and adopting fixed formaldehyde, benzene, ammonia and CO2The gas detector respectively controls the concentration of formaldehyde in the cabin to be 0.3mg/m3The benzene concentration was 0.5mg/m3Ammonia concentration of 0.4mg/m3、CO2The concentration is 0mg/m3After 24 hours, testing formaldehyde, benzene, ammonia and CO in the solution2The change in concentration.
Formaldehyde removal rate ═ CFormaldehyde (I)-C0)/C0*100％，
Benzene removal rate ═ CBenzene and its derivatives-C1)/C1*100％，
Removal rate of ammonia (C)Ammonia-C2)/C2*100％，
Wherein C0, C1 and C2 are the concentrations of formaldehyde, benzene and ammonia after the reaction of the experimental group; cFormaldehyde (I)、CBenzene and its derivatives、CAmmoniaThe concentration of formaldehyde, benzene and ammonia after reaction is the control group;
2) the experiment was repeated 5 times and the average was taken.
3) After the glass sprayed with the indoor visible-light-responsive catalyst solution and water prepared in 7 examples was placed in an indoor environment at normal temperature and normal pressure for 365 days, the removal rate of formaldehyde, benzene and ammonia was measured according to the method of step (1).
Through practical detection, 7 examples prepared Fe @ TiO2The mass percent of Fe in the powder is 0.5-5%; Au/Fe @ TiO2The mass percentage of Au in the composite catalyst is within 0.05-0.2%.
Specific test data are as follows:
referring to the attached drawings, FIG. 1 shows Au/Fe @ TiO prepared by the invention2The synthesis and action principle schematic diagram of the degraded harmful gas;
FIGS. 2-3 are Au/Fe @ TiO prepared in example 12The ultraviolet-visible light absorption spectrum and the transmission electron microscope picture of the composite material can show Au/Fe @ TiO2Has a dodecahedral nano-structure with high proportion of (001) planes, has higher catalytic activity andAu/Fe@TiO2the absorption peak in a visible light region is obvious, the visible light response activity is higher, and the degradation efficiency is high.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all equivalent structural changes made by using the contents of the present specification and the drawings, or applied directly or indirectly to other related technical fields, are included in the scope of the present invention.
Claims (10)
1. A preparation method of an indoor visible light response catalyst is characterized by comprising the following steps: the method comprises the following steps:
firstly, preparing Fe @ TiO by adopting hydrothermal method process2：
S1, ultrasonically dissolving 10-20g of a titanium source, 30-50ml of isopropanol, 10-30ml of deionized water and a proper amount of diethylenetriamine in a beaker at room temperature to form solution A;
s2, taking 10-30ml of ethanol, 20-40ml of deionized water, 1-5ml of nitric acid and 0.1-1g of iron source at room temperature, and carrying out ultrasonic homogenization for 5-15 minutes to form solution B;
s3, adding the solution A and the solution B into a polytetrafluoroethylene lining, mixing, performing ultrasonic homogenization, and performing continuous constant-temperature heating treatment in an oven;
s4, naturally cooling to room temperature, ultrasonically crushing, centrifuging, washing with ethanol and deionized water for three times respectively, and drying to obtain Fe @ TiO2Powder;
secondly, preparing Au/Fe @ TiO by adopting sol-gel process2：
S5, mixing the above 10-20g Fe @ TiO2Adding the powder, 0.1-0.2g of chloroauric acid and 0.1-0.2g of polyvinylpyrrolidone into 30-90ml of deionized water to dissolve to prepare an aqueous solution C;
s6, adding a reducing reagent into 5-20ml of deionized water to form a solution D;
s7, rapidly adding the solution D into the solution C with high-speed stirring under an ice bath condition, and continuously stirring to obtain a light purple solution E;
s8, centrifuging the solution E, washing the solution E with deionized water for three times to obtain light purple powder, and reducing and roasting the powder in the hydrogen atmosphere at the temperature of 200-300 ℃ to obtain the catalystTo Au/Fe @ TiO2And (3) compounding a catalyst.
2. The preparation method of the indoor visible light response catalyst according to claim 1, wherein the preparation method comprises the following steps: the titanium source in step S1 is one of titanium tetrachloride, n-butyl titanate, and isopropyl titanate.
3. The preparation method of the indoor visible light response catalyst according to claim 1, wherein the preparation method comprises the following steps: the addition amount of the diethylenetriamine in the step S1 is 1-8 ml.
4. The preparation method of the indoor visible light response catalyst according to claim 1, wherein the preparation method comprises the following steps: the iron source in the step S2 is one of ferric nitrate, ferric chloride and ferric sulfate.
5. The preparation method of the indoor visible light response catalyst according to claim 1, wherein the preparation method comprises the following steps: the heating temperature of the oven in the step S3 is 100-200 ℃, and the heating time is 0.5-5 hours.
6. The preparation method of the indoor visible light response catalyst according to claim 1, wherein the preparation method comprises the following steps: the Fe @ TiO dried in the step S42The mass percentage of Fe in the powder is 0.5-5%.
7. The preparation method of the indoor visible light response catalyst according to claim 1, wherein the preparation method comprises the following steps: the reducing agent in the step S6 is one of hydrogen peroxide, sodium borohydride, hydrazine hydrate and ascorbic acid, and the addition amount is 0.5-1 g.
8. The preparation method of the indoor visible light response catalyst according to claim 1, wherein the preparation method comprises the following steps: the Au/Fe @ TiO obtained by roasting in the step S82The mass percentage of Au in the composite catalyst is 0.05-0.2%.
9. An indoor visible light responsive catalyst, characterized in that: prepared by the preparation method of any one of claims 1 to 8.
10. Use of the indoor visible light-responsive catalyst of claim 9 in the field of contaminant degradation.
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| US20140011674A1 (en) * | 2012-07-09 | 2014-01-09 | National Chi Nan University | Process of producing a titanium dioxide-based photocatalyst used for degradation of organic pollutants |
| CN106111126A (en) * | 2016-06-23 | 2016-11-16 | 上海交通大学 | The metal-modified titania hydrosol of high visible-light activity and synthesis and application |
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| CN102716747A (en) * | 2012-06-19 | 2012-10-10 | 北京化工大学 | (001) surface exposure Fe (ferrum) doping TiO2 (titanium dioxide) multi-stage catalyst and preparation method of Fe doping TiO2 multi-stage catalyst |
| US20140011674A1 (en) * | 2012-07-09 | 2014-01-09 | National Chi Nan University | Process of producing a titanium dioxide-based photocatalyst used for degradation of organic pollutants |
| CN106111126A (en) * | 2016-06-23 | 2016-11-16 | 上海交通大学 | The metal-modified titania hydrosol of high visible-light activity and synthesis and application |
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