CN104588004A - Catalyst for ultraviolet photocatalytic degradation of organic pollutants and preparation method thereof - Google Patents
Catalyst for ultraviolet photocatalytic degradation of organic pollutants and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a catalyst for ultraviolet photocatalytic degradation of organic pollutants and a preparation method thereof. The preparation method comprises the following steps of pouring tetrabutyl titanate, acetic acid, methanol and polyvinylpyrrolidone into a conical flask, stirring to obtain a sol, carrying out electrospinning on the sol to obtain a nanometer fiber membrane and calcining to obtain TiO2 nanofibers; and placing the TiO2 nanofibers in a silver nitrate liquid, stirring and reducing and carrying out UV irradiation to obtain the Ag/TiO2 catalyst. By the preparation method, the problems that narrow energy gap, slow electron transfer speed and high electron-hole recombination velocity of the single TiO2 as a photocatalyst are overcome and the photocatalytic degradation efficiency of the organic pollutants is improved. By preparing the TiO2 nanofiber catalyst through the electrospinning, the light-generated electron-hole recombination velocity is reduced and the transfer rate and the catalytic degradation efficiency are increased. The synthesis method is simple and the reaction conditions are mild. By the catalyst, the ultraviolet photocatalytic degradation efficiency under the condition that methyl orange is used as an organic pollution substrate is high and the photocatalytic degradation effect on the organic pollutants is remarkable especially in the use of neutral conditions.
Description
Technical field
The present invention relates to a kind of organic pollutant degradation method.Specifically, the preparation method of especially ultraviolet degradation organic pollutant catalyst.
Background technology
In recent years, problem of environmental pollution is day by day serious, and a large amount of coloured dye is discharged in environment, discharges tool virose or even have the material of carcinogenicity.People by various physics, chemical process, as precipitation, absorption, counter-infiltration, ultrafiltration etc. are separated these harmful substances.But these technology are only that these pollutants have been transferred to other positions such as mud from water body, do not eradicate these pollutants, thus cause new pollution.Therefore, find a kind of new processing mode, noxious pollutant being converted to free of contamination material becomes study hotspot in recent years.
Can be employed and photocatalysis field (Fujishima and K.Honda owing to having narrower energy gap, very strong absorbing properties, good chemical stability, anti-light corrosivity and cheap cost at Fujishima and Honda reported first titanium dioxide, Nature 238,37 (1972)).But because the recombination rate of photo-generate electron-hole in titanium dioxide is too fast, have a strong impact on its application in photocatalysis.Therefore, find a kind of suitable method to reduce the recombination rate of its photo-generate electron-hole, the transfer rate improving light induced electron becomes current urgent problem.
Current such problem of solution main method have by reducing the particle diameter of titanium dioxide, improve its specific area, increase the generation quantity of light induced electron, to improve its photocatalytic activity; By modifying titanium dioxide surface, accelerate the transfer rate of light induced electron, to improve its photocatalytic activity.
Chen Q., Zhou W., Du G.H., Peng L.M..Advanced Materials.2002,14:1208-121, discloses a kind of hydrothermal synthesis method;
Shigeru K, Shinji K, Tatsuo M, et al.Shapu Giho, 1987,38:269, discloses a kind of sol-gel process;
Pileni M.P., J Phys Chem, 1993,97:6961, discloses a kind of microemulsion method; CN101284226, discloses a kind of method of electrostatic spinning.
All there is the shortcomings such as severe reaction conditions, the reaction time is long, cost is higher, catalytic efficiency is low in these methods existing, is difficult to carry out large-scale production.Which also limits its application in practice.
Summary of the invention
A kind of ultraviolet catalytic degradable organic pollutant catalyst of the shortcomings such as primary and foremost purpose of the present invention is to provide a kind of and overcomes severe reaction conditions existing for existing degradable organic pollutant catalyst preparation method, the reaction time is long, cost is higher, catalytic efficiency is low; Preparation method.
Another object of the present invention is the preparation method providing a kind of ultraviolet catalytic degradable organic pollutant catalyst;
Another object of the present invention is the application for photocatalysis degradation organic contaminant providing described catalyst.
A kind of ultraviolet catalytic degradable organic pollutant catalyst is prepared from by mass fraction by following raw materials according:
A preparation method for light degradation organic pollutant catalyst, comprises the following steps:
A, 8-15g butyl titanate (TBT), 5-10ml acetic acid, 100-140ml methyl alcohol and 5-7g polyvinylpyrrolidone (PVP) are poured in 250mL conical flask, after stirred at ambient temperature 4 ~ 8h, obtain PVP/TBT colloidal sol;
B, by PVP/TBT colloidal sol electrostatic spinning, obtain PVP/TBT nano fibrous membrane;
C, at 500 DEG C by the PVP/TBT nano fibrous membrane of gained calcining 4h, obtained TiO
2nanofiber;
D, by 50mgTiO
2evenly spread in the quartzy bottle filling 5-50mL 0.001mol/L liquor argenti nitratis ophthalmicus, lucifuge stirs 2h, makes the silver ion in solution be adsorbed onto TiO
2nanofiber surface;
E, the TiO of silver ion will be adsorbed with
2nanofiber, through UV-irradiation 30min ~ 1h, filters, and washing is dry, obtains Ag/TiO
2catalyst.
The load capacity of silver is 1-9%.
Described at TiO
2upper load silver also comprises centrifugal for in-situ reducing product, that washing is also dry step.
Described drying condition is that ambient temperature in vacuum is dry.
Silver/titanium dioxide catalyst is used for ultraviolet degradation organic pollution.
Beneficial effect: the present invention's silver is as loaded article, overcome in prior art and use the problem that single titanium dioxide is narrow as the energy gap existed during photochemical catalyst, electron transfer speed slow, electron-hole recombination rate is fast, thus improve the efficiency of photocatalysis degradation organic contaminant.The titanium dioxide nanofiber depositing nano silver obtained with electrostatic spinning obtains catalyst, reduces the recombination rate of photo-generate electron-hole, improves the transfer rate of light induced electron, the catalytic degradation efficiency of catalyst is improved.Synthetic method is easy and simple to handle, reaction condition is gentle.Prepared catalyst, having higher efficiency to ultraviolet degradation using methyl orange under the condition of organic contamination substrate, has significant effect, uses especially in neutral conditions in photocatalysis degradation organic contaminant.
Accompanying drawing explanation
Fig. 1 is that titanium dioxide and load have the XRD of the titanium dioxide of 9% silver medal to scheme.
Fig. 2 is that load has the XPS of the titanium dioxide of 9% silver medal to scheme.
Fig. 3 is that load has the EDS of the titanium dioxide of 9% silver medal to scheme.
Fig. 4 is the SEM figure of titanium dioxide, and wherein a is titanium dioxide; B is the titanium dioxide that load has 9% silver medal.
Fig. 5 be titanium dioxide, different molar concentration silver-colored carried titanium dioxide and not containing the degradation rate broken line graph of catalyst.
Fig. 6 to be molar concentration be 5% the block diagram in silver/titanium dioxide catalyst service life.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in further detail.Should be understood that following examples only for illustration of the present invention but not for limiting the scope of the invention.
In context of the present invention, term " in-situ reducing " refer to by silver-colored load titania fiber surface time, by the irradiation of ultraviolet light, make the silver salt being adsorbed on titania fiber surface be reduced to silver.Silver salt used is silver nitrate.
A kind of ultraviolet catalytic degradable organic pollutant catalyst is prepared from by mass fraction by following raw materials according:
A preparation method for light degradation organic pollutant catalyst, comprises the following steps:
A, 8-15g butyl titanate (TBT), 5-10ml acetic acid, 100-140ml methyl alcohol and 5-7g polyvinylpyrrolidone (PVP) are poured in 250mL conical flask, after stirred at ambient temperature 4 ~ 8h, obtain PVP/TBT colloidal sol;
B, by PVP/TBT colloidal sol electrostatic spinning, obtain PVP/TBT nano fibrous membrane;
C, at 500 DEG C by the PVP/TBT nano fibrous membrane of gained calcining 4h, obtained TiO
2nanofiber;
D, by 50mgTiO
2evenly spread in the quartzy bottle filling 5-50mL 0.001mol/L liquor argenti nitratis ophthalmicus, lucifuge stirs 2h, makes the silver ion in solution be adsorbed onto TiO
2nanofiber surface;
E, the TiO of silver ion will be adsorbed with
2nanofiber, through UV-irradiation 30min ~ 1h, filters, and washing is dry, obtains Ag/TiO
2catalyst.
The load capacity of silver is 1-9%.
Described at TiO
2upper load silver also comprises centrifugal for in-situ reducing product, that washing is also dry step.
Embodiment 1
A, 10g butyl titanate (TBT), 7mL acetic acid, 120mL methyl alcohol and 5.6g polyvinylpyrrolidone (PVP) are poured in 250mL conical flask, after stirred at ambient temperature 4h, obtain PVP/TBT colloidal sol;
B, just PVP/TBT colloidal sol electrostatic spinning, obtain PVP/TBT nano fibrous membrane;
C, at 500 DEG C by the PVP/TBT nano fibrous membrane of gained calcining 4h, obtained TiO
2nanofiber;
D, by 50mgTiO
2evenly spread in the quartzy bottle filling 5.25mL 0.001mol/L liquor argenti nitratis ophthalmicus, lucifuge stirs 2h, makes the silver ion in solution be adsorbed onto TiO
2nanofiber surface;
E, the TiO of silver ion will be adsorbed with
2nanofiber, through UV-irradiation 45min, filters, washing, and ambient temperature in vacuum is dry, obtains 1%Ag/TiO
2catalyst.
Embodiment 2
A, 8g butyl titanate (TBT), 5ml acetic acid, 100ml methyl alcohol and 5g polyvinylpyrrolidone (PVP) are poured in 250mL conical flask, after stirred at ambient temperature 7h, obtain PVP/TBT colloidal sol;
B, just PVP/TBT colloidal sol electrostatic spinning, obtain PVP/TBT nano fibrous membrane;
C, at 500 DEG C by the PVP/TBT nano fibrous membrane of gained calcining 4h, obtained TiO
2nanofiber;
D, by 50mgTiO
2evenly spread in the quartzy bottle filling 15.75mL 0.001mol/L liquor argenti nitratis ophthalmicus, lucifuge stirs 2h, makes the silver ion in solution be adsorbed onto TiO
2nanofiber surface;
E, the TiO of silver ion will be adsorbed with
2nanofiber, through UV-irradiation 30min, filters, and washing is dry, obtains 3%Ag/TiO
2catalyst.
Embodiment 3
A, 15g butyl titanate (TBT), 10ml acetic acid, 140ml methyl alcohol and 7g polyvinylpyrrolidone (PVP) are poured in 250mL conical flask, after stirred at ambient temperature 6h, obtain PVP/TBT colloidal sol;
B, just PVP/TBT colloidal sol electrostatic spinning, obtain PVP/TBT nano fibrous membrane;
C, at 500 DEG C by the PVP/TBT nano fibrous membrane of gained calcining 4h, obtained TiO
2nanofiber;
D, by 50mgTiO
2evenly spread in the quartzy bottle filling 26.25mL 0.001mol/L liquor argenti nitratis ophthalmicus, lucifuge stirs 2h, makes the silver ion in solution be adsorbed onto TiO
2nanofiber surface;
E, the TiO of silver ion will be adsorbed with
2nanofiber, through UV-irradiation 50min, filters, and washing is dry, obtains 5%Ag/TiO
2catalyst.
Embodiment 4
A, 13g butyl titanate (TBT), 8ml acetic acid, 130ml methyl alcohol and 6.5g polyvinylpyrrolidone (PVP) are poured in 250mL conical flask, after stirred at ambient temperature 8h, obtain PVP/TBT colloidal sol;
B, just PVP/TBT colloidal sol electrostatic spinning, obtain PVP/TBT nano fibrous membrane;
C, at 500 DEG C by the PVP/TBT nano fibrous membrane of gained calcining 4h, obtained TiO
2nanofiber;
D, by 50mgTiO
2evenly spread in the quartzy bottle filling 36.75mL 0.001mol/L liquor argenti nitratis ophthalmicus, lucifuge stirs 2h, makes the silver ion in solution be adsorbed onto TiO
2nanofiber surface;
E, the TiO of silver ion will be adsorbed with
2nanofiber, through UV-irradiation 1h, filters, and washing is dry, obtains Ag/TiO
2catalyst.
Embodiment 5
A, 12g butyl titanate (TBT), 10ml acetic acid, 110ml methyl alcohol and 7g polyvinylpyrrolidone (PVP) are poured in 250mL conical flask, after stirred at ambient temperature 5h, obtain PVP/TBT colloidal sol;
B, just PVP/TBT colloidal sol electrostatic spinning, obtain PVP/TBT nano fibrous membrane;
C, at 500 DEG C by the PVP/TBT nano fibrous membrane of gained calcining 4h, obtained TiO
2nanofiber;
D, by 50mgTiO
2evenly spread in the quartzy bottle filling 47.25mL 0.001mol/L liquor argenti nitratis ophthalmicus, lucifuge stirs 2h, makes the silver ion in solution be adsorbed onto TiO
2nanofiber surface;
E, the TiO of silver ion will be adsorbed with
2nanofiber, through UV-irradiation 45min, filters, and washing is dry, obtains Ag/TiO
2catalyst.
Embodiment 6,
A, 9g butyl titanate (TBT), 7.25ml acetic acid, 82.5ml methyl alcohol and 5.25g polyvinylpyrrolidone (PVP) are poured in 250mL conical flask, after stirred at ambient temperature 5h, obtain PVP/TBT colloidal sol;
B, just PVP/TBT colloidal sol electrostatic spinning, obtain PVP/TBT nano fibrous membrane;
C, at 500 DEG C by the PVP/TBT nano fibrous membrane of gained calcining 4h, obtained TiO
2nanofiber, is designated as TiO
2catalyst.
Embodiment 7,
By the 10mg Ag/TiO obtained in embodiment 1-6
2catalyst is put into respectively and the quartzy bottle that 100mL mass fraction is the methyl orange solution of 1mg/L is housed, and dark place is stirred 30min and reached adsorption-desorption balance to make catalyst to methyl orange solution.
Open light source and start light degradation, reaction temperature is room temperature, and light source is 250W mercury lamp, and the distance between light source and reactor is 15cm, installs optical filter is greater than 420nm visible ray with elimination wavelength between light source and reactor additional.
Reaction 15-30min, takes out 6mL reaction solution from reactor, by the catalyst filtration in solution, detects the absorption spectrum of solution with ultraviolet-visible spectrophotometer.After reaction 150min, close light source, stop experiment.
Catalyst is to the degradation efficiency result of methyl orange:
Catalyst degradation efficiency (c/c prepared by embodiment 1
0× 100%) be 71.73;
Catalyst degradation efficiency (c/c prepared by embodiment 2
0× 100%) be 86.02;
Catalyst degradation efficiency (c/c prepared by embodiment 3
0× 100%) be 92.82;
Catalyst degradation efficiency (c/c prepared by embodiment 4
0× 100%) be 83.36;
Catalyst degradation efficiency (c/c prepared by embodiment 5
0× 100%) be 83.06;
Catalyst degradation efficiency (c/c prepared by embodiment 6
0× 100%) be 26.02.
Claims (5)
1. a ultraviolet catalytic degradable organic pollutant catalyst, is characterized in that, is to be prepared from by mass fraction by following raw materials according:
2. a preparation method for light degradation organic pollutant catalyst, is characterized in that: comprise the following steps:
A, 8-15g butyl titanate (TBT), 5-10mL acetic acid, 100-140mL methyl alcohol and 5-7g polyvinylpyrrolidone (PVP) are poured in 250mL conical flask, after stirred at ambient temperature 4 ~ 8h, obtain PVP/TBT colloidal sol;
B, just PVP/TBT colloidal sol electrostatic spinning, obtain PVP/TBT nano fibrous membrane;
C, at 500 DEG C by the PVP/TBT nano fibrous membrane of gained calcining 4h, obtained TiO
2nanofiber;
D, by 50mgTiO
2evenly spread in the quartzy bottle filling 5-50mL 0.001mol/L liquor argenti nitratis ophthalmicus, lucifuge stirs 2h, makes the silver ion in solution be adsorbed onto TiO
2nanofiber surface;
E, the TiO of silver ion will be adsorbed with
2nanofiber, through UV-irradiation 30min ~ 1h, filters, and washing is dry, obtains Ag/TiO
2catalyst.
3. according to the preparation method of light degradation organic pollutant catalyst according to claim 2, it is characterized in that: the load capacity of silver is 1-9%.
4. according to the preparation method of light degradation organic pollutant catalyst according to claim 4, it is characterized in that: described drying condition is that ambient temperature in vacuum is dry.
5. according to light degradation organic pollutant catalyst according to claim 1, it is characterized in that: silver/titanium dioxide catalyst is used for ultraviolet degradation organic pollution.
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Cited By (10)
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|---|---|---|---|---|
| CN104907580A (en) * | 2015-06-16 | 2015-09-16 | 华北电力大学 | Preparation method for hollow titanium dioxide nanofiber containing metal nanoparticles |
| CN104998638A (en) * | 2015-06-30 | 2015-10-28 | 宁波工程学院 | Applications of high-purity Ag-loaded TiO2 mesoporous nanofiber as high-efficiency photocatalyst |
| CN105013478A (en) * | 2015-06-30 | 2015-11-04 | 宁波工程学院 | Preparation method of high-purity Ag-loading TiO2 full-mesoporous nanofiber |
| CN105032411A (en) * | 2015-06-30 | 2015-11-11 | 宁波工程学院 | High-purity TiO2 mesoporous nano fiber loaded with Ag |
| CN106577750A (en) * | 2016-11-29 | 2017-04-26 | 青岛海之星生物科技有限公司 | Preparing method for titanium-dioxide composite nanometer antibacterial material and product thereof |
| CN109999918A (en) * | 2019-04-01 | 2019-07-12 | 江苏奥净嘉环保科技有限公司 | A kind of preparation method of cotton fiber original position load nano-titanium dioxide |
| CN113083268A (en) * | 2021-04-02 | 2021-07-09 | 西安建筑科技大学 | Crystal form controllable TiO2Preparation method of photocatalytic material |
| CN113351127A (en) * | 2021-05-31 | 2021-09-07 | 浙江传化功能新材料有限公司 | Composite functional phase change microcapsule and preparation method thereof |
| CN113351126A (en) * | 2021-05-31 | 2021-09-07 | 浙江传化功能新材料有限公司 | Nano Ag/TiO2Method for modifying microcapsules and products thereof |
| CN113717463A (en) * | 2020-05-25 | 2021-11-30 | 海信（山东）空调有限公司 | Antibacterial and antiviral high polymer material, air conditioner filter screen and air conditioner |
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| CN104907580A (en) * | 2015-06-16 | 2015-09-16 | 华北电力大学 | Preparation method for hollow titanium dioxide nanofiber containing metal nanoparticles |
| CN104998638A (en) * | 2015-06-30 | 2015-10-28 | 宁波工程学院 | Applications of high-purity Ag-loaded TiO2 mesoporous nanofiber as high-efficiency photocatalyst |
| CN105013478A (en) * | 2015-06-30 | 2015-11-04 | 宁波工程学院 | Preparation method of high-purity Ag-loading TiO2 full-mesoporous nanofiber |
| CN105032411A (en) * | 2015-06-30 | 2015-11-11 | 宁波工程学院 | High-purity TiO2 mesoporous nano fiber loaded with Ag |
| CN106577750A (en) * | 2016-11-29 | 2017-04-26 | 青岛海之星生物科技有限公司 | Preparing method for titanium-dioxide composite nanometer antibacterial material and product thereof |
| CN109999918A (en) * | 2019-04-01 | 2019-07-12 | 江苏奥净嘉环保科技有限公司 | A kind of preparation method of cotton fiber original position load nano-titanium dioxide |
| CN113717463A (en) * | 2020-05-25 | 2021-11-30 | 海信（山东）空调有限公司 | Antibacterial and antiviral high polymer material, air conditioner filter screen and air conditioner |
| CN113717463B (en) * | 2020-05-25 | 2024-04-02 | 海信空调有限公司 | Antibacterial and antiviral polymer material, air conditioner filter screen obtained by antibacterial and antiviral polymer material and air conditioner |
| CN113083268A (en) * | 2021-04-02 | 2021-07-09 | 西安建筑科技大学 | Crystal form controllable TiO2Preparation method of photocatalytic material |
| CN113351127A (en) * | 2021-05-31 | 2021-09-07 | 浙江传化功能新材料有限公司 | Composite functional phase change microcapsule and preparation method thereof |
| CN113351126A (en) * | 2021-05-31 | 2021-09-07 | 浙江传化功能新材料有限公司 | Nano Ag/TiO2Method for modifying microcapsules and products thereof |
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