CN104587999B - Porous Bi2WO6The preparation method of nanosheet photocatalytic material - Google Patents
Porous Bi2WO6The preparation method of nanosheet photocatalytic material Download PDFInfo
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Abstract
The present invention relates to porous Bi2WO6The preparation method of nanosheet photocatalytic material, includes next coming in order step：By Bi (NO3)3Pressed powder evenly laid out in beaker bottom, then Na2WO4Solution is slowly added in beaker along walls of beaker, constant temperature standing and reacting, and gained sediment, through filtering, washing and be dried, obtains the amorphous Bi of atresia2WO6Nanometer sheet；It is placed in 200 800 DEG C of high-temperature heat treatment 0.5 5h, that is, obtain porous Bi2WO6Nanosheet photocatalytic material.The beneficial effects of the present invention is：It is a kind of quick, economic, green porous Bi2WO6The synthetic method of nanosheet photocatalytic material.Porous Bi being synthesized by this method2WO6Nanosheet photocatalytic material has larger specific surface area, so that Bi2WO6Show high photocatalysis performance.
Description
Technical field
The present invention relates to the technical field of porous material and sheetlike material, relate particularly to porous Bi2WO6Nanometer
The preparation method of piece catalysis material.
Technical background
Because global problem of environmental pollution is increasingly serious, had in terms of degradable organic pollutant extensively using catalysis material
Wealthy development prospect.It is known that the energy gap of bismuth tungstate is about 2.7eV, it is more than the sunlight visible ray of 420nm in wavelength
There is very strong absorption in region, and light-catalyzed reaction can occur.Bismuth tungstate after the irradiation by visible ray, absorb photon energy and
Excite and create light induced electron and hole, and and then produce active oxygen and hydroxyl radical free radical etc., there is very strong oxidability, it
Can make majority of organic pollutants oxidation decomposition.Therefore, on solving problem of environmental pollution, good work can be played
With.On this basis, due to quantum size effect, the band gap of nanoparticle increases nano material with the reduction of particle size
Greatly, it is led to have stronger photo-catalysis capability.Additionally, again because porous material has density is low, quality is little, specific surface area is big etc.
Advantage, has the Bi of loose structure2WO6Nanosheet photocatalytic material will have great advantage in light-catalysed performance.At present,
The synthetic method of porous material mainly has hard template method and soft template method.However, template is typically by calcination or chemistry extraction
Remove non-material component and pore-creating, its complex operation, and easily cause to material structure during non-material component removes
Destruction.Therefore, there is the Bi of loose structure and nanoscale using simple, green template-free method synthesis2WO6Become one
Individual important research direction.
The current micro structure study on regulation with regard to bismuth tungstate catalysis material be concentrated mainly on nanoparticle, laminated structure and
The research of the aspects such as spherical structure.As far as we know, there is presently no using the synthesizing porous Bi of template-free method2WO6Nanometer sheet light is urged
Change material, to improve the relevant report of its photocatalysis performance.
Content of the invention
The technical problem to be solved is for above-mentioned prior art, proposes a kind of porous Bi2WO6Nanometer sheet light
The preparation method of catalysis material：On the premise of not using any template and pore creating material, by regulating and controlling WO in solution4 2-Ion
In solid Bi (NO3)3The reaction rate on surface, to prepare Bi2WO6Nanometer sheet presoma；Pass through again to control heat treatment temperature to obtain
Must have the Bi of loose structure2WO6Nanosheet photocatalytic material.
The present invention solves above-mentioned technical problem and be employed technical scheme comprise that：Porous Bi2WO6Nanosheet photocatalytic material
Preparation method, includes next coming in order step：
1) by Na2WO4It is dissolved in formation homogeneous solution, wherein Na in distilled water2WO4Solubility is 0.005-0.50mol/L；
2) by Bi (NO3)3Pressed powder evenly laid out in beaker bottom, then by step 1) the 50mL Na of gained2WO4Solution
It is slowly added in beaker along walls of beaker, the mol ratio of wherein Bi and W is 1:0.25-1:6, in 25-90 DEG C of constant temperature standing and reacting
1-72h, gained sediment, through filtering, washing and be dried, obtains the amorphous Bi of atresia2WO6Nanometer sheet；
3) by step 2) the amorphous Bi of atresia that obtains2WO6Nanometer sheet is placed in 200-800 DEG C of high-temperature heat treatment 0.5-5h, that is,
Obtain porous Bi2WO6Nanosheet photocatalytic material.
By such scheme, step 1) described in Na2WO4Concentration is 0.03-0.30mol/L.
By such scheme, step 2) described in standing and reacting temperature be 25-60 DEG C, the response time be 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 be 1-
3h.
The present invention proposes under no template action, first with solid Bi (NO3)3And Na2WO4The standing self assembly of solution is anti-
Should, by regulating and controlling WO in solution4 2-Ion is in solid Bi (NO3)3The reaction rate on surface, generates Bi2WO6Nanometer sheet presoma,
Again by the heat treatment temperature control to presoma, to obtain the Bi with loose structure2WO6Nanometer sheet, it is substantially former that it synthesizes
Reason is：
2Bi(NO3)3(s)+WO4 2-(aq)+2H2O(l)→Bi2WO6(s)+4H+(aq)+6NO3 -(aq)
Porous Bi2WO6The photocatalytic activity of nanosheet photocatalytic material is by Photocatalytic Degradation of Phenol solution under ultraviolet light
Characterized.Experimentation is as follows：By 0.10g porous Bi2WO6Nanosheet photocatalytic material is dispersed in molten equipped with 10mL phenol
Liquid (20mg L-1) reaction bulb in, reaction bulb is positioned over dark place 2h to reach catalyst and the intermolecular absorption of phenol-de-
Attached balance.At ambient temperature, the ultraviolet LED light source (wavelength being 4W with power：UV-365nm) irradiate, measure every 5min molten
Phenol concentration in liquid.In degradation solution, the concentration of phenol is measured by ultraviolet-visible absorption spectroscopy instrument (UVmini 1240, Japan).
Porous Bi2WO6The Characterization for Microstructure method of nanosheet photocatalytic material：Observed with field emission scanning electron microscope (FESEM)
Pattern and granular size, crystallize situation with X-ray diffraction (XRD) spectrum analyses, observe the hole knot of material with transmission electron microscope (TEM)
Structure and crystal structure, with the light absorbs situation of UV-vis analysis of material.
The beneficial effects of the present invention is：The synthesizing porous Bi of employing template-free method of the present invention2WO6Nanometer sheet light is urged
Change material, any template or other additives need not be added, building-up process have the advantages that simply, environmental protection, pollution-free, be one
Plant quick, economic, green porous Bi2WO6The synthetic method of nanosheet photocatalytic material.The porous being synthesized by this method
Bi2WO6Nanosheet photocatalytic material has larger specific surface area, so that Bi2WO6Show high photocatalysis performance.This
Bright have the advantages that to operate that very simple, equipment requirements are low, various reaction units that need not be expensive, be easy to high-volume and synthesize, and has
Hope and produce good Social and economic benef@.
Brief description
Fig. 1 is porous Bi in embodiment 12WO6The FESEM figure of nanometer sheet；
Fig. 2 is porous Bi in embodiment 12WO6The XRD spectrum of nanometer sheet：
Fig. 3 is porous Bi in embodiment 12WO6The TEM figure of nanometer sheet；
Fig. 4 is porous Bi in embodiment 12WO6The UV-vis collection of illustrative plates of nanometer sheet：
Fig. 5 is porous Bi in embodiment 12WO6The degradation rate constant k of nanometer sheet Pyrogentisinic Acid:(a)Bi2WO6；(b)Pt/
Bi2WO6
Fig. 6 is the Bi in embodiment 1 without high-temperature heat treatment2WO6The FESEM figure of nanometer sheet；
Fig. 7 is the Bi in embodiment 1 without high-temperature heat treatment2WO6The XRD spectrum of nanometer sheet.
Specific embodiment
With reference to embodiment, the present invention will be further described in detail, but this explanation will not be constituted to the present invention's
Limit.
Embodiment 1：
Porous Bi2WO6The building-up process of nanosheet photocatalytic material is as follows：1) by Na2WO4It is dissolved in distilled water and being formed all
Even solution, wherein Na2WO4Solubility is 0.125mol/L；2) by Bi (NO3)3Pressed powder evenly laid out in beaker bottom, then will
Step 1) gained 50mL Na2WO4Solution is slowly added in beaker along walls of beaker, and the mol ratio of wherein Bi and W is 1:3, in
25 DEG C of constant temperature standing and reacting 48h, gained sediment, through filtering, washing and be dried, obtains the amorphous Bi of atresia2WO6Nanometer sheet；3) will
Step 2) the amorphous Bi of atresia that obtains2WO6Nanometer sheet is placed in 500 DEG C of high-temperature heat treatment 2h, that is, obtain porous Bi2WO6Nanometer sheet
Catalysis material.
Fig. 1 is porous Bi2WO6The FESEM figure of nanosheet photocatalytic material.Prepared by can be seen that from Figure 1A and Figure 1B
Sample is existed with loose aggregation, and assumes obvious porous laminated structure.Can be seen that each Bi from Fig. 1 C and 1D2WO6
Nanometer sheet is made up of many nano-particle, and its size is 30-100nm；Meanwhile, Bi2WO6Exist many between nano-particle
Less hole, its aperture is 20-80nm.
Fig. 2 is porous Bi2WO6The XRD spectra of nanosheet photocatalytic material.Result shows：Each diffraction maximum position and standard
Bi2WO6Result consistent it was demonstrated that prepared sample is Bi2WO6Material；Meanwhile, each diffraction maximum peak intensity is narrower, and porous is described
Bi2WO6The degree of crystallinity of nanometer sheet is higher, and grain size is less.
Fig. 3 is porous Bi2WO6The TEM figure of nanosheet photocatalytic material.Institute can be more clearly visible that from Fig. 3 A, 3B and 3C
The sample of preparation is lamellar Bi with loose structure2WO6Material, the size of pore structure is consistent with the result of FESEM.Fig. 3 D
For lamellar Bi2WO6Between nanoparticle, the high-resolution TEM figure at interface, shows Bi2WO6There is between the particle of nanometer sheet good combination
Effect.
Fig. 4 is porous Bi2WO6The UV-vis collection of illustrative plates of nanosheet photocatalytic material.It can be seen that porous Bi2WO6
Nanometer sheet has good absorbent properties in visible region, and absorbable wavelength reaches the visible ray of 500nm it was demonstrated that can as one kind
See light catalysis material.
Fig. 5 is porous Bi2WO6The degradation rate constant of nanosheet photocatalytic material Pyrogentisinic Acid's solution.Can from figure
Go out, porous Bi modified without Pt2WO6Nanometer sheet Pyrogentisinic Acid is hardly degraded performance, and after modifying through Pt, porous Bi2WO6
Nanosheet photocatalytic material shows obvious Photocatalytic Degradation Property, and its speed constant is 0.0074min-1.Ground according to forefathers
Study carefully result, Bi2WO6The conduction level of material be about+0.3V so as to light induced electron effectively can not reduce oxygen, so almost not having
There is the performance of Photocatalytic Degradation of Phenol；And Pt metal can effectively make Bi as effective auxiliary agent of catalysis material2WO6Conduction band electricity
Son is quickly transferred on Pt, and then reduces oxygen by polyelectron hydrogen reduction path, thus showing high photocatalysis performance.
Fig. 6 is the Bi without high-temperature heat treatment2WO6The FESEM figure of nanometer sheet presoma.Fig. 6 A and Fig. 6 B shows, without height
The Bi that warm is processed2WO6Though nanometer sheet presoma has flaky nanometer structure, there is no pore structure, show Bi2WO6Piece
Shape structure can pass through solid Bi (NO3)3With Na2WO4Between self-assembling reaction obtain, and the loose structure in nanometer sheet is to pass through
The high-temperature heat treatment in later stage and formed.
Fig. 7 is the Bi without high-temperature heat treatment2WO6The XRD spectrum of nanometer sheet presoma.With Fig. 2 contrast it can be seen that not
Bi through high-temperature heat treatment2WO6Nanometer sheet degree of crystallinity is very low, is substantially at amorphous state, thus the high-temperature heat treatment mistake in later stage
Journey both ensure that Bi2WO6Crystallization, cause being effectively formed of loose structure again.
Embodiment 2：
In order to check Na2WO4Concentration is to porous Bi2WO6The impact of nanosheet photocatalytic material structure, except Na2WO4Concentration with
Outward, other reaction conditions are as follows：Reaction temperature (25 DEG C), response time (48h), the mol ratio (1 of Bi and W:3), at high warm
Reason temperature (500 DEG C), high-temperature heat treatment time (2h) etc. are all same as Example 1.Result shows, works as Na2WO4Concentration is
During 0.005mol/L, due to WO in system4 2-Concentration is too low, Bi2WO6Self assembly speed is less, leads to its laminated structure inconspicuous.
Work as Na2WO4When concentration is between 0.03-0.30mol/L, can get the larger Bi of thinner thickness, area2WO6Presoma.When
Na2WO4When concentration is 0.50mol/L, due to WO4 2-Excessive concentration, Bi2WO6Crystal growth rate is too fast, leads to each flake crystalline
It is stacked between body, piece thickness increases so as to specific surface area reduces.Therefore, in porous Bi2WO6Nanosheet photocatalytic material
In building-up process, Na2WO4The optimum range of concentration is 0.03-0.30mol/L.
Embodiment 3：
In order to check reaction temperature to porous Bi2WO6The impact of nanosheet photocatalytic material, in addition to the reaction temperature, other
Reaction condition is as follows：Na2WO4Concentration (0.125mol/L), response time (48h), the mol ratio (1 of Bi and W:3), at high warm
Reason temperature (500 DEG C), high-temperature heat treatment time (2h) etc. are all same as Example 1.Result shows, when reaction temperature is in 25-60
DEG C when, self assembly speed is moderate, can obtain high-purity and the good Bi of lamellar structure in the short period of time2WO6Nanometer sheet.When
, when 90 DEG C, reaction rate is too fast for reaction temperature, leads to be stacked between each flat crystal, and piece thickness also thus increase
Plus.Therefore, in porous Bi2WO6In 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 response time to porous Bi2WO6The impact of nanosheet photocatalytic material, in addition to the response time, other
Reaction condition is as follows：Na2WO4Concentration (0.125mol/L), reaction temperature (25 DEG C), the mol ratio (1 of Bi and W:3), at high warm
Reason temperature (500 DEG C), high-temperature heat treatment time (2h) etc. are all same as Example 1.Result shows, when reacted between for 1h when,
Na2WO4Solution and Bi (NO3)3Solid is completely incomplete, and with Bi (NO3)3The formation of hydrolysising by-product.Between when reacted it is
During 24-48h, raw material is fully reacted, and can obtain the Bi that purity is high, surface area is big2WO6Nanometer sheet.Between when reacted it is
During 72h, the Bi of gained2WO6Nanometer sheet is completed already due to reaction, and the structure of nanometer sheet is had no significant effect, in time cost
On cause waste.Therefore, in porous Bi2WO6In the building-up process of nanosheet photocatalytic material, the optimum range in response time is
24-48h.
Embodiment 5：
In order to check the mol ratio of Bi and W to porous Bi2WO6The impact of nanosheet photocatalytic material, except Bi and W mole
In addition, other reaction conditions are as follows for ratio：Na2WO4Concentration (0.125mol/L), reaction temperature (25 DEG C), response time (48h), height
Warm treatment temperature (500 DEG C), high-temperature heat treatment time (2h) etc. are all same as Example 1.Result shows, Bi and W mole
Than for 1:When 0.25, raw material Bi (NO3)3Reaction is insufficient, so that product purity is reduced and causes Bi (NO3)3Wastage of material.Work as Bi
Mol ratio with W is 1:1-1:When 3, raw material reaction is abundant, and the Bi of gained2WO6Nanometer sheet purity is high, pattern is preferable.When Bi with
The mol ratio of W is 1:When 6, the Bi of gained2WO6Nanometer sheet purity does not have with WO4 2-Excess and raise, and raw material can be caused
Na2WO4Waste.Therefore, in porous Bi2WO6In the building-up process of nanosheet photocatalytic material, the optimal model of Bi and W mol ratio
Enclose is 1:1-1:3.
Embodiment 6：
In order to check high-temperature heat treatment temperature to porous Bi2WO6The impact of nanosheet photocatalytic material, except high-temperature heat treatment
Beyond temperature, other reaction conditions are as follows：Na2WO4Concentration (0.125mol/L), reaction temperature (25 DEG C), the response time (48h),
The mol ratio (1 of Bi and W:3), high-temperature heat treatment time (2h) etc. is all same as Example 1.Result shows, high-temperature heat treatment temperature
When spending for 200 DEG C, Bi2WO6Crystal formation does not convert completely, and degree of crystallinity is relatively low, and pore structure is formed seldom simultaneously.When high-temperature heat treatment temperature
When spending for 350-600 DEG C, Bi2WO6Nanometer sheet forerunner's physical ability transforms into higher porous Bi of degree of crystallinity2WO6Nanometer sheet.Work as height
When warm treatment temperature is 800 DEG C, porous Bi2WO6The pore structure of nanometer sheet can be destroyed.Therefore, in porous Bi2WO6Nanometer
In the building-up process of piece catalysis 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 Bi2WO6The impact of nanosheet photocatalytic material, except high-temperature heat treatment
Beyond time, other reaction conditions are as follows：Na2WO4Concentration (0.125mol/L), reaction temperature (25 DEG C), the response time (48h),
The mol ratio (1 of Bi and W:3), high-temperature heat treatment temperature (500 DEG C) etc. is all same as Example 1.Result shows, at high warm
When the reason time is 0.5h, Bi2WO6Nanometer sheet presoma leads to degree of crystallinity to decline because the response time is insufficient, and pore structure is not
Substantially.When the high-temperature heat treatment time being 1-3h, Bi2WO6Nanometer sheet presoma fully reacts, and degree of crystallinity is higher and pore structure is complete
Whole.When the high-temperature heat treatment time being 5h, Bi2WO6Nanometer sheet presoma does not change with the prolongation of high-temperature heat treatment time,
Cause the consumption of the excessively unnecessary energy, and cause the decline of preparation efficiency.Therefore, in porous Bi2WO6Nanometer sheet photocatalysis material
In the building-up process of material, the optimum range of high-temperature heat treatment time is 1-3h.
Claims (5)
1. porous Bi2WO6The preparation method of nanosheet photocatalytic material, includes next coming in order step：
1) by Na2WO4It is dissolved in formation homogeneous solution, wherein Na in distilled water2WO4Concentration is 0.005-0.50mol/L；
2) by Bi (NO3)3Pressed powder evenly laid out in beaker bottom, then by step 1) the 50mL Na of gained2WO4Solution is along burning
Wall of cup is slowly added in beaker, and the mol ratio of wherein Bi and W is 1:0.25-1:6, in 25-90 DEG C of constant temperature standing and reacting 1-
72h, gained sediment, through filtering, washing and be dried, obtains the amorphous Bi of atresia2WO6Nanometer sheet；
3) by step 2) the amorphous Bi of atresia that obtains2WO6Nanometer sheet is placed in 200-800 DEG C of high-temperature heat treatment 0.5-5h, that is, obtain
Porous Bi2WO6Nanosheet photocatalytic material.
2. porous Bi according to claim 12WO6The preparation method of nanosheet photocatalytic material is it is characterised in that step 1)
Described Na2WO4Concentration is 0.03-0.30mol/L.
3. porous Bi according to claim 12WO6The preparation method of nanosheet photocatalytic material is it is characterised in that step 2)
Described standing and reacting temperature is 25-60 DEG C, and the response time is 24-48h.
4. porous Bi according to claim 12WO6The preparation method of nanosheet photocatalytic material is it is characterised in that step 2)
The mol ratio of described Bi and W is 1:1-1:3.
5. porous Bi according to claim 12WO6The preparation method of nanosheet photocatalytic material is it is characterised in that step 3)
Described high-temperature heat treatment temperature is 350-600 DEG C, and the high-temperature heat treatment time is 1-3h.
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| CN114011403B (en) * | 2021-12-16 | 2022-07-12 | 广东工业大学 | Preparation method and application of 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 |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
|---|
| Rapid sonochemical synthesis of irregular nanolaminar-like Bi2WO6 as efficient visible-light-active photocatalysts;Feng-Jun Zhang等;《Ultrasonics Sonochemistry》;20120804;第20卷;第209-215页 * |
| Synthesis, characterization and visible-light photocatalytic properties of Bi2WO6 and Bi2W2O9 obtained by co-precipitation method;S. Obregón Alfaro等;《Applied Catalysis A: General》;20100601;第383卷;第128-133页 * |
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