CN102274739A - Copper-nitrogen double-doped titanium dioxide photocatalytic material - Google Patents

Copper-nitrogen double-doped titanium dioxide photocatalytic material Download PDF

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CN102274739A
CN102274739A CN2011101441915A CN201110144191A CN102274739A CN 102274739 A CN102274739 A CN 102274739A CN 2011101441915 A CN2011101441915 A CN 2011101441915A CN 201110144191 A CN201110144191 A CN 201110144191A CN 102274739 A CN102274739 A CN 102274739A
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copper
titanium dioxide
temperature
nitrogen
photocatalysis material
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CN102274739B (en
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范晓芸
王传义
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Beijing Xiangshunyuan Science & Technology Co., Ltd.
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Xinjiang Technical Institute of Physics and Chemistry of CAS
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Abstract

The invention relates to a copper-nitrogen double-doped titanium dioxide photocatalytic material, which is a photocatalytic composite material of TiO2 doped with the metallic element Cu and the inorganic non-metallic element N. Prepared by a hydrothemal method, the material is water insoluble white powder. Compared with TiO2 (P25), the material of the invention has high catalytic activity, and has a degradation rate of over 95% to methylene blue. The material provided in the invention has the characteristics of rapid degradation speed, no secondary pollution, easily available and cheap catalyst, low operation cost, simple equipment, small investment and good effect.

Description

Copper-nitrogen codope photocatalysis material of titanium dioxide
Technical field
The present invention relates to a kind of use Hydrothermal Preparation transition metal Cu and inorganic non-metallic element N codope TiO 2Catalysis material and its production and use.
Background technology
Along with world population constantly increases, industrialized level improves day by day, the contradiction of energy and environment becomes a global problem.Clean energy resource rational and efficient use and environmental improvement are the great demands of the economic sustainable development of China.The discharging of pollutants such as industrial wastewater, sanitary sewage, industrial waste gas and refuse, house refuse makes that Global Ecological worsens, environmental quality descends.For this pollutant it is handled effectively is the difficult problem in environmental improvement field always, technologies such as traditional treatment method such as biological treatment, coagulating sedimentation, absorption, membrane technology are poor for the mineralization ability of persistent organic pollutants, and cause secondary pollution easily, do not find a kind of more satisfactory method to its harmless treatment in addition so far yet.Studies show that in a large number, various poisonous and hazardous pollutants in the water and air, various alkane, aromatic hydrocarbons and derivative thereof, halides, polycyclic aromatic hydrocarbon and the heterocyclic compound etc. that discharge in the Chemical Manufacture greatly can both be by photocatalytic degradations.Pure pollution-free and inexhaustible luminous energy is used the catalyst, the consersion unit that combine light with environmental protection be used for degrading that industrial wastewater is poisonous, harmful, the research of difficult decomposing organic matter has far-reaching strategic importance; be that current environment is administered one of challenge that the field faced, the catalysis technique that with the catalysis material is core is to solve this difficult problem to lay the foundation.
Titanium dioxide (TiO 2) be a kind of environmental friendliness green functional material, penetrate in illumination and form strong oxidation atmosphere down, almost all organic poison matter exhaustive oxidations can be resolved into carbon dioxide, the small-molecule substance that water etc. are nontoxic.Solar energy is to clean and the economic energy TiO 2The energy gap of photochemical catalyst is 3.2eV, in the solar radiation ripple that arrives ground, can only absorb to account for and reach the ultraviolet light of ground solar energy below 5% (λ＜387nm), can not effectively utilize to account for most visible light parts in the sunshine, utilization ratio is very low.Can expand TiO by to catalyst modification 2It is one of key technology that improves its solar energy utilization ratio that absorption spectrum moves to visible light.
Can to be photo-generated carrier by mixing be diffused into surperficial required time in the body shortens, and the body that has reduced photo-generated carrier is mutually compound, and specific area increases, and has strengthened the ability of catalyst absorption pollutant, thereby has improved the efficient of photocatalytic degradation pollutant.In recent years, researcher is round improving the photocatalysis quantum efficiency and expanding the photochemical catalyst spectral response range and carried out a series of researchs both at home and abroad, and catalyst modification can reduce following four aspects: (1) metal ion mixing; (2) noble metal loading; (3) semiconductor is compound; (4) organic dyestuff photoactivate.Therefore, make TiO by modification 2Visible light is had photoresponse, reduce electronics and hole-recombination probability, utilizing solar energy to solve environmental problem efficiently becomes TiO 2One big focus of photocatalysis field research.Foremost TiO 2Commercial product is Degussa P25, is used as marker and is widely used in laboratory and commercial Application exploratory development.
Metal ion and nonmetallic ion composite mixed is to TiO 2In the study on the modification, metal ion replaces TiO 2In Ti 4+, the doped energy-band of formation is near TiO 2The position of conduction band, and nonmetallic ion is to replace TiO 2Middle O 2-The position, introduce the oxygen room, the doped energy-band of formation is near TiO 2The position of valence band.Owing among the forbidden band, doped energy-band place, can receive TiO 2Excitation electron on the valence band or absorption long wavelength light are Zi making electron transition to TiO 2Conduction band on, thereby expanded TiO 2The scope of absorption spectrum.Can make light induced electron-hole to obtaining effective separation by the two synergy, thereby improve TiO 2Photocatalysis performance.Use Cu or N mix to it separately a lot of researchs, but Cu element and N element are not reported the research of its modification as yet by mixing simultaneously.
Summary of the invention
The purpose of this invention is to provide a kind of copper-nitrogen codope photocatalysis material of titanium dioxide;
Another object of the present invention provides a kind of Hydrothermal Preparation copper easy and simple to handle-nitrogen codope photocatalysis material of titanium dioxide that uses;
Another purpose of the present invention provides the purposes of copper-nitrogen codope photocatalysis material of titanium dioxide degradable organic pollutant.
A kind of copper of the present invention-nitrogen codope photocatalysis material of titanium dioxide adopts Hydrothermal Preparation, and concrete operations follow these steps to carry out:
A, titanium dioxide is placed the beaker of deionized water, add the compound that is dissolved with nitrogenous acetic acid solution and water-soluble copper successively, add alcohol solvent again, in temperature is under 20-50 ℃, place ultrasonic wave to handle 30min, it is mixed, add HCl and regulate pH 3-7;
B, the mixture of step a is transferred in the water heating kettle, places in the drying box of temperature programmed control and react, temperature is 120-180 ℃, and time of repose is 4-8h;
After c, reaction finish, be cooled to room temperature, the mixture among the step b is washed 3 times with deionized water and ethanol, centrifugal, obtain whiteness;
D, with the whiteness that step c obtains, place 60-80 ℃ of vacuum drying chamber temperature, dry 2-4h can obtain copper-nitrogen codope photocatalysis material of titanium dioxide.
Step a copper-containing compound is CuCl 22H 2O, Cu (NO 3) 2Or Cu (CH 3COO) 2H 2O, nitrogenous compound are H 2NCONH 2
Ti among the step a in the compound of titanium dioxide, nitrogen and copper: N: the mol ratio of Cu element is: 1: 0.01-0.05: 0.001-0.01.
Described copper-nitrogen codope photocatalysis material of titanium dioxide is as the purposes in the preparation degradable organic pollutant.
A kind of copper of the present invention-nitrogen codope photocatalysis material of titanium dioxide, this material is white powder, and is water insoluble.
The invention provides a kind of copper-nitrogen codope photocatalysis material of titanium dioxide, it is fast that this material has a degradation speed to the organic pollutant wastewater of difficult degradation and pollutant, non-secondary pollution, catalyst is easy to get, cheaply, operating cost is low, and equipment is simple, the small investment good effectiveness.
TiO among the present invention 2For German Dugess produces P-25, the copper-containing compound of doping is the commercially available prod, and the nitrogen of doping is in the urea and provides.
Description of drawings
Fig. 1 is an X-ray diffracting spectrum of the present invention, and wherein a is the X-ray diffracting spectrum of P25, and b is the X-ray diffracting spectrum of copper-nitrogen codope photocatalysis material of titanium dioxide;
Fig. 2 is photocatalytic degradation methylene blue ultraviolet-visible absorption spectroscopy under the UV-irradiation of the present invention.
Fig. 3 for the present invention under same light source irradiation and test condition, P25 and material degradation methylene blue comparison diagram of the present invention.
The specific embodiment
The present invention is described in detail below in conjunction with drawings and Examples:
Embodiment 1:
By Ti: N: the mol ratio of Cu element is: 1: 0.01: 0.001, take by weighing TiO respectively 2, H 2NCONH 2And CuCl 22H 2O is with TiO 2Pressed powder places the beaker of 15mL deionized water, adds successively to be dissolved with H 2NCONH 2Acetic acid solution 25mL and CuCl 22H 2O adds solvent strength 95% ethanol 20mL again, is under 20 ℃ in temperature, places ultrasonic wave to handle 30min, and it is mixed, and adds HCl and regulates pH3;
Mixture system is transferred in the water heating kettle, places the drying box of temperature programmed control to react, 120 ℃ of temperature, quiescent time 6h;
Reaction finishes the back takes out, and is cooled to room temperature, and mixture system is used concentration 95% ethanol and deionized water washing 3 times successively, centrifugal, obtains whiteness;
With the whiteness that obtains, place 60 ℃ of vacuum drying chamber temperature, dry 2h can obtain white powder material copper-nitrogen codope photocatalysis material of titanium dioxide (Cu-N-P25).
The photocatalysis experiment:
Take by weighing the Cu-N-P25 nano-powder 0.5g that embodiment 1 obtains, add in the 200mL methylene blue solution, place ultrasonic 30min, magnetic agitation 30min fully disperses it again, and make its absorption reach balance, in will the mixed solution impouring quartz reactor after adsorption equilibrium, with 300w ultraviolet ray high pressure xenon lamp, the photocatalytic degradation reaction be carried out in irradiation, the concentration of sampling and measuring methylene blue at regular intervals, sample is 10cm apart from the distance of light source; From Fig. 2 as seen, along with the variation of time, methylene blue had degradation speed faster in preceding 60 minutes, and that can degrade in 2 hours is more thorough, and degradation rate reaches 95%; As can be seen from Figure 3, relative P25, the copper of gained of the present invention-nitrogen codope photocatalysis material of titanium dioxide within a short period of time is comparatively thorough to the methylene blue degraded.
Embodiment 2:
By Ti: N: the mol ratio of Cu element is: 1: 0.02: 0.003, take by weighing respectively and take by weighing TiO respectively 2, H 2NCONH 2And Cu (NO 3) 2, with TiO 2Pressed powder places the beaker of 15mL deionized water, adds successively to be dissolved with H 2NCONH 2Acetic acid solution 25mL and Cu (NO 3) 2, add solvent strength 95% ethanol 20mL again, under 30 ℃ of temperature, place ultrasonic wave to handle 30min, it is mixed, add HCl and regulate pH4;
Mixture system is transferred in the water heating kettle, places the drying box of temperature programmed control to react, 150 ℃ of temperature, quiescent time 3h;
Reaction finishes the back takes out, and is cooled to room temperature, and mixture system is used concentration 95% ethanol and deionized water washing 3 times successively, centrifugal, obtains whiteness;
With the whiteness that obtains, place 70 ℃ of dry 3h of vacuum drying chamber temperature, can obtain white powder material copper-nitrogen codope photocatalysis material of titanium dioxide (Cu-N-P25).
According to the experiment of the photocatalysis among the embodiment 1, take by weighing this sample of 0.5g and carry out the photocatalysis experiment, after xenon lamp was waited according to 1h, its degradation rate to methylene blue was 96%.
Embodiment 3:
By Ti: N: the mol ratio of Cu element is: 1: 0.03: 0.005, take by weighing respectively and take by weighing TiO respectively 2, H 2NCONH 2And Cu (NO 3) 2, with TiO 2Pressed powder is placed in the beaker of 15mL deionized water, adds successively to be dissolved with H 2NCONH 2Acetic acid solution 25mL and Cu (CH 3COO) 2H 2O adds solvent strength 95% ethanol 20mL again, is under 40 ℃ in temperature, places ultrasonic wave to handle 30min, and it is mixed, and adds HCl and regulates pH 5;
Mixture system is transferred in the water heating kettle, places the drying box of temperature programmed control to react, 150 ℃ of temperature, quiescent time 6h;
Reaction finishes the back takes out, and is cooled to room temperature, and mixture system is used concentration 95% ethanol and deionized water washing 3 times successively, centrifugal, obtains whiteness;
With the whiteness that obtains, place 75 ℃ of vacuum drying chamber temperature, dry 2.5h can obtain white powder material copper-nitrogen codope photocatalysis material of titanium dioxide (Cu-N-P25).
According to the experiment of the photocatalysis among the embodiment 1, take by weighing this sample of 0.5g and carry out the photocatalysis experiment, after xenon lamp was waited according to 1h, its degradation rate to methylene blue was 98%.
Embodiment 4:
By Ti: N: the mol ratio of Cu element is: 1: 0.04: 0.008, take by weighing respectively and take by weighing TiO respectively 2, H 2NCONH 2And Cu (NO 3) 2, with TiO 2Pressed powder places the beaker of 15mL deionized water, adds successively to be dissolved with H 2NCONH 2Acetic acid solution 25mL and Cu (NO 3) 2, adding solvent strength 95% ethanol 20mL again, temperature is under 45 ℃, places ultrasonic wave to handle 30min, and it is mixed, and adds HCl and regulates pH6;
Mixture system is transferred in the water heating kettle, places the drying box of temperature programmed control to carry out 160 ℃ of reaction temperatures, quiescent time 7h;
Reaction finishes the back takes out, and is cooled to room temperature, and mixture system is used concentration 95% ethanol and deionized water washing 3 times successively, centrifugal, obtains whiteness;
With the whiteness that obtains, place 75 ℃ of vacuum drying chamber temperature, dry 3.5h can obtain white powder material copper-nitrogen codope photocatalysis material of titanium dioxide (Cu-N-P25).
According to the experiment of the photocatalysis among the embodiment 1, take by weighing this sample of 0.5g and carry out the photocatalysis experiment, after xenon lamp was waited according to 1h, its degradation rate to methylene blue was 97%.
Embodiment 5:
By Ti: N: the mol ratio of Cu element is: 1: 0.05: 0.01, take by weighing respectively and take by weighing TiO respectively 2, H 2NCONH 2And Cu (NO 3) 2, with TiO 2Pressed powder places the beaker of 15mL deionized water, adds successively to be dissolved with H 2NCON H 2Acetic acid solution 25mL and CuCl 22H 2O adds solvent strength 95% ethanol 20mL again, is under 50 ℃ in temperature, places ultrasonic wave to handle 30min, and it is mixed, and adds HCl and regulates pH7;
Mixture system is transferred in the water heating kettle, places in the drying box of temperature programmed control and react, temperature is 180 ℃, and time of repose is 8h;
Reaction finishes the back takes out, and is cooled to room temperature, and mixture system is used concentration 95% ethanol and deionized water washing 3 times successively, centrifugal, obtains whiteness;
With the whiteness that obtains, place 80 ℃ of vacuum drying chamber temperature, dry 4h can obtain white powder material copper-nitrogen codope photocatalysis material of titanium dioxide (Cu-N-P25).
According to the experiment of the photocatalysis among the embodiment 1, take by weighing this sample of 0.5g and carry out the photocatalysis experiment, after xenon lamp was waited according to 1h, its degradation rate to methylene blue was 99%.

Claims (4)

1. copper-nitrogen codope photocatalysis material of titanium dioxide is characterized in that adopting Hydrothermal Preparation, and concrete operations follow these steps to carry out:
A, titanium dioxide is placed the beaker of deionized water, add successively and be dissolved with nitrogenous acetic acid solution and water-soluble copper compound, add alcohol solvent again, in temperature is under 20-50 ℃, place ultrasonic wave to handle 30min, it is mixed, add HCl and regulate pH 3-7;
B, the mixture of step a is transferred in the water heating kettle, places in the drying box of temperature programmed control and react, temperature is 120-180 ℃, and time of repose is 4-8h;
After c, reaction finish, be cooled to room temperature, the mixture among the step b is washed 3 times with deionized water and ethanol, centrifugal, obtain whiteness;
D, with the whiteness that step c obtains, place 60-80 ℃ of vacuum drying chamber temperature, dry 2-4h can obtain copper-nitrogen codope photocatalysis material of titanium dioxide.
2. copper according to claim 1-nitrogen codope photocatalysis material of titanium dioxide is characterized in that step a copper-containing compound is CuCl 22H 2O, Cu (NO 3) 2Or Cu (CH 3COO) 2H 2O, nitrogenous compound are H 2NCONH 2
3. copper according to claim 2-nitrogen codope photocatalysis material of titanium dioxide, it is characterized in that the Ti in the compound of titanium dioxide, nitrogen and copper among the step a: N: the mol ratio of Cu element is: 1: 0.01-0.05: 0.001-0.01.
4. copper according to claim 1-nitrogen codope photocatalysis material of titanium dioxide is as the purposes in the preparation degradable organic pollutant.
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Cited By (8)

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CN103239827A (en) * 2013-05-24 2013-08-14 中国科学院新疆理化技术研究所 Method for dechlorinating chlorophenol pollutants by bromine potassium borate under photocatalysis
CN103418334A (en) * 2013-08-05 2013-12-04 江苏大学 Preparation method of highly adsorptive N, I co-doped TiO2porous network powder
CN103831123A (en) * 2014-02-17 2014-06-04 中国科学院过程工程研究所 Co-doped titanium dioxide catalyst and a preparing method
CN108993503A (en) * 2017-06-06 2018-12-14 天津城建大学 A method of copper/nitrogen is prepared based on xerogel-hydro-thermal method and is co-doped with nano TiO 2 powder
CN109663609A (en) * 2017-10-16 2019-04-23 天津城建大学 A method of copper/nitrogen is prepared based on xerogel -ol thermal method and is co-doped with nano TiO 2 powder
CN109999888A (en) * 2019-05-06 2019-07-12 西北师范大学 The preparation of copper and nitrogen co-doped modified titanium dioxide photocatalyst and the application for toluene of degrading
CN111632619A (en) * 2020-06-17 2020-09-08 湖北民族大学 Copper-nitrogen co-doped titanium dioxide photocatalytic material, preparation method and application
CN111952078A (en) * 2019-05-15 2020-11-17 青岛海尔特种电冰柜有限公司 Thin-film solar cell for refrigerating device and preparation method and application thereof

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CN107088405A (en) * 2017-04-24 2017-08-25 太原理工大学 A kind of preparation method of modified nano-titanium dioxide photochemical catalyst
CN109529825A (en) * 2018-11-26 2019-03-29 中南民族大学 One kind being based on sylphon shape TiO2Nano bionic Photoreactor and its preparation method and application

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CN103239827A (en) * 2013-05-24 2013-08-14 中国科学院新疆理化技术研究所 Method for dechlorinating chlorophenol pollutants by bromine potassium borate under photocatalysis
CN103418334A (en) * 2013-08-05 2013-12-04 江苏大学 Preparation method of highly adsorptive N, I co-doped TiO2porous network powder
CN103418334B (en) * 2013-08-05 2016-04-27 江苏大学 High absorbent-type N, I codope TiO 2porous network raw powder's production technology
CN103831123A (en) * 2014-02-17 2014-06-04 中国科学院过程工程研究所 Co-doped titanium dioxide catalyst and a preparing method
CN103831123B (en) * 2014-02-17 2015-12-30 中国科学院过程工程研究所 A kind of codope TiO 2catalysts and its preparation method
CN108993503A (en) * 2017-06-06 2018-12-14 天津城建大学 A method of copper/nitrogen is prepared based on xerogel-hydro-thermal method and is co-doped with nano TiO 2 powder
CN108993503B (en) * 2017-06-06 2021-06-01 天津城建大学 Cu/N codoped TiO prepared based on xerogel-hydrothermal method2Application of nano powder in degrading acetone in photocatalytic reaction
CN109663609A (en) * 2017-10-16 2019-04-23 天津城建大学 A method of copper/nitrogen is prepared based on xerogel -ol thermal method and is co-doped with nano TiO 2 powder
CN109999888A (en) * 2019-05-06 2019-07-12 西北师范大学 The preparation of copper and nitrogen co-doped modified titanium dioxide photocatalyst and the application for toluene of degrading
CN111952078A (en) * 2019-05-15 2020-11-17 青岛海尔特种电冰柜有限公司 Thin-film solar cell for refrigerating device and preparation method and application thereof
CN111952078B (en) * 2019-05-15 2023-07-14 青岛海尔特种电冰柜有限公司 Thin film solar cell for refrigeration device and preparation method and application thereof
CN111632619A (en) * 2020-06-17 2020-09-08 湖北民族大学 Copper-nitrogen co-doped titanium dioxide photocatalytic material, preparation method and application

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