CN104587999A - Preparation method of porous Bi2WO6 nanosheet photocatalytic material - Google Patents
Preparation method of porous Bi2WO6 nanosheet photocatalytic material Download PDFInfo
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- CN104587999A CN104587999A CN201510017455.9A CN201510017455A CN104587999A CN 104587999 A CN104587999 A CN 104587999A CN 201510017455 A CN201510017455 A CN 201510017455A CN 104587999 A CN104587999 A CN 104587999A
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Abstract
The invention relates to a preparation method of a porous Bi2WO6 nanosheet photocatalytic material. The preparation method sequentially comprises the following steps: tiling Bi(NO3)3 solid powder evenly on the bottom of a flask; adding a Na2WO4 solution slowing into the flask slowly along the wall of the flask, carrying out constant-temperature standing reaction, filtering the obtained precipitate, washing and drying so as to obtain a pore-free amorphous Bi2WO6 nanosheet; and carrying out thermal treatment at high temperature of 200-800 DEG C for 0.5-5 hours, thereby obtaining the porous Bi2WO6 nanosheet photocatalytic material. The preparation method has the beneficial effects that the preparation is a rapid, economical and environment-friendly synthetic method of the porous Bi2WO6 nanosheet photocatalytic material; the porous Bi2WO6 nanosheet photocatalytic material synthesized by the method has relatively high specific surface area, so that Bi2WO6 shows high photocatalytic performance.
Description
Technical field
The present invention relates to the technical field of porous material and sheetlike material, particularly relate to porous Bi
2wO
6the preparation method of nanosheet photocatalytic material.
Technical background
Because global problem of environmental pollution is day by day serious, catalysis material is used to have vast potential for future development in degradable organic pollutant.As everyone knows, the energy gap of bismuth tungstate is about 2.7eV, and there is very strong absorption the sunshine visible region being greater than 420nm at wavelength, and light-catalyzed reaction can occur.Bismuth tungstate after the irradiation being subject to visible ray, absorb photons energy and excite and create light induced electron and hole, and and then produce active oxygen and hydroxyl radical free radical etc., have very strong oxidability, they can make majority of organic pollutants oxidation decomposition.Therefore, on solution problem of environmental pollution, good effect can be played.On this basis, nano material is due to quantum size effect, and the band gap of nano particle increases along with the reduction of particle size, causes it to have stronger photo-catalysis capability.In addition, again because porous material has the advantages such as density is low, quality is little, specific area is large, there is the Bi of loose structure
2wO
6nanosheet photocatalytic material will have great advantage in light-catalysed performance.At present, the synthetic method of porous material mainly contains hard template method and soft template method.But template normally removes non-material component and pore-creating by calcination or chemical extraction, its complicated operation, and in the process removed at non-material component, easily cause the destruction to material structure.Therefore, simple and easy, the green Bi without Template synthesis with loose structure and nanoscale is adopted
2wO
6become an important research direction.
The current micro-structural study on regulation about bismuth tungstate catalysis material mainly concentrates on the research in nano particle, laminated structure and spherical structure etc.As far as we know, also do not use without Template synthesis porous Bi at present
2wO
6nanosheet photocatalytic material, to improve the relevant report of its photocatalysis performance.
Summary of the invention
Technical problem to be solved by this invention is for above-mentioned prior art, proposes a kind of porous Bi
2wO
6the preparation method of nanosheet photocatalytic material: under the prerequisite not using any template and pore creating material, by WO in regulation and control solution
4 2-ion is at solid Bi (NO
3)
3the reaction rate on surface, to prepare Bi
2wO
6nanometer sheet presoma; Again by controlling heat treatment temperature to obtain the Bi with loose structure
2wO
6nanosheet photocatalytic material.
The present invention solves the problems of the technologies described above adopted technical scheme: porous Bi
2wO
6the preparation method of nanosheet photocatalytic material, includes next coming in order step:
1) by Na
2wO
4be dissolved in distilled water and form homogeneous solution, wherein Na
2wO
4solubility is 0.005-0.50mol/L;
2) by Bi (NO
3)
3pressed powder is evenly laid in beaker bottom, then by step 1) the 50mL Na of gained
2wO
4solution slowly joins in beaker along walls of beaker, and wherein the mol ratio of Bi and W is 1:0.25-1:6, leaves standstill reaction 1-72h in 25-90 DEG C of constant temperature, gained sediment after filtration, washing and dry, obtain the amorphous Bi of atresia
2wO
6nanometer sheet;
3) by step 2) the amorphous Bi of atresia that obtains
2wO
6nanometer sheet is placed in 200-800 DEG C of high-temperature heat treatment 0.5-5h, namely obtains porous Bi
2wO
6nanosheet photocatalytic material.
By such scheme, step 1) described in Na
2wO
4concentration is 0.03-0.30mol/L.
By such scheme, step 2) described in standing reaction temperature be 25-60 DEG C, the reaction time is 24-48h.
By such scheme, step 2) described in the mol ratio of Bi and W be 1:1-1:3.
By such scheme, step 3) described in high-temperature heat treatment temperature be 350-600 DEG C, the high-temperature heat treatment time is 1-3h.
The present invention proposes without under template action, first with solid Bi (NO
3)
3and Na
2wO
4the standing self-assembling reaction of solution, by WO in regulation and control solution
4 2-ion is at solid Bi (NO
3)
3the reaction rate on surface, generates Bi
2wO
6nanometer sheet presoma, then by controlling the heat treatment temperature of presoma, to obtain the Bi with loose structure
2wO
6nanometer sheet, the general principle of its synthesis is:
2Bi(NO
3)
3(s)+WO
4 2-(aq)+2H
2O(l)→Bi
2WO
6(s)+4H
+(aq)+6NO
3 -(aq)
Porous Bi
2wO
6the photocatalytic activity of nanosheet photocatalytic material is characterized by Photocatalytic Degradation of Phenol solution under ultraviolet light.Experimentation is as follows: by 0.10g porous Bi
2wO
6nanosheet photocatalytic material is dispersed in and 10mL phenol solution (20mgL is housed
-1) reaction bulb in, reaction bulb is positioned over dark place 2h to reach catalyst and the intermolecular adsorption-desorption of phenol balances.At ambient temperature, irradiate with the ultraviolet LED light source (wavelength: UV-365nm) that power is 4W, measure the phenol concentration in solution every 5min.In degradation solution, the concentration of phenol is measured by ultraviolet-visible absorption spectroscopy instrument (UVmini 1240, Japan).
Porous Bi
2wO
6the Characterization for Microstructure method of nanosheet photocatalytic material: observe pattern and granular size with field emission scanning electron microscope (FESEM), by X-ray diffraction (XRD) spectrum analysis crystallization situation, pore structure and the crystal structure of material is observed, by the light absorption situation of UV-vis analysis of material with transmission electron microscope (TEM).
Beneficial effect of the present invention is: employing of the present invention is without Template synthesis porous Bi
2wO
6nanosheet photocatalytic material, without the need to adding any template or other additives, building-up process has simple and easy, environmental protection, the advantage such as pollution-free, is a kind of quick, economic, green porous Bi
2wO
6the synthetic method of nanosheet photocatalytic material.By the porous Bi that this method is synthesized
2wO
6nanosheet photocatalytic material has larger specific area, thus makes Bi
2wO
6show high photocatalysis performance.The present invention has that operation is very simple, equipment requirement is low, without the need to costliness various reaction units, be easy to the advantages such as synthesis in enormous quantities, be expected to the Social and economic benef@that generation is good.
Accompanying drawing explanation
Fig. 1 is porous Bi in embodiment 1
2wO
6the FESEM figure of nanometer sheet;
Fig. 2 is porous Bi in embodiment 1
2wO
6the XRD collection of illustrative plates of nanometer sheet:
Fig. 3 is porous Bi in embodiment 1
2wO
6the TEM figure of nanometer sheet;
Fig. 4 is porous Bi in embodiment 1
2wO
6the UV-vis collection of illustrative plates of nanometer sheet:
Fig. 5 is porous Bi in embodiment 1
2wO
6the degradation rate constant k:(a of nanometer sheet Pyrogentisinic Acid) Bi
2wO
6; (b) Pt/Bi
2wO
6
Fig. 6 is the Bi without high-temperature heat treatment in embodiment 1
2wO
6the FESEM figure of nanometer sheet;
Fig. 7 is the Bi without high-temperature heat treatment in embodiment 1
2wO
6the XRD collection of illustrative plates of nanometer sheet.
Detailed description of the invention
Below in conjunction with embodiment, the present invention will be further described in detail, but this explanation can not be construed as limiting the invention.
Embodiment 1:
Porous Bi
2wO
6the building-up process of nanosheet photocatalytic material is as follows: 1) by Na
2wO
4be dissolved in distilled water and form homogeneous solution, wherein Na
2wO
4solubility is 0.125mol/L; 2) by Bi (NO
3)
3pressed powder is evenly laid in beaker bottom, then by step 1) the 50mL Na of gained
2wO
4solution slowly joins in beaker along walls of beaker, and wherein the mol ratio of Bi and W is 1:3, leaves standstill reaction 48h in 25 DEG C of constant temperature, gained sediment after filtration, washing and dry, obtain the amorphous Bi of atresia
2wO
6nanometer sheet; 3) by step 2) the amorphous Bi of atresia that obtains
2wO
6nanometer sheet is placed in 500 DEG C of high-temperature heat treatment 2h, namely obtains porous Bi
2wO
6nanosheet photocatalytic material.
Fig. 1 is porous Bi
2wO
6the FESEM figure of nanosheet photocatalytic material.Can find out that prepared sample exists with loose aggregation from Figure 1A and Figure 1B, and present obvious porous laminated structure.As can be seen from Fig. 1 C and 1D, each Bi
2wO
6nanometer sheet is made up of many nano particles, and its particle size is 30-100nm; Meanwhile, Bi
2wO
6there is many less holes between nano particle, its aperture is 20-80nm.
Fig. 2 is porous Bi
2wO
6the XRD spectra of nanosheet photocatalytic material.Result shows: each diffraction maximum position and standard Bi
2wO
6result consistent, the sample prepared by proving is Bi
2wO
6material; Meanwhile, each diffraction peak-to-peak is strong narrower, and porous Bi is described
2wO
6the degree of crystallinity of nanometer sheet is higher, and grain size is less.
Fig. 3 is porous Bi
2wO
6the TEM figure of nanosheet photocatalytic material.Can be more clearly visible prepared sample from Fig. 3 A, 3B and 3C is the sheet Bi with loose structure
2wO
6material, the size of pore structure is consistent with the result of FESEM.Fig. 3 D is sheet Bi
2wO
6between nano particle, the high-resolution TEM at interface schemes, and shows Bi
2wO
6between the particle of nanometer sheet, there is good combination.
Fig. 4 is porous Bi
2wO
6the UV-vis collection of illustrative plates of nanosheet photocatalytic material.As can be seen from the figure, porous Bi
2wO
6nanometer sheet has good absorbent properties at visible region, and Absorbable rod wavelength reaches the visible ray of 500nm, proves to can be used as a kind of visible-light photocatalysis material.
Fig. 5 is porous Bi
2wO
6the degradation rate constant of nanosheet photocatalytic material Pyrogentisinic Acid solution.As can be seen from the figure, without the porous Bi that Pt modifies
2wO
6nanometer sheet Pyrogentisinic Acid does not almost have degradation property, and after Pt modifies, porous Bi
2wO
6nanosheet photocatalytic material demonstrates obvious Photocatalytic Degradation Property, and its speed constant is 0.0074min
-1.According to previous karyotype studies, Bi
2wO
6the conduction level of material is about+0.3V, makes its light induced electron effectively can not reduce oxygen, so almost do not have the performance of Photocatalytic Degradation of Phenol; And Pt metal can be used as effective auxiliary agent of catalysis material, effectively Bi can be made
2wO
6conduction band electron is quickly transferred on Pt, and then by polyelectron hydrogen reduction path restore oxygen, thus show high photocatalysis performance.
Fig. 6 is the Bi without high-temperature heat treatment
2wO
6the FESEM figure of nanometer sheet presoma.Fig. 6 A and Fig. 6 B shows, without the Bi of high-temperature heat treatment
2wO
6though nanometer sheet presoma has flaky nanometer structure, but does not have pore structure, show Bi
2wO
6laminated structure by solid Bi (NO
3)
3with Na
2wO
4between self-assembling reaction obtain, and the loose structure in nanometer sheet is formed by the high-temperature heat treatment in later stage.
Fig. 7 is the Bi without high-temperature heat treatment
2wO
6the XRD collection of illustrative plates of nanometer sheet presoma.With Fig. 2 contrast, the Bi without high-temperature heat treatment can be found out
2wO
6nanometer sheet degree of crystallinity is very low, is substantially in amorphous state, and thus the high-temperature heat treatment process in later stage both ensure that Bi
2wO
6crystallization, cause again effective formation of loose structure.
Embodiment 2:
In order to check Na
2wO
4concentration is to porous Bi
2wO
6the impact of nanosheet photocatalytic material structure, except Na
2wO
4beyond concentration, other reaction conditions are as follows: the mol ratio (1:3), high-temperature heat treatment temperature (500 DEG C), high-temperature heat treatment time (2h) etc. of reaction temperature (25 DEG C), reaction time (48h), Bi and W are all identical with embodiment 1.Result shows, works as Na
2wO
4when concentration is 0.005mol/L, due to WO in system
4 2-concentration is too low, Bi
2wO
6self assembly speed is less, causes its laminated structure not obvious.Work as Na
2wO
4when concentration is between 0.03-0.30mol/L, thinner thickness, Bi that area is larger can be obtained
2wO
6presoma.Work as Na
2wO
4when concentration is 0.50mol/L, due to WO
4 2-excessive concentration, Bi
2wO
6crystal growth rate is too fast, causes between each flat crystal mutually stacking, and sheet thickness increases, and its specific area is reduced.Therefore, at porous Bi
2wO
6in the building-up process of nanosheet photocatalytic material, Na
2wO
4the optimum range of concentration is 0.03-0.30mol/L.
Embodiment 3:
In order to check reaction temperature to porous Bi
2wO
6the impact of nanosheet photocatalytic material, in addition to the reaction temperature, other reaction conditions are as follows: Na
2wO
4the mol ratio (1:3), high-temperature heat treatment temperature (500 DEG C), high-temperature heat treatment time (2h) etc. of concentration (0.125mol/L), reaction time (48h), Bi and W are all identical with embodiment 1.Result shows, when reaction temperature is at 25-60 DEG C, self assembly speed is moderate, can obtain high-purity in the short period of time and the good Bi of lamellar structure
2wO
6nanometer sheet.When reaction temperature is at 90 DEG C, reaction rate is too fast, cause between each flat crystal mutually stacking, and thus sheet thickness also increases.Therefore, at porous Bi
2wO
6in the building-up process of nanosheet photocatalytic material, the optimum range of reaction temperature is 25-60 DEG C.
Embodiment 4:
In order to check the reaction time to porous Bi
2wO
6the impact of nanosheet photocatalytic material, except the reaction time, other reaction conditions are as follows: Na
2wO
4the mol ratio (1:3), high-temperature heat treatment temperature (500 DEG C), high-temperature heat treatment time (2h) etc. of concentration (0.125mol/L), reaction temperature (25 DEG C), Bi and W are all identical with embodiment 1.Result shows, when being 1h when reacted, and Na
2wO
4solution and Bi (NO
3)
3solid is completely incomplete, and with Bi (NO
3)
3the formation of hydrolysising by-product.When being when reacted 24-48h, raw material is able to abundant reaction, can obtain the Bi that purity is high, surface area is large
2wO
6nanometer sheet.When being when reacted 72h, the Bi of gained
2wO
6nanometer sheet completes already owing to reacting, and has no significant effect the structure of nanometer sheet, and time cost causes waste.Therefore, at porous Bi
2wO
6in the building-up process of nanosheet photocatalytic material, the optimum range in reaction time is 24-48h.
Embodiment 5:
In order to check the mol ratio of Bi and W to porous Bi
2wO
6the impact of nanosheet photocatalytic material, except the mol ratio of Bi and W, other reaction conditions are as follows: Na
2wO
4concentration (0.125mol/L), reaction temperature (25 DEG C), reaction time (48h), high-temperature heat treatment temperature (500 DEG C), high-temperature heat treatment time (2h) etc. are all identical with embodiment 1.Result shows, when the mol ratio of Bi and W is 1:0.25, and raw material Bi (NO
3)
3react insufficient, product purity is reduced and causes Bi (NO
3)
3wastage of material.When the mol ratio of Bi and W is 1:1-1:3, raw material reaction is abundant, and the Bi of gained
2wO
6nanometer sheet purity is high, pattern is better.When the mol ratio of Bi and W is 1:6, the Bi of gained
2wO
6nanometer sheet purity is not with WO
4 2-excessive and raise, and raw material Na can be caused
2wO
4waste.Therefore, at porous Bi
2wO
6in the building-up process of nanosheet photocatalytic material, the optimum range of Bi and W mol ratio is 1:1-1:3.
Embodiment 6:
In order to check high-temperature heat treatment temperature to porous Bi
2wO
6the impact of nanosheet photocatalytic material, except high-temperature heat treatment temperature, other reaction conditions are as follows: Na
2wO
4the mol ratio (1:3), high-temperature heat treatment time (2h) etc. of concentration (0.125mol/L), reaction temperature (25 DEG C), reaction time (48h), Bi and W are all identical with embodiment 1.Result shows, when high-temperature heat treatment temperature is 200 DEG C, and Bi
2wO
6crystal formation does not transform completely, and degree of crystallinity is lower, and pore structure is formed seldom simultaneously.When high-temperature heat treatment temperature is 350-600 DEG C, Bi
2wO
6nanometer sheet forerunner physical efficiency transforms into the more much higher hole Bi of degree of crystallinity
2wO
6nanometer sheet.When high-temperature heat treatment temperature is 800 DEG C, porous Bi
2wO
6the pore structure of nanometer sheet can be destroyed.Therefore, at porous Bi
2wO
6in the building-up process of nanosheet photocatalytic material, the optimum range of high-temperature heat treatment temperature is 350-600 DEG C.
Embodiment 7:
In order to check the high-temperature heat treatment time to porous Bi
2wO
6the impact of nanosheet photocatalytic material, except the high-temperature heat treatment time, other reaction conditions are as follows: Na
2wO
4the mol ratio (1:3), high-temperature heat treatment temperature (500 DEG C) etc. of concentration (0.125mol/L), reaction temperature (25 DEG C), reaction time (48h), Bi and W are all identical with embodiment 1.Result shows, when the high-temperature heat treatment time is 0.5h, and Bi
2wO
6nanometer sheet presoma causes degree of crystallinity to decline because the reaction time is insufficient, and pore structure is not obvious.When the high-temperature heat treatment time is 1-3h, Bi
2wO
6nanometer sheet presoma fully reacts, and degree of crystallinity is higher and pore structure is complete.When the high-temperature heat treatment time is 5h, Bi
2wO
6nanometer sheet presoma does not change with the prolongation of high-temperature heat treatment time, causes the consumption of the too much unnecessary energy, and causes the decline of preparation efficiency.Therefore, at porous Bi
2wO
6in the building-up process of nanosheet photocatalytic material, the optimum range of high-temperature heat treatment time is 1-3h.
Claims (5)
1. porous Bi
2wO
6the preparation method of nanosheet photocatalytic material, includes next coming in order step:
1) by Na
2wO
4be dissolved in distilled water and form homogeneous solution, wherein Na
2wO
4solubility is 0.005-0.50mol/L;
2) by Bi (NO
3)
3pressed powder is evenly laid in beaker bottom, then by step 1) the 50mL Na of gained
2wO
4solution slowly joins in beaker along walls of beaker, and wherein the mol ratio of Bi and W is 1:0.25-1:6, leaves standstill reaction 1-72h in 25-90 DEG C of constant temperature, gained sediment after filtration, washing and dry, obtain the amorphous Bi of atresia
2wO
6nanometer sheet;
3) by step 2) the amorphous Bi of atresia that obtains
2wO
6nanometer sheet is placed in 200-800 DEG C of high-temperature heat treatment 0.5-5h, namely obtains porous Bi
2wO
6nanosheet photocatalytic material.
2. porous Bi according to claim 1
2wO
6the preparation method of nanosheet photocatalytic material, is characterized in that step 1) described in Na
2wO
4concentration is 0.03-0.30mol/L.
3. porous Bi according to claim 1
2wO
6the preparation method of nanosheet photocatalytic material, is characterized in that step 2) described in standing reaction temperature be 25-60 DEG C, the reaction time is 24-48h.
4. porous Bi according to claim 1
2wO
6the preparation method of nanosheet photocatalytic material, is characterized in that step 2) described in the mol ratio of Bi and W be 1:1-1:3.
5. porous Bi according to claim 1
2wO
6the preparation method of nanosheet photocatalytic material, is characterized in that step 3) described in high-temperature heat treatment temperature be 350-600 DEG C, the high-temperature heat treatment time is 1-3h.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114011403A (en) * | 2021-12-16 | 2022-02-08 | 广东工业大学 | Preparation method and application of amorphous bismuth tungstate photocatalytic material |
CN115254187A (en) * | 2022-08-03 | 2022-11-01 | 江苏理工学院 | Preparation method and application of mesoporous amorphous bismuth tungstate photocatalytic material |
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US20070123730A1 (en) * | 2005-11-29 | 2007-05-31 | Saudi Basic Industries Corporation | Catalyst composition without antimony or molybdenum for ammoxidation of alkanes, a process of making and a process of using thereof |
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US20070123730A1 (en) * | 2005-11-29 | 2007-05-31 | Saudi Basic Industries Corporation | Catalyst composition without antimony or molybdenum for ammoxidation of alkanes, a process of making and a process of using thereof |
Non-Patent Citations (2)
Title |
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FENG-JUN ZHANG等: "Rapid sonochemical synthesis of irregular nanolaminar-like Bi2WO6 as efficient visible-light-active photocatalysts", 《ULTRASONICS SONOCHEMISTRY》 * |
S. OBREGÓN ALFARO等: "Synthesis, characterization and visible-light photocatalytic properties of Bi2WO6 and Bi2W2O9 obtained by co-precipitation method", 《APPLIED CATALYSIS A: GENERAL》 * |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114011403A (en) * | 2021-12-16 | 2022-02-08 | 广东工业大学 | Preparation method and application of amorphous bismuth tungstate photocatalytic material |
CN114011403B (en) * | 2021-12-16 | 2022-07-12 | 广东工业大学 | Preparation method and application of amorphous bismuth tungstate photocatalytic material |
CN115254187A (en) * | 2022-08-03 | 2022-11-01 | 江苏理工学院 | Preparation method and application of mesoporous amorphous bismuth tungstate photocatalytic material |
CN115254187B (en) * | 2022-08-03 | 2023-06-30 | 江苏理工学院 | Preparation method and application of mesoporous amorphous bismuth tungstate photocatalytic material |
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