CN104209118A - Method for preparing bismuth hydroxide/bismuth tungstate compound photo-catalyst by heating one-pot solvent - Google Patents

Method for preparing bismuth hydroxide/bismuth tungstate compound photo-catalyst by heating one-pot solvent Download PDF

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CN104209118A
CN104209118A CN201410496161.4A CN201410496161A CN104209118A CN 104209118 A CN104209118 A CN 104209118A CN 201410496161 A CN201410496161 A CN 201410496161A CN 104209118 A CN104209118 A CN 104209118A
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张国英
崔燕
杨立民
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Tianjin Normal University
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Abstract

The invention discloses a method for preparing a bismuth hydroxide/bismuth tungstate compound photo-catalyst by heating an one-pot solvent. A novel Bi(OH)3/Bi2WO6 visible responsive photo-catalyst is prepared by taking ethanol and water as a mixed solvent, heating the one-pot solvent, and only excessively using and dissolving one bismuth source Bi (NO3)3.5H2O. The photocatalytic activity of the product is systematically researched under the impact of ethanol content, reaction temperature and time, Bi(OH)3 compound content and other experiment parameters, and the optimal conditions for preparing Bi (OH)3)/Bi2WO6 include alcohol-water volume ratio of 9 : 8, solvent hot temperature of 200 degrees centigrade, reaction time of 6 hours, and Bi (OH)3) compound mole ratio of 0.3. The preparation method has the characteristics of simpleness, low cost and energy saving, the prepared compound photo-catalyst has the excellent photocatalytic performance, thereby solving the problem that the present pure bismuth tungstate is relatively weak in catalytic performance and restricted in actual application.

Description

One pot of solvent-thermal method is adopted to prepare the method for bismuth hydroxide/bismuth tungstate composite photocatalyst
The application obtains Tianjin innovation team of institution of higher education training plan and subsidizes (TD12-5038).
technical field
The invention belongs to environmental protection technical field, relate to a kind of preparation method of high-performance optical catalyst, be specifically related to a kind of employing one pot of solvent-thermal method and prepare bismuth hydroxide/bismuth tungstate Bi (OH) 3/ Bi 2wO 6the method of composite photo-catalyst.
background technology
Environmental pollution and energy shortage are 21st century two great difficult problems facing of human survival.Photocatalysis oxidation technique, because of its deep oxidation, non-secondary pollution and can directly utilize solar energy to drive the feature such as reaction as light source, shows huge application prospect, and therefore becomes one of study hotspot in recent years in environmental pollution improvement.Exploitation has the technological core that efficient sunlight responsive photocatalyst has become photocatalysis field.
Bi 2wO 6be a kind of novel photocatalyst be found in recent years, its band-gap energy is about 2.69 eV, can respond the visible ray of 400-460 nm, and due to Bi 2wO 6by WO in structure 6octahedral layer and Bi 2o 2the Lamellar character that layer alternately forms, makes it easily form the 3D superstructure assembled by nanometer sheet, can provide more property sites, have again and better reclaim cyclicity, thus in the depollution of environment, show potential using value for light-catalyzed reaction.
Although Bi 2wO 6than traditional photochemical catalyst TiO 2more can utilize solar energy, but be subject to the restriction of its Intrinsic Gettering threshold value (460nm), still there is the following bottleneck problem limiting its practical application in pure bismuth tungstate photocatalyst; One is narrower to the absorption region of visible ray, and two is that photo-generated carrier recombination rate is very fast.Constructing heterojunction structure is one of approach effectively solved the problem.Overlap effect of being with between semiconductor can impel absorbing wavelength red shift, thus widens photoresponse scope; In addition, the space potential produced between hetero-junctions is poor, and photo-generated carrier can be impelled irreversible migration to occur in internal electric field and is separated, thus improves photo-quantum efficiency.As the TiO that reports 2/ Bi 2wO 6, Bi 2o 3/ Bi 2wO 6certain collaborative catalytic effect altogether is all shown etc. system.The hetero-junctions constructing foreign peoples needs to use more complicated flow process usually, as multistep processes preparation, sol-gel process, microwave assisting method etc.From economize energy, simplify the practical standpoint of preparation technology, explore and a kind ofly prepare simple, with low cost and the NEW TYPE OF COMPOSITE photochemical catalyst with greater efficiency has important theoretical and practical significance.
The present invention, from point of view of practicability, considers above-mentioned factor, and the ingenious facile hydrolysis characteristic utilizing Bi source, only uses a kind of bismuth source and make it excessive, obtains Bi (OH) with one pot of solvent-thermal method 3the Bi of compound 2wO 6heterogeneous photochemical catalyst.Measure than prepared pure Bi with Bi, W etc. 2wO 6compare, the activity of composite photo-catalyst significantly improves.Current alkaloids is to Bi 2wO 6compound there is not been reported, and the present invention has that technique simplifies, product cost is low, performance is high, recyclability is strong etc. advantage, effectively can solve Bi 2wO 6the bottleneck problem that photochemical catalyst is faced in actual applications.
Summary of the invention
For achieving the above object, the invention discloses a kind of employing one pot of solvent-thermal method and prepare bismuth hydroxide/bismuth tungstate Bi (OH) 3/ Bi 2wO 6the method of composite photo-catalyst, it is characterized in that carrying out as follows:
Step 1: take a certain amount of Na 2wO 42H 2o is the storing solution A of 0.13mol/L with distilled water compound concentration;
Step 2: take a certain amount of Bi (NO 3) 35H 2o, adds the precursor liquid B of distilled water preparation variable concentrations, wherein Bi (NO 3) 35H 2o:H 2the ratio of quality and the number of copies 28-165:1 of O; Preferred mass portion rate is 120-160:1.
Step 3: get a certain amount of A storing solution and drip in above-mentioned B precursor liquid, magnetic agitation 30min, adds a certain amount of solvent wherein, and gained suspension is transferred to hydrothermal reaction kettle, in 160-200 DEG C of reaction 6-12h;
Step 4: after being cooled to room temperature, product is centrifugal, washing also drying, obtains the Bi (OH) of serial different mol ratio 3/ Bi 2wO 6composite photo-catalyst; Described solvent is the mixed solvent of second alcohol and water, and wherein the volume ratio of second alcohol and water is 0.05-1.85:1; Described Bi (NO 3) 35H 2o:Na 2wO 42H 2o mol ratio is 2-2.5:1, and the scope of bismuth source excess percentage is 0-25%; It has the shape characteristic of the lamella package assembly shown in diffracting spectrum characteristic sum accompanying drawing 2 shown in Figure of description 1.
The present invention is characterized in: only use a kind of bismuth source Bi (NO 3) 35H 2o, the excessive and obtained Bi (OH) of hydrolysis by it 3the Bi of compound 2wO 6photochemical catalyst.
Employing of the present invention one pot of solvent-thermal method prepares Bi (OH) 3/ Bi 2wO 6the method of composite photo-catalyst, wherein Bi (OH) 3and Bi 2wO 6mol ratio is in the scope of 0.1-0.5:1.
Employing of the present invention one pot of solvent-thermal method prepares Bi (OH) 3/ Bi 2wO 6the method of composite photo-catalyst, wherein Bi (OH) 3and Bi 2wO 6(optimization) mol ratio is 0.3.
The more detailed preparation method of the present invention is as follows:
One for mixed solvent, by simple one pot of solvent-thermal method, is only using a kind of bismuth source Bi (NO with second alcohol and water 3) 35H 2o, makes it excessive and under the condition of thoroughly hydrolysis, prepares Bi (OH) 3/ Bi 2wO 6the method of composite photo-catalyst.
First take a certain amount of Na 2wO 42H 2o, in small beaker, adds distilled water and is stirred to abundant dissolving, and obtained concentration is the Na of 0.13mol/L 2wO 42H 2o storing solution; Then a certain amount of Bi (NO is directly taken 3) 35H 2o, in polytetrafluoroethyllining lining, adds distilled water and magnetic agitation, the Bi (NO of obtained variable concentrations 3) 35H 2o precursor liquid, wherein Bi (NO 3) 35H 2the mass ratio of O and distilled water is 28-165:1, and preferred mass portion rate is 120-160:1.
Get a certain amount of above-mentioned Na 2wO 42H 2o storing solution drips in Bi (NO 3) 35H 2in O precursor liquid, about magnetic agitation 30min, then add a certain amount of absolute ethyl alcohol wherein, continue to stir 10min, then gained mixed liquor is carried out solvent thermal reaction at a certain temperature.Naturally cool to after room temperature until hydrothermal reaction kettle, product centrifugation, washing is also dry, obtain serial Bi (OH) 3/ Bi 2wO 6composite photo-catalyst.
It should be noted that: Bi (OH) 3be generate in the process of this solvent heat, it is not raw material, but product.If the consumption in Bi source and W source just for wait measure ratio, i.e. Bi (NO 3) 35H 2o:Na 2wO 42H 2o mol ratio is 2:1, then that obtain is pure Bi 2wO 6, and in our method, employing adds excessive Bi source, like this except generating Bi 2wO 6outward, unnecessary Bi source then forms Bi (OH) by being thoroughly hydrolyzed in experimentation 3.Thus end product is Bi (OH) 3/ Bi 2wO 6composite photo-catalyst.
Present system explores the experiment parameters such as volume ratio of alcohol to water, reaction temperature, reaction time, Bi source consumption to the impact of product photocatalysis performance.Wherein under fixing solvent total amount is the prerequisite of 17mL, ethanol consumption interval is 1-11ml, and namely volume ratio of alcohol to water is 0.0625-1.85:1; Range of reaction temperature is 160-200 DEG C, and the reaction time is 6-12h, regulates Bi source consumption to make Bi (OH) 3and Bi 2wO 6mol ratio be 0-0.5:1.By the adjustment of above-mentioned serial reaction parameter, obtained serial composite photo-catalyst, by the contrast to its photocatalysis performance, determines preparation high-performance Bi (OH) 3/ Bi 2wO 6the optimum condition of composite photo-catalyst is: volume ratio of alcohol to water example is 1.13:1, and reaction temperature is 200 DEG C, reaction time 6h, Bi (OH) 3and Bi 2wO 6mol ratio be 0.3:1.
Employing disclosed by the invention one pot of solvent-thermal method prepares Bi (OH) 3/ Bi 2wO 6the method of composite photo-catalyst, compared with prior art had good effect is:
(1) Bi (OH) 3to Bi 2wO 6the heterogeneous photochemical catalyst carrying out compound has not yet to see report;
(2) adopt preparation method to be one pot of hot method of alcohol-water mixed solvent, with preparation pure Bi 2wO 6raw material used is identical, just excessive by ingehious design Bi source, and makes its thoroughly hydrolysis generation Bi (OH) in course of reaction 3, thus obtain Bi (OH) 3/ Bi 2wO 6composite photo-catalyst.Preparation process simple economy, is easy to amplify and produces.
(3) this Bi (OH) 3/ Bi 2wO 6compound system is compared to the pure Bi under equal conditions 2wO 6, photocatalytic activity significantly improves, and pseudo-first order reaction kinetics constant even improves nearly 28 times, thus has broad application prospects in sewage disposal.
The present invention further discloses Bi (OH) 3/ Bi 2wO 6the application of composite photo-catalyst in degraded industrial wastewater, industrial wastewater wherein mainly refers to the waste water that papermaking or printing and dyeing industry produce.The waste water that papermaking produces refers to the refractory organics aromatic compounds contained in paper machine room institute sewer; The waste water that printing and dyeing industry produces refers to the soluble azo dyes with carcinogenicity conventional in printing and dyeing industry.
Accompanying drawing illustrates:
As follows to the structure of gained part photocatalyst, pattern and performance characterization result:
Fig. 1 is the XRD figure of prepared photochemical catalyst;
Fig. 1 is Bi prepared by alcohol water mixed solvent heat 2wO 6, Bi (OH) 3and Bi (OH) 3/ Bi 2wO 6the XRD powder diagram of-0.3 composite photo-catalyst; As shown in uppermost diffraction pattern, than gained sample under condition, there is strong and sharp-pointed diffraction maximum in meterings such as Bi, W, show that degree of crystallinity is higher, diffraction pattern and standard card (JCPDS No. 73-1126) fit like a glove, and show that it is the pure Bi of orthorhombic crystal phase 2wO 6; And under the condition only having Bi source, as shown in least significant end collection of illustrative plates, sample also has good degree of crystallinity, and Bi (OH) can be attributed to 3crystalline phase (JCPDS No.001-0898); Exist in Bi, W source, and under the condition in Bi source excessive 15%, gained sample has obvious multiphase feature, is Bi simultaneously 2wO 6with Bi (OH) 3compound; Prove in this solvent heat process, excessive by suitable Bi source, Bi (OH) can be obtained 3/ Bi 2wO 6composite photo-catalyst;
Fig. 2 is scanning electron microscope (SEM) photograph (a-b) Bi of photochemical catalyst 2wO 6; (c-d) Bi (OH) 3/ Bi 2wO 6-0.3;
Fig. 2 is prepared Bi under optimal conditions 2wO 6and Bi (OH) 3/ Bi 2wO 6the scanning electron microscope (SEM) photograph of-0.3 composite photo-catalyst.The pattern of composite photo-catalyst and Bi as seen from the figure 2wO 6matrix sample has obvious difference; Wherein:
A is pure Bi 2wO 6sEM image, it is the octahedron assembled by nanometer sheet, size about about 2 μm, grows complete and good dispersion; B is high magnification SEM image, shows that its lamella is thicker, about 30-50nm.
As shown in c-d, when introducing Bi (OH) in system 3after, the pattern of gained composite photo-catalyst has with it obvious difference; Octahedral structure disappears substantially, and the substitute is the irregular assembling of two-dimentional lamella, and its lamella is obviously thinning, under high power SEM, even can observe part translucent thin slice, lamellar spacing is about 10nm, has embrittlement phenomenon to exist.Compared to octahedral structure, the irregular assembling of this nanometer sheet can be the pore passage structure that light-catalyzed reaction provides abundanter; In addition, this superthin structure can shorten the transmission range of carrier greatly, thus improves photocatalytic activity;
Fig. 3 is serial Bi (OH) 3/ Bi 2wO 6the Performance comparision of photochemical catalyst; Wherein (a) is the efficiency of photocatalytic degradation RhB, and (b) is pseudo first order reaction speed constant;
Fig. 3 is serial different B i (OH) obtained under optimal conditions 3the photocatalysis performance of content sample.Photocatalysis condition is: 500W Xe lamp (attached 420nm filter plate) is light source, and it is 10 that 5mg photochemical catalyst is scattered in 10ml concentration -5the RhB dye solution of mol/L, interval 15min samples; Obviously, compared to pure Bi 2wO 6system, all Bi (OH) 3/ Bi 2wO 6photochemical catalyst all shows the photocatalytic degradation efficiency significantly improved, after illumination 60min all composite photo-catalysts all can by least 95% dye decolored, and pure Bi 2wO 6only 22.7% is reached to the degradation efficiency of RhB; And being increased to 0.3 from 0.1 along with compound content, photocatalytic activity also increases gradually, wherein Bi (OH) 3/ Bi 2wO 6-0.3 shows optimal light catalytic performance; Compound content continues to raise, and the Carrier recombination caused by excessive grain boundary defects makes catalytic activity in a slight decrease again on the contrary; The pseudo-first order reaction kinetics constant of Fig. 3 b also show this trend, and wherein mol ratio is the composite photo-catalyst of 0.3, and its speed constant is up to pure Bi 2wO 6nearly 28 times; Obvious Bi (OH) 3with Bi 2wO 6between there is good synergy, its introducing significantly improves Bi 2wO 6photocatalytic activity.
detailed description of the invention:
In order to explain the present invention further, provide following preparation method's embodiment.The statement of following examples does not limit the present invention, and one of skill in the art can make improvements according to spirit of the present invention and change, and these described improvement and change all should be considered as within the scope of the invention.Various raw material of the present invention such as Na 2wO 42H 2o, Bi (NO 3) 35H 2o all has commercially available.
Embodiment 1
Take 0.40mmol Na 2wO 42H 2o, adds 3.0ml distilled water and is stirred to abundant dissolving; Take 0.84mmol Bi (NO 3) 35H 2o, in 25ml polytetrafluoroethylene (PTFE) inner liner of reaction kettle, adds 5ml distilled water magnetic agitation 15min, by Na 2wO 42H 2o solution drips in reactor, continues magnetic agitation 30min, then drips 9.0ml absolute ethyl alcohol, to stir this suspension after 10min in 200 DEG C of solvent thermal reaction 6h.To be cooled to room temperature, product centrifugation, washing is also dry, obtain Bi (OH) 3/ Bi 2wO 6-0.1 photochemical catalyst sample.By adjustment Bi (NO 3) 35H 2o consumption, repeats aforesaid operations, can obtain the Bi (OH) of different composite ratio 3/ Bi 2wO 6composite photo-catalyst, performance is described by accompanying drawing 3.As above explain, Bi (OH) 3being product, is not reactant, just adds excessive Bi (NO simultaneously 3) 35H 2o, and Bi (OH) is obtained by hydrolysis in course of reaction 3.
Embodiment 2
Take 0.40mmol Na 2wO 42H 2o, adds 3ml distilled water and is stirred to abundant dissolving; Take 0.92mmol Bi (NO 3) 35H 2o, in the polytetrafluoroethylene (PTFE) inner liner of reaction kettle of 25ml, adds 11ml distilled water magnetic agitation 15min, by Na 2wO 42H 2o solution drips in reactor, continues magnetic agitation 30min, drips 3.0ml absolute ethyl alcohol, to stir this white suspension after 10min in 180 DEG C of solvent thermal reaction 6h.To be cooled to room temperature, product centrifugation, washing is also dry, and obtaining volume ratio of alcohol to water is 3:14, Bi (OH) 3/ Bi 2wO 6the faint yellow photocatalyst powder of-0.3.By adjustment ethanol content, repeat aforesaid operations, the Bi (OH) of serial different ethanol content can be obtained 3mol ratio is the Bi (OH) of 0.3 3/ Bi 2wO 6composite photo-catalyst.
Table 1 Bi (OH) 3/ Bi 2wO 6-0.3, the photocatalysis performance of different ethanol content series of samples
Photocatalysis performance after this series of samples radiation of visible light 40min is as shown in table 1, result shows that ethanol consumption is one of important parameter affecting composite photo-catalyst performance, when volume ratio of alcohol to water is 9:8, when namely alcohol volume content is 52.9%, photocatalytic activity is optimum.
Embodiment 3
Take 0.40mmol Na 2wO 42H 2o, adds 3ml distilled water and is stirred to abundant dissolving; Take 0.88mmol Bi (NO 3) 35H 2o, in the polytetrafluoroethylene (PTFE) inner liner of reaction kettle of 25ml, adds 5ml distilled water magnetic agitation 15min, by Na 2wO 42H 2o solution drips in reactor, continues magnetic agitation 30min, then drips 9ml absolute ethyl alcohol, to stir this white suspension after 10min in 160 DEG C of solvent thermal reaction 12h.To be cooled to room temperature, product centrifugation, washing is also dry, and mol ratio is the Bi (OH) of 0.2 3/ Bi 2wO 6photochemical catalyst sample.Be 160 DEG C, 180 DEG C, 200 DEG C by set temperature, and adjust Bi (NO 3) 35H 2the consumption of O, repeats aforesaid operations, can obtain the Bi (OH) of different mol ratio example under serial differential responses temperature conditions 3/ Bi 2wO 6composite photo-catalyst.
The sample prepared under the different hydrothermal temperature of table 2 contrasts the degradation efficiency of RhB dyestuff
Illustrate: Bi (OH) 3/ Bi 2wO 6bOH/BWO is abbreviated as in upper table.
Photocatalysis performance after this series of samples radiation of visible light 30min is as shown in table 2, and result shows that reaction temperature is another key factor affecting photocatalysis performance, and the photocatalytic activity of composite sample is all obviously better than Bi 2wO 6, and the sample of same compositely proportional, photocatalytic activity presents the trend of enhancing with the rising of reaction temperature, when 200 DEG C, performance is best.
Embodiment 4
Take 0.40mmol Na 2wO 42H 2o, adds 3ml distilled water and is stirred to abundant dissolving; Take 1.0 mmol Bi (NO 3) 35H 2o, in the polytetrafluoroethylene (PTFE) inner liner of reaction kettle of 25ml, adds 5ml distilled water magnetic agitation 15min, by Na 2wO 42H 2o solution drips in reactor, continues magnetic agitation 30min, then drips 9ml absolute ethyl alcohol, after stirring 10min, white suspension is reacted 6h in 200 DEG C.To be cooled to room temperature, by product centrifugation, washing dry, can obtain the reaction time be 6h, mol ratio be 0.5 Bi (OH) 3/ Bi 2wO 6photochemical catalyst.By arranging the differential responses time, repeating aforesaid operations, the Bi (OH) of series through differential responses time gained can be obtained 3/ Bi 2wO 6photochemical catalyst.
Bi (OH) prepared by the table 3 differential responses time 3/ Bi 2wO 6the photocatalytic degradation efficiency of-0.3 couple of RhB
The RhB degradation efficiency contrast of differential responses time sample visible light exposure 30min is as shown in table 3, reaction time is also the important experiment parameter affecting composite photo-catalyst performance, wherein the sample of solvent thermal reaction 6h and 12h all has high photocatalytic degradation efficiency, but the properties of sample of 6h is obviously higher, its degradation efficiency about 99%, the reaction time shorter is in addition conducive to economize energy.Therefore preferably 6h is optimum reacting time.

Claims (5)

1. one kind adopts one pot of solvent-thermal method to prepare Bi (OH) 3/ Bi 2wO 6the method of composite photo-catalyst, is characterized in that carrying out as follows:
Step 1: take a certain amount of Na 2wO 42H 2o is the Na of 0.13mol/L with distilled water compound concentration 2wO 42H 2o storing solution A;
Step 2: take a certain amount of Bi (NO 3) 35H 2o, adds the precursor liquid B of distilled water preparation variable concentrations, wherein Bi (NO 3) 35H 2o:H 2the ratio of quality and the number of copies of O is 28-165:1;
Step 3: get a certain amount of A storing solution and drip in above-mentioned B precursor liquid, magnetic agitation 30min, adds a certain amount of solvent wherein, and gained suspension is transferred to hydrothermal reaction kettle, in 160-200 DEG C, reaction 6-12h;
Step 4: after being cooled to room temperature, product is centrifugal, washing also drying, obtains the Bi (OH) of serial different mol ratio 3/ Bi 2wO 6composite photo-catalyst; Described solvent is the mixed solvent of second alcohol and water, and wherein the volume ratio of second alcohol and water is 0.05-1.85:1; Described Bi (NO 3) 35H 2o:Na 2wO 42H 2o mol ratio is 2-2.5:1, and the scope of bismuth source excess percentage is 0-25%; It has the shape characteristic of the lamella package assembly shown in diffracting spectrum characteristic sum accompanying drawing 2 shown in Figure of description 1.
2. described in claim 1, adopt one pot of solvent-thermal method to prepare Bi (OH) 3/ Bi 2wO 6the method of composite photo-catalyst, is characterized in that, volume ratio of alcohol to water example is 1.13:1, and reaction temperature is 200 DEG C, reaction time 6h.
3. described in claim 1, adopt one pot of solvent-thermal method to prepare Bi (OH) 3/ Bi 2wO 6the method of composite photo-catalyst, is characterized in that, only uses a kind of bismuth source Bi (NO 3) 35H 2o, the excessive and obtained Bi (OH) of hydrolysis by it 3the Bi of compound 2wO 6photochemical catalyst.
4. described in claim 2, adopt one pot of solvent-thermal method to prepare Bi (OH) 3/ Bi 2wO 6the method of composite photo-catalyst, wherein Bi (OH) 3and Bi 2wO 6mol ratio is in the scope of 0.1-0.5:1.
5. described in claim 3, adopt one pot of solvent-thermal method to prepare Bi (OH) 3/ Bi 2wO 6the method of composite photo-catalyst, wherein Bi (OH) 3and Bi 2wO 6mol ratio be 0.3.
CN201410496161.4A 2014-09-25 2014-09-25 Use the method that one pot of solvent-thermal method prepares bismuth hydroxide/bismuth tungstate composite photocatalyst Expired - Fee Related CN104209118B (en)

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CN110841626A (en) * 2019-10-24 2020-02-28 江苏大学 Tungsten oxide/bismuth oxide net-sheet composite material and preparation method and application thereof
CN112604679A (en) * 2020-12-30 2021-04-06 上海纳米技术及应用国家工程研究中心有限公司 Preparation method, product and application of oxygen-deficient bismuth tungstate nanobelt photocatalytic material

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