CN102553569A - Method for preparing nitrogen-doped bismuth tungstate powder photocatalyst through microwave hydrothermal method - Google Patents

Method for preparing nitrogen-doped bismuth tungstate powder photocatalyst through microwave hydrothermal method Download PDF

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CN102553569A
CN102553569A CN2011104504526A CN201110450452A CN102553569A CN 102553569 A CN102553569 A CN 102553569A CN 2011104504526 A CN2011104504526 A CN 2011104504526A CN 201110450452 A CN201110450452 A CN 201110450452A CN 102553569 A CN102553569 A CN 102553569A
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photochemical catalyst
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谈国强
宋丽花
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Shaanxi University of Science and Technology
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Abstract

The invention provides a method for preparing a nitrogen-doped bismuth tungstate powder photocatalyst through a microwave hydrothermal method. The method comprises the following steps of: adding de-ionized water into bismuth nitrate pentahydrate and sodium tungstate dihydrate serving as raw materials and urea serving as an N source, stirring to uniformly mix the raw materials, stopping the stirring and producing white precipitate; placing in an ultrasonic instrument to perform ultrasonic treatment for 10-30 minutes; performing complete precipitation reaction to obtain precursor of microwave hydrothermal reaction; transferring the precursor into a reaction kettle; reacting by using the microwave hydrothermal method for 30-90 minutes at 160-200 DEG C; and taking out of the reaction kettle, collecting the precipitate, cleaning and drying. The method has the advantages of low reaction temperature of about 180 DEG C and short reaction time of probability 50-60 minutes; and the prepared powder has high reaction activity and low energy consumption and is environmentally-friendly.

Description

Microwave-hydrothermal method prepares the method for nitrogen doping wolframic acid bismuth meal body photochemical catalyst
Technical field
The invention belongs to field of functional materials, relate to the method that a kind of microwave hydrothermal method prepares nitrogen doping wolframic acid bismuth meal body photochemical catalyst.
Background technology
Photocatalytic is one of semi-conductive special performance; Utilize the semiconductor light-catalyst can photolysis water hydrogen; Purify the air of a room photocatalysis automatically cleaning, mildew-resistant, photocatalysis antibacterial; Photocatalysis sewage processing etc., photocatalysis technology administer the pollution protection environment, tapping a new source of energy has broad application prospects aspect restructuring the use of energy.
Tradition photochemical catalyst titanium dioxide (TiO 2) have advantages such as cost is low, nontoxic, high, the easy preparation of stability, be to study more and actual photochemical catalyst commonly used in the past few decades, however because TiO 2Energy gap is bigger, only under UV-irradiation, just has photocatalytic activity, and the energy in ultraviolet light zone accounts for the less than 5% of solar energy, and the utilization rate of sunshine is not high.
Semiconductor bismuth tungstate (Bi 2WO 6) be the most bismuth laminated (Aurivillius) oxide, contain WO 6Perovskite structure lamella and Bi 2O 2Layer, stability is high, and environmental friendliness has performances such as dielectric, luminous, ion conductor, catalysis, is widely used in association area.With TiO 2Compare Bi 2WO 6Energy gap narrower, have high visible light response.1999, reported first such as Kudo utilize Bi 2WO 6Successful decomposition water produces H under visible radiation 2, afterwards, Zou equals discovery in 2004 at visible light-responded Bi down 2WO 6The organic pollutions such as chloroform and acetaldehyde of can degrading effectively.In order to promote that photo-generated carrier separates, migration, it is compound to suppress carrier, improves quantum efficiency, and people carry out nonmetallic ion-doped study on the modification to the bismuth tungstate photochemical catalyst, further improve its visible light catalysis activity.
High temperature solid-state method is a kind of process of traditional preparation powder, has advantages such as cost is low, output is big, preparation technology is simple, early Bi 2WO 6High-temperature solid phase reaction method is adopted in the preparation of powder more, but this method energy consumption is big, efficient is low, and the particle that makes is big, specific area is less, causes photocatalytic activity relatively low.
Hydro-thermal is synthetic to be meant in special closed reactor (autoclave); Adopt the aqueous solution as reaction system; Through reaction system is heated, pressurizes (or spontaneous vapour pressure); Create the reaction environment of a relatively-high temperature, high pressure, make common indissoluble or insoluble substance dissolves and recrystallization come the synthesizing inorganic solid phase material.
The electromagnetic wave that it is 1mm in the 0.1mm scope that microwave typically refers to wavelength, its correspondent frequency scope is 300MHz～300GHz.To be electromagnetic energy be radiated medium inside with the form of ripple in heating using microwave, utilizes the dielectric loss heating of medium.Because this kind energy is from reactant solvents inside, the medium that itself need not conduct heat do not lean on convection current; Can make medium molecule reach the state of activation in the short time at the utmost point, the motion and the collision of aggravation molecule, fast reaction speed greatly; Shorten reaction time; And because of inside and outside heating simultaneously, system is heated evenly, no hysteresis effect.Microwave also has non-thermal effect except having the dielectric heating effect.Because the ability of material absorbing microwave energy depends on the dielectric property of self, the ability that different medium absorbs microwave is different, can heat selectively, thereby make chemical reaction have certain selectivity.
Microwave-hydrothermal method as mode of heating, prepares a kind of new method of nano-powder in conjunction with traditional hydro-thermal method with microwave, has the incomparable superiority of some other method.Microwave hydrothermal is synthetic has compared following characteristics with conventional solid state reaction:
(1) low temperature of microwave hydrothermal, equipressure, solution condition, help defective few, be orientated, the growth of perfect cystal, and the granularity of synthetic product degree of crystallinity height and product crystal is easy to control.
(2) the microwave hydrothermal rate of heat addition is fast, and system is heated evenly, and no hysteresis effect can be synthesized purity height, fine size, the uniform powder of grain size distribution at short notice.
(3) ambiance under the hydrothermal condition is easy to regulate, and helps the generation of lower valency, middle valence state and special valence state compound, and can mix equably.
(4) owing to the change of reactant reaction performance under the microwave hydrothermal condition, active raising, the synthetic reaction that microwave hydro-thermal synthesis method might replace solid phase reaction and be difficult to carry out.
Summary of the invention
Technical problem to be solved by this invention provides the method that a kind of microwave-hydrothermal method prepares nitrogen doping wolframic acid bismuth meal body photochemical catalyst; Its reaction temperature is low; Reaction time is short; The preparation powder granule little, specific area is big, photocatalytic activity is high, and technology is simple, efficient is high, energy consumption is low, with low cost, environmentally friendly.
For realizing above-mentioned purpose, the method that the present invention also provides a kind of microwave-hydrothermal method to prepare nitrogen doping wolframic acid bismuth meal body photochemical catalyst is a raw material with five water bismuth nitrates, tungstate dihydrate acid sodium, and urea is the N source; Add deionized water, stirring mixes raw material, stops to stir the back and produces white precipitate; White precipitate is put into Ultrasound Instrument, ultrasonic 10～30min, precipitation reaction is complete; Get the precursor liquid of microwave hydrothermal reaction, precursor liquid is moved into agitated reactor, adopt microwave-hydrothermal method at 160～200 ℃ of reaction 30～90mins; Take out agitated reactor, the collecting precipitation thing cleans dry the getting final product in extremely neutral back.
In the mixture that said five water bismuth nitrates, tungstate dihydrate acid sodium, urea and water form, the molar concentration of bismuth nitrate is 0.04～2mol/L, and the molar concentration of sodium tungstate is 0.02～0.1mol/L, and the mol ratio of N and Bi is 0.4～2;
The power of said microwave hydrothermal reaction is 300～500W;
Said agitated reactor is the teflon-lined agitated reactor.
The method that microwave hydrothermal method of the present invention prepares nitrogen doping wolframic acid bismuth meal body photochemical catalyst has the following advantages: compare with the routine heating; Heating using microwave does not need the conduction and the convection current of heat, makes medium molecule reach the state of activation in the short time at the utmost point, the motion and the collision of aggravation molecule; Fast reaction speed greatly; Shorten reaction time, and because of inside and outside heating simultaneously, system is heated evenly; No hysteresis effect, so the inventive method energy consumption is little, efficient is high, the powder granule of preparation is little, specific area is big, photocatalytic activity is high.
Description of drawings
Fig. 1 is nitrogen doping wolframic acid bismuth meal body of the present invention and pure tungsten acid bismuth meal body XRD figure (reaction temperature is 180 ℃, and the reaction time is 60mins);
Fig. 2 is the XRD figure (reaction temperature be 180 ℃, reaction time be 60mins) of nitrogen doping wolframic acid bismuth meal body of the present invention and pure tungsten acid bismuth meal body diffraction maximum position in 2 θ=27.5～29.0 °;
Fig. 3 is the degradation rate figure (light source: xenon lamp, 350W of nitrogen doping wolframic acid bismuth meal body of the present invention and pure tungsten acid bismuth meal body rhodamine B solution as photochemical catalyst and when not adding catalyst; RhB concentration: 5ppm).
The specific embodiment
Embodiment 1
Step 1: take by weighing Bi (NO 3) 35H 2O, Na 2WO 42H 2O and CO (NH 2) 2Put into beaker, in beaker, add appropriate amount of deionized water, wherein Bi (NO 3) 3Concentration is 0.05mol/L, Na 2WO 4Concentration is 0.025mol/L, R NFor: R N=0 (R NMol ratio for N and Bi), fully stir until producing white precipitate, the container that fills white precipitate is put into the ultrasonic 30mins of Ultrasound Instrument, precipitation reaction is complete, gets the precursor liquid of microwave hydrothermal reaction;
Step 2: the precursor liquid of step 1 gained is put into the teflon-lined agitated reactor, again agitated reactor is put into microwave hydrothermal reaction MDS-8, setting power 400w, reaction stops reaction after 60 minutes under temperature is 180 ℃;
Step 3: after being cooled to room temperature, take out the sediment in the agitated reactor, water and absolute ethyl alcohol to neutral, 80 ℃ of dryings 10 hours down, promptly get nitrogen doping wolframic acid bismuth meal body photochemical catalyst with the sediment washing at last.
Embodiment 2
Step 1: take by weighing Bi (NO 3) 35H 2O, Na 2WO 42H 2O and CO (NH 2) 2Put into beaker, in beaker, add appropriate amount of deionized water, wherein Bi (NO 3) 3Concentration is 0.1mol/L, Na 2WO 4Concentration is 0.05mol/L, R NBe R N=2 (R NMol ratio for N and Bi), fully stir until producing white precipitate, the container that fills white precipitate is put into the ultrasonic 30mins of Ultrasound Instrument, precipitation reaction is complete, gets the precursor liquid of microwave hydrothermal reaction;
Step 2: the precursor liquid of step 1 gained is put into the teflon-lined agitated reactor, again agitated reactor is put into microwave hydrothermal reaction MDS-8, setting power 500w, reaction stops reaction after 30 minutes under temperature is 200 ℃;
Step 3: after being cooled to room temperature, take out the sediment in the agitated reactor, water and absolute ethyl alcohol to neutral, 80 ℃ of dryings 10 hours down, promptly get nitrogen doping wolframic acid bismuth meal body photochemical catalyst with the sediment washing at last.
Embodiment 3
Step 1: take by weighing Bi (NO 3) 35H 2O, Na 2WO 42H 2O and CO (NH 2) 2Put into beaker, in beaker, add appropriate amount of deionized water, wherein Bi (NO 3) 3Concentration is 0.04mol/L, Na 2WO 4Concentration is 0.02mol/L, R NBe R N=0.8 (R NMol ratio for N and Bi), fully stir until producing white precipitate, the container that fills white precipitate is put into the ultrasonic 10mins of Ultrasound Instrument, precipitation reaction is complete, gets the precursor liquid of microwave hydrothermal reaction;
Step 2: the precursor liquid of step 1 gained is put into the teflon-lined agitated reactor, again agitated reactor is put into microwave hydrothermal reaction MDS-8, setting power 350w, reaction stops reaction after 40 minutes under temperature is 200 ℃;
Step 3: after being cooled to room temperature, take out the sediment in the agitated reactor, water and absolute ethyl alcohol to neutral, 80 ℃ of dryings 10 hours down, promptly get nitrogen doping wolframic acid bismuth meal body photochemical catalyst with the sediment washing at last.
Embodiment 4
Step 1: take by weighing Bi (NO 3) 35H 2O, Na 2WO 42H 2O and CO (NH 2) 2Put into beaker, in beaker, add appropriate amount of deionized water, wherein Bi (NO 3) 3Concentration is 0.08mol/L, Na 2WO 4Concentration is 0.04mol/L, R NBe R N=0.4 (R NMol ratio for N and Bi), fully stir until producing white precipitate, the container that fills white precipitate is put into the ultrasonic 25mins of Ultrasound Instrument, precipitation reaction is complete, gets the precursor liquid of microwave hydrothermal reaction;
Step 2: the precursor liquid of step 1 gained is put into the teflon-lined agitated reactor, again agitated reactor is put into microwave hydrothermal reaction MDS-8, setting power 350w, reaction stops reaction after 60 minutes under temperature is 180 ℃;
Step 3: after being cooled to room temperature, take out the sediment in the agitated reactor, water and absolute ethyl alcohol to neutral, 80 ℃ of dryings 10 hours down, promptly get nitrogen doping wolframic acid bismuth meal body photochemical catalyst with the sediment washing at last.
Embodiment 5
Step 1: take by weighing Bi (NO 3) 35H 2O, Na 2WO 42H 2O and CO (NH 2) 2Put into beaker, in beaker, add appropriate amount of deionized water, wherein Bi (NO 3) 3Concentration is 0.5mol/L, Na 2WO 4Concentration is 0.1mol/L, R NBe R N=1 (R NMol ratio for N and Bi), fully stir until producing white precipitate, the container that fills white precipitate is put into the ultrasonic 20mins of Ultrasound Instrument, precipitation reaction is complete, gets the precursor liquid of microwave hydrothermal reaction;
Step 2: the precursor liquid of step 1 gained is put into the teflon-lined agitated reactor, again agitated reactor is put into microwave hydrothermal reaction MDS-8, setting power 300w, reaction stops reaction after 90 minutes under temperature is 160 ℃;
Step 3: after being cooled to room temperature, take out the sediment in the agitated reactor, water and absolute ethyl alcohol to neutral, 80 ℃ of dryings 10 hours down, promptly get nitrogen doping wolframic acid bismuth meal body photochemical catalyst with the sediment washing at last.
Embodiment 6
Step 1: take by weighing Bi (NO 3) 35H 2O, Na 2WO 42H 2O and CO (NH 2) 2Put into beaker, in beaker, add appropriate amount of deionized water, wherein Bi (NO 3) 3Concentration is 0.9mol/L, Na 2WO 4Concentration is 0.06mol/L, R NBe R N=1.2 (R NMol ratio for N and Bi), fully stir until producing white precipitate, the container that fills white precipitate is put into the ultrasonic 15mins of Ultrasound Instrument, precipitation reaction is complete, gets the precursor liquid of microwave hydrothermal reaction;
Step 2: the precursor liquid of step 1 gained is put into the teflon-lined agitated reactor, again agitated reactor is put into microwave hydrothermal reaction MDS-8, setting power 450w, reaction stops reaction after 80 minutes under temperature is 170 ℃;
Step 3: after being cooled to room temperature, take out the sediment in the agitated reactor, water and absolute ethyl alcohol to neutral, 80 ℃ of dryings 10 hours down, promptly get nitrogen doping wolframic acid bismuth meal body photochemical catalyst with the sediment washing at last.
Embodiment 7
Step 1: take by weighing Bi (NO 3) 35H 2O, Na 2WO 42H 2O and CO (NH 2) 2Put into beaker, in beaker, add appropriate amount of deionized water, wherein Bi (NO 3) 3Concentration is 1.3mol/L, Na 2WO 4Concentration is 0.08mol/L, R NBe R N=1.5 (R NMol ratio for N and Bi), fully stir until producing white precipitate, the container that fills white precipitate is put into the ultrasonic 15mins of Ultrasound Instrument, precipitation reaction is complete, gets the precursor liquid of microwave hydrothermal reaction;
Step 2: the precursor liquid of step 1 gained is put into the teflon-lined agitated reactor, again agitated reactor is put into microwave hydrothermal reaction MDS-8, setting power 480w, reaction stops reaction after 70 minutes under temperature is 180 ℃;
Step 3: after being cooled to room temperature, take out the sediment in the agitated reactor, water and absolute ethyl alcohol to neutral, 80 ℃ of dryings 10 hours down, promptly get nitrogen doping wolframic acid bismuth meal body photochemical catalyst with the sediment washing at last.
Embodiment 8
Step 1: take by weighing Bi (NO 3) 35H 2O, Na 2WO 42H 2O and CO (NH 2) 2Put into beaker, in beaker, add appropriate amount of deionized water, wherein Bi (NO 3) 3Concentration is 1.6mol/L, Na 2WO 4Concentration is 0.1mol/L, R NBe R N=1.8 (R NMol ratio for N and Bi), fully stir until producing white precipitate, the container that fills white precipitate is put into the ultrasonic 10mins of Ultrasound Instrument, precipitation reaction is complete, gets the precursor liquid of microwave hydrothermal reaction;
Step 2: the precursor liquid of step 1 gained is put into the teflon-lined agitated reactor, again agitated reactor is put into microwave hydrothermal reaction MDS-8, setting power 500w, reaction stops reaction after 65 minutes under temperature is 185 ℃;
Step 3: after being cooled to room temperature, take out the sediment in the agitated reactor, water and absolute ethyl alcohol to neutral, 80 ℃ of dryings 10 hours down, promptly get nitrogen doping wolframic acid bismuth meal body photochemical catalyst with the sediment washing at last.
Embodiment 9
Step 1: take by weighing Bi (NO 3) 35H 2O, Na 2WO 42H 2O and CO (NH 2) 2Put into beaker, in beaker, add appropriate amount of deionized water, wherein Bi (NO 3) 3Concentration is 2mol/L, Na 2WO 4Concentration is 0.1mol/L, R NBe R N=2 (R NMol ratio for N and Bi), fully stir until producing white precipitate, the container that fills white precipitate is put into the ultrasonic 10mins of Ultrasound Instrument, precipitation reaction is complete, gets the precursor liquid of microwave hydrothermal reaction;
Step 2: the precursor liquid of step 1 gained is put into the teflon-lined agitated reactor, again agitated reactor is put into microwave hydrothermal reaction MDS-8, setting power 500w, reaction stops reaction after 50 minutes under temperature is 200 ℃;
Step 3: after being cooled to room temperature, take out the sediment in the agitated reactor, water and absolute ethyl alcohol to neutral, 80 ℃ of dryings 10 hours down, promptly get nitrogen doping wolframic acid bismuth meal body photochemical catalyst with the sediment washing at last.
With the thing phase composition structure of XRD determining powder, its result is as depicted in figs. 1 and 2, as can beappreciated from fig. 1: synthetic Bi 2WO 6((JCPDS No.39-0256's powder) conforms to, and powder is Bi with PDF standard diagram card 2WO 6The quadrature crystalline phase, mixing does not cause the generation of new crystalline phase.Can find out that from Fig. 2 the nitrogen doping wolframic acid bismuth meal body diffraction maximum for preparing with the inventive method to low-angle minor shifts has taken place, this is because N 3-Ion ratio O 2-Radius is big.
Fig. 3 reaches the degradation rate figure of rhodamine B solution when not adding catalyst as photochemical catalyst for nitrogen doping wolframic acid bismuth meal body of the present invention and pure tungsten acid bismuth meal body; Can find out; Nitrogen doping wolframic acid bismuth meal body and pure tungsten acid bismuth meal body all have good visible light activity, and the visible light activity of nitrogen doping enhancing bismuth tungstate powder.
The above is merely one embodiment of the present invention; It or not whole or unique embodiment; The conversion of any equivalence that those of ordinary skills take technical scheme of the present invention through reading specification of the present invention is claim of the present invention and contains.

Claims (5)

1. a microwave-hydrothermal method prepares the method for nitrogen doping wolframic acid bismuth meal body photochemical catalyst, it is characterized in that: with five water bismuth nitrates, tungstate dihydrate acid sodium is raw material, and urea is the N source; Add deionized water, stirring mixes raw material, stops to stir the back and produces white precipitate; White precipitate is put into Ultrasound Instrument, ultrasonic 10～30min, precipitation reaction is complete; Get the precursor liquid of microwave hydrothermal reaction, precursor liquid is moved into agitated reactor, adopt microwave-hydrothermal method at 160～200 ℃ of reaction 30～90mins; Take out agitated reactor, the collecting precipitation thing cleans dry the getting final product in extremely neutral back.
2. microwave-hydrothermal method as claimed in claim 1 prepares the method for nitrogen doping wolframic acid bismuth meal body photochemical catalyst; It is characterized in that: in the mixture that said five water bismuth nitrates, tungstate dihydrate acid sodium, urea and water form; The molar concentration of bismuth nitrate is 0.04～2mol/L; The molar concentration of sodium tungstate is 0.02～0.1mol/L, and the mol ratio of N and Bi is 0.4～2.
3. microwave-hydrothermal method as claimed in claim 1 prepares the method for nitrogen doping wolframic acid bismuth meal body photochemical catalyst, it is characterized in that: the power of said microwave hydrothermal reaction is 300～500W.
4. microwave-hydrothermal method as claimed in claim 1 prepares the method for nitrogen doping wolframic acid bismuth meal body photochemical catalyst, and it is characterized in that: said agitated reactor is the teflon-lined agitated reactor.
5. a microwave-hydrothermal method prepares the method for nitrogen doping wolframic acid bismuth meal body photochemical catalyst, it is characterized in that: may further comprise the steps:
Step 1: take by weighing Bi (NO 3) 35H 2O, Na 2WO 42H 2O and CO (NH 2) 2Put into beaker, in beaker, add deionized water, after stirring, form mixture A, wherein Bi (NO 3) 3Concentration is 0.04～2mol/L, Na 2WO 4Concentration is 0.02～0.1mol/L, and the mol ratio of N and Bi is 0.4～2, leaves standstill until producing white precipitate, and the beaker that fills white precipitate is put into the ultrasonic 10～30mins of Ultrasound Instrument, and precipitation reaction is complete, gets the precursor liquid of microwave hydrothermal reaction;
Step 2: the precursor liquid of step 1 gained is put into the teflon-lined agitated reactor; Again agitated reactor is put into microwave hydrothermal reaction; Set the power 300～500w of microwave hydrothermal reaction, be 160～200 ℃ in temperature and stop reaction behind reaction 30～90mins down;
Step 3: after question response was accomplished, the sediment in the agitated reactor was taken out in cooling, spends deionised water to neutrality, uses absolute ethanol washing again, at last at 80 ℃ of following freeze-day with constant temperature, promptly obtains nitrogen doping wolframic acid bismuth meal body photochemical catalyst.
CN2011104504526A 2011-12-19 2011-12-19 Method for preparing nitrogen-doped bismuth tungstate powder photocatalyst through microwave hydrothermal method Pending CN102553569A (en)

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CN103623812A (en) * 2013-09-12 2014-03-12 陕西科技大学 Flake-shaped visible light response Yb-modified Bi2WO6 photocatalyst as well as preparation method and application thereof
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CN103638923B (en) * 2013-09-12 2015-10-28 陕西科技大学 A kind of rare earth element nd doping Bi 2wO 6composite photo-catalyst and its preparation method and application
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CN109420490A (en) * 2017-08-29 2019-03-05 钱诗旋 A kind of Bi2WO6C composite and preparation method thereof
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CN103611527A (en) * 2013-09-12 2014-03-05 陕西科技大学 Visible-light response Ce doped Bi2WO6 microcrystal, preparation method and application thereof
CN103623812A (en) * 2013-09-12 2014-03-12 陕西科技大学 Flake-shaped visible light response Yb-modified Bi2WO6 photocatalyst as well as preparation method and application thereof
CN103623813A (en) * 2013-09-12 2014-03-12 陕西科技大学 Visible-light response Er/Bi2WO6 microspheres and preparation method and application thereof
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CN109420490A (en) * 2017-08-29 2019-03-05 钱诗旋 A kind of Bi2WO6C composite and preparation method thereof
CN107552081A (en) * 2017-09-11 2018-01-09 常州大学 A kind of preparation method of N doping manganese molybdate photochemical catalyst
CN112958135A (en) * 2021-03-02 2021-06-15 陕西科技大学 Cerium-doped and cerium-nitrogen-codoped bismuth tungstate photocatalytic material and preparation method thereof
CN113333009A (en) * 2021-05-29 2021-09-03 安徽大学 Nitrogen-doped gamma-Bi2MoO6Method for preparing photocatalyst
CN113333009B (en) * 2021-05-29 2022-02-18 安徽大学 Nitrogen-doped gamma-Bi2MoO6Method for preparing photocatalyst

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Application publication date: 20120711