CN104588005A - Preparation method of nanometer silver-loaded titanic oxide photocatalyst - Google Patents
Preparation method of nanometer silver-loaded titanic oxide photocatalyst Download PDFInfo
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- CN104588005A CN104588005A CN201510053214.XA CN201510053214A CN104588005A CN 104588005 A CN104588005 A CN 104588005A CN 201510053214 A CN201510053214 A CN 201510053214A CN 104588005 A CN104588005 A CN 104588005A
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Abstract
The invention discloses a preparation method of a photocatalyst, and particularly relates to a preparation method of nanometer silver-loaded titanic oxide photocatalyst. The preparation method comprises the following steps: putting 20g of hydrogen peroxide and 2.5g of sodium hydroxide into a reaction kettle; after dissolving, slowly adding 20g of titanium tetrachloride; heating and pressurizing under sealing, preserving heat, cooling and refluxing to prepare a titanium dioxide nanocrystalline hydrosol for later use; adding 0.017g of silver nitrate into 10ml of absolute ethyl alcohol and then adding into 20ml of ethanol with 0.10g of polyvinylpyrrolidone, and reacting to obtain spherical nanometer silver for later use; reacting 0.01g of the prepared spherical nanometer silver with 10g of the prepared titanium dioxide nanocrystalline hydrosol and further carrying out ultrasonic dispersion for 30 minutes to prepare a photocatalyst. The photocatalyst prepared by the invention is characterized by good dispersibility, stable storage and stronger photocatalytic performance compared with that of nanometer titanium dioxide simultaneously when reserving the antibacterial property and other properties of nanometer silver.
Description
Technical field
The present invention relates to a kind of preparation method of photochemical catalyst, particularly relate to a kind of preparation method of nano-silver loaded titanium dioxide optical catalyst.
Background technology
Light catalytic purifying is the redox ability and purifying contaminated thing that have under Ultraviolet radiation based on photochemical catalyst.Photochemical catalyst is utilized to purify the reaction condition gentleness of the organic pollution removed in air, organic pollution can be decomposed into the inorganic molecules such as carbon dioxide and water, clean-up effect is thorough, photochemical catalyst stable chemical nature, oxidation-reduction quality is strong, cost is low, there is not absorption saturated phenomenon, long service life.
Photochemical catalyst purification has the advantages that secondary pollution is little, operating cost is low, and it can utilize sunshine for reaction light source, so the purification of volatile organic compounds in the special suitable chamber of photocatalysis, shows huge application potential in deep purifying.Common photochemical catalyst mostly is metal oxide and sulfide, as titanium dioxide, and ZnO, CdS, WO
3deng, wherein the combination property of titanium dioxide is best, most widely used.Titanium dioxide has good anti-light corrosivity and catalytic activity, and stable performance, cheap and easy to get, nontoxic, is the optimal light catalyst of generally acknowledging at present.
Existing silver-colored titanium composite nanoparticle manufacturing technology, is adopt the form of silver ion and titanium dioxide to be formed to adulterate mostly, makes
twotitania photocatalyst, this
twothere is the technical problem that dispersiveness is poor, store instability in titania photocatalyst.
Summary of the invention
The present invention is exactly to solve the problems of the technologies described above, and the preparation method of a kind of nano-silver loaded titanium dioxide optical catalyst provided, it has good dispersion, stable storing, while remaining the performance such as antibacterial of Nano Silver, possess the photocatalysis performance stronger than nano titanium oxide.
In order to achieve the above object, the present invention is achieved through the following technical solutions:
The preparation method of nano-silver loaded titanium dioxide optical catalyst of the present invention is as follows:
In the miniature high pressure reaction still of ice water circulation cooling, drop into 20 grams of hydrogen peroxide, 2.5 grams of NaOH, 20 grams of titanium tetrachlorides are slowly added after dissolving, heated sealed is forced into 115-150 DEG C, be incubated 5 hours, material enters into return duct cooling for reflux 15 hours, and the obtained titanium dioxide nanocrystalline hydrosol is for subsequent use;
0.017g silver nitrate is joined in 10ml absolute ethyl alcohol, be stirred to and dissolve completely, then it is dropwise added dropwise to prepare in advance containing 0.10g polyvinylpyrrolidone 20ml ethanol in, mixed liquor being proceeded to cumulative volume is in the polytetrafluoroethyllining lining autoclave of 40ml again, be placed in 180 DEG C of baking oven reactions 24 hours, naturally cool to room temperature, centrifugation, products therefrom mass ratio is deionized water and the alcohol mixeding liquid washing of 1:1, wash rear 50 DEG C of vacuum drying, obtained spherical nano-silver is for subsequent use;
The spherical nano-silver 0.01g getting aforementioned preparation is placed in bottle, adds 2ml ethanol, ultrasonic 10min under room temperature, then adds the 10g titanium dioxide nanocrystalline hydrosol of aforementioned preparation, continues ultrasonic disperse 30min, vacuum drying, obtained photochemical catalyst.
Owing to adopting technique scheme, tool of the present invention is had the following advantages and effect:
Photochemical catalyst favorable dispersibility prepared by the present invention, stable storing, while it preserves the performance such as antibacterial of Nano Silver, has possessed the photocatalysis performance stronger than nano titanium oxide.
Accompanying drawing explanation
Fig. 1 is that photochemical catalyst of the present invention adopts DX-2000X x ray diffractometer x (XRD) scanning display diffraction maximum figure.
Fig. 2 is the performance chart of photochemical catalyst of the present invention.
Detailed description of the invention
Description below by way of detailed description of the invention is described in further detail the present invention, but this is not limitation of the present invention, those skilled in the art are according to basic thought of the present invention, various amendment or improvement can be made, but only otherwise depart from basic thought of the present invention, all within the scope of the present invention.
Method in following embodiment, if no special instructions, is conventional method.
Percentage composition (%) in following embodiment if no special instructions, is mass percentage.
embodiment 1
The preparation method of nano-silver loaded titanium dioxide optical catalyst of the present invention is as follows:
In the miniature high pressure reaction still of ice water circulation cooling, drop into 20 grams of hydrogen peroxide, 2.5 grams of NaOH, 20 grams of titanium tetrachlorides are slowly added after dissolving, heated sealed is forced into 115-150 DEG C, be incubated 5 hours, material enters into return duct cooling for reflux 15 hours, and the obtained titanium dioxide nanocrystalline hydrosol is for subsequent use;
0.017g silver nitrate is joined in 10ml absolute ethyl alcohol, be stirred to and dissolve completely, then it is dropwise added dropwise to prepare in advance containing 0.10g polyvinylpyrrolidone 20ml ethanol in, mixed liquor being proceeded to cumulative volume is in the polytetrafluoroethyllining lining autoclave of 40ml again, be placed in 180 DEG C of baking oven reactions 24 hours, naturally cool to room temperature, centrifugation, products therefrom mass ratio is that the deionized water of 1:1 and alcohol mixeding liquid wash 3 times, wash rear 50 DEG C of vacuum drying, obtained spherical nano-silver is for subsequent use;
The spherical nano-silver 0.01g getting aforementioned preparation is placed in bottle, adds 2ml ethanol, ultrasonic 10min under room temperature, then adds the 10g titanium dioxide nanocrystalline hydrosol of aforementioned preparation, continues ultrasonic disperse 30min, vacuum drying, obtained photochemical catalyst.
Experimental data is as follows:
The crystal phase structure of catalyst sample prepared by the embodiment of the present invention 1, adopts DX-2000X x ray diffractometer x (XRD) to detect.Utilize SEM (SEM, JEOLJSM-5600LV), the shape characteristic of transmission electron microscope observation product.The optical absorptive character of sample measures on ultraviolet-visible spectrophotometer.Photocatalysis performance is tested in self-made Instrument (the sub-bright 125W high-pressure sodium lamp in Shanghai, main emission wavelength is 365nm), with methyl orange (20mg/ L) for degraded object, maximum absorption wavelength 464nm, photocatalyst concentrations 1g/L, represents photocatalysis efficiency with degradation rate.The results are shown in Figure 1.
Through XRD scanning display, do not observe the diffraction maximum of AgO and Ag2O, show that silver ion is completely reduced, product exists with simple substance Ag form.
As shown in Figure 2, be the performance chart of the photochemical catalyst of embodiment 1 preparation.
Nano-silver loaded optically catalytic TiO 2 performance is significantly increased, and the undope optically catalytic TiO 2 performance of the nano titanium oxide of Nano Silver and doping nano-Ag of contrast is as follows:
After photocatalytic degradation 30min, non-impurity-doped titanium dioxide, Ag1 (cubic)/titanium dioxide, Ag2 (spherical)/titanium dioxide reach 57%, 85% and 93% respectively to the degradation rate of methyl orange solution.Silver granuel footpath is less, is more conducive to the raising of photocatalytic activity.This is that the fermi level of elemental silver owing to being attached to titanium dioxide surface is lower than titanium dioxide, effectively can catch the light induced electron that titanium dioxide produces, make photohole mobile to titanium dioxide nano-particle surface, improve the quantum yield of light induced electron, thus improve the photocatalysis performance of titanium dioxide.
Photocatalysis performance test shows, under 25W ultraviolet lamps irradiates, adopt nano-silver loaded nano-titania photocatalyst to decompose ammonia experiment in closed system and show, after the illumination cumulative time reaches 15 hours, the resolution ratio of ammonia is 80%, illumination is accumulative after 30 hours, and resolution ratio reaches 99%.Decompose completely, faster than the nano titanium oxide of contrast test used 20 little time.
The photochemical catalyst favorable dispersibility prepared by the visible embodiment of the present invention 1 of above-mentioned experimental data, stable storing, while it preserves the performance such as antibacterial of Nano Silver, has possessed the photocatalysis performance stronger than nano titanium oxide.
Claims (1)
1. the preparation method of nano-silver loaded titanium dioxide optical catalyst, is characterized in that step is as follows:
In the miniature high pressure reaction still of ice water circulation cooling, drop into 20 grams of hydrogen peroxide, 2.5 grams of NaOH, 20 grams of titanium tetrachlorides are slowly added after dissolving, heated sealed is forced into 115-150 DEG C, be incubated 5 hours, material enters into return duct cooling for reflux 15 hours, and the obtained titanium dioxide nanocrystalline hydrosol is for subsequent use;
0.017g silver nitrate is joined in 10ml absolute ethyl alcohol, be stirred to and dissolve completely, then it is dropwise added dropwise to prepare in advance containing 0.10g polyvinylpyrrolidone 20ml ethanol in, mixed liquor being proceeded to cumulative volume is in the polytetrafluoroethyllining lining autoclave of 40ml again, be placed in 180 DEG C of baking oven reactions 24 hours, naturally cool to room temperature, centrifugation, products therefrom mass ratio is deionized water and the alcohol mixeding liquid washing of 1:1, wash rear 50 DEG C of vacuum drying, obtained spherical nano-silver is for subsequent use;
The spherical nano-silver 0.01g getting aforementioned preparation is placed in bottle, adds 2ml ethanol, ultrasonic 10min under room temperature, then adds the 10g titanium dioxide nanocrystalline hydrosol of aforementioned preparation, continues ultrasonic disperse 30min, vacuum drying, obtained photochemical catalyst.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107008258A (en) * | 2017-04-20 | 2017-08-04 | 河南科技学院 | TiO2Application of the nanometer Ag photochemical catalyst of load in degradation of phenol |
| CN107029709A (en) * | 2017-04-20 | 2017-08-11 | 河南科技学院 | A kind of TiO2The preparation method of the tetrahexahedron pattern nanometer Ag photochemical catalyst of the high miller index surface of load |
| CN107497428A (en) * | 2017-08-28 | 2017-12-22 | 中山大学 | A kind of TiO of more shell nanoparticles2Photochemical catalyst and preparation method and application |
| CN108264125A (en) * | 2018-03-06 | 2018-07-10 | 辽宁海润环保技术股份有限公司 | A kind of advanced treatment method for sewage water |
| CN117380172A (en) * | 2023-10-11 | 2024-01-12 | 齐鲁工业大学(山东省科学院) | Photocatalytic self-cleaning metal hydroxide/TiO with amphiphilic structure 2 Hydrosol and preparation method and application thereof |
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| CN102909009A (en) * | 2012-11-16 | 2013-02-06 | 厦门大学 | Preparing method of crystalline silver loaded TiO2 nanometer particle |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107008258A (en) * | 2017-04-20 | 2017-08-04 | 河南科技学院 | TiO2Application of the nanometer Ag photochemical catalyst of load in degradation of phenol |
| CN107029709A (en) * | 2017-04-20 | 2017-08-11 | 河南科技学院 | A kind of TiO2The preparation method of the tetrahexahedron pattern nanometer Ag photochemical catalyst of the high miller index surface of load |
| CN107008258B (en) * | 2017-04-20 | 2019-07-05 | 河南科技学院 | TiO2Application of the nanometer Ag photochemical catalyst of load in degradation of phenol |
| CN107497428A (en) * | 2017-08-28 | 2017-12-22 | 中山大学 | A kind of TiO of more shell nanoparticles2Photochemical catalyst and preparation method and application |
| CN108264125A (en) * | 2018-03-06 | 2018-07-10 | 辽宁海润环保技术股份有限公司 | A kind of advanced treatment method for sewage water |
| CN117380172A (en) * | 2023-10-11 | 2024-01-12 | 齐鲁工业大学(山东省科学院) | Photocatalytic self-cleaning metal hydroxide/TiO with amphiphilic structure 2 Hydrosol and preparation method and application thereof |
| CN117380172B (en) * | 2023-10-11 | 2024-04-16 | 齐鲁工业大学(山东省科学院) | Photocatalytic self-cleaning metal hydroxide/TiO with amphiphilic structure 2 Hydrosol and preparation method and application thereof |
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