CN105582909A - Preparation method and application of bismuth tungstate/expanded graphite sheet nanocomposite - Google Patents
Preparation method and application of bismuth tungstate/expanded graphite sheet nanocomposite Download PDFInfo
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- CN105582909A CN105582909A CN201510979059.4A CN201510979059A CN105582909A CN 105582909 A CN105582909 A CN 105582909A CN 201510979059 A CN201510979059 A CN 201510979059A CN 105582909 A CN105582909 A CN 105582909A
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- expanded graphite
- bismuth tungstate
- bismuth
- tungstate
- composite material
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- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 71
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 71
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 title claims abstract description 68
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 62
- 239000010439 graphite Substances 0.000 title claims abstract description 62
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000002114 nanocomposite Substances 0.000 title abstract description 3
- 239000002131 composite material Substances 0.000 claims abstract description 43
- 239000002086 nanomaterial Substances 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- 239000008367 deionised water Substances 0.000 claims abstract description 17
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 17
- 238000005406 washing Methods 0.000 claims abstract description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000004927 clay Substances 0.000 claims abstract description 12
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims abstract description 11
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 238000000227 grinding Methods 0.000 claims abstract description 4
- 241000446313 Lamella Species 0.000 claims description 23
- 229960000892 attapulgite Drugs 0.000 claims description 8
- 229910052625 palygorskite Inorganic materials 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 7
- 238000009413 insulation Methods 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- 238000001354 calcination Methods 0.000 claims description 2
- 238000006555 catalytic reaction Methods 0.000 claims description 2
- 230000014759 maintenance of location Effects 0.000 claims description 2
- 230000015572 biosynthetic process Effects 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 9
- 239000000203 mixture Substances 0.000 abstract description 4
- 230000003197 catalytic effect Effects 0.000 abstract description 3
- WUTHJWCAESRVMV-UHFFFAOYSA-N [W].[Bi] Chemical compound [W].[Bi] WUTHJWCAESRVMV-UHFFFAOYSA-N 0.000 abstract 1
- 238000005054 agglomeration Methods 0.000 abstract 1
- 230000002776 aggregation Effects 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract 1
- 238000004321 preservation Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 25
- 238000013019 agitation Methods 0.000 description 18
- 238000001027 hydrothermal synthesis Methods 0.000 description 7
- CXKWCBBOMKCUKX-UHFFFAOYSA-M methylene blue Chemical compound [Cl-].C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 CXKWCBBOMKCUKX-UHFFFAOYSA-M 0.000 description 7
- 229960000907 methylthioninium chloride Drugs 0.000 description 7
- 239000002244 precipitate Substances 0.000 description 7
- 230000015556 catabolic process Effects 0.000 description 6
- 238000006731 degradation reaction Methods 0.000 description 6
- 239000011259 mixed solution Substances 0.000 description 6
- 238000001556 precipitation Methods 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 238000005352 clarification Methods 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- -1 compound sodium tungstate Chemical class 0.000 description 2
- 239000004567 concrete Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 238000009830 intercalation Methods 0.000 description 2
- 230000002687 intercalation Effects 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000002023 wood Substances 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000012876 carrier material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 238000004537 pulping Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical compound FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/24—Chromium, molybdenum or tungsten
- B01J23/31—Chromium, molybdenum or tungsten combined with bismuth
-
- B01J35/39—
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/40—Organic compounds containing sulfur
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
The invention belongs to the technical field of supported composites and particularly relates to a preparation method and an application of a nanomaterial taking bismuth tungsten as an active component. Bismuth nitrate, sodium tungstate and expanded graphite are added to deionized water while stirring, then the mixture is transferred to a reaction kettle to have a heat preservation reaction under the hydrothermal condition, water washing, alcohol washing, drying and grinding are performed, and thus the bismuth tungstate/expanded graphite sheet nanocomposite is obtained. The composite is high in catalytic activity and can be applied to photocatalytic degradation of organic matters; besides, the reduction of the particle size of single bismuth tungstate particles on a supporter is effectively controlled, and agglomeration is fully avoided when prepared small-particle bismuth tungstate is supported on other clay supporters.
Description
Technical field
The invention belongs to support type technical field of composite materials, particularly a kind of taking expanded graphite nanometer sheet as carrier, bismuth tungstateFor preparation method and the application thereof of the nano material of active component.
Background technology
Bismuth tungstate (Bi2WO6) be layer structure, have dielectric, luminous, from characteristics such as conductors, and bismuth tungstate is at visible rayUnder there is photocatalysis performance, can photodissociation water and light degradation organic pollution, therefore bismuth tungstate (Bi under visible ray2WO6) veryMany association areas have good application prospect, are carried on clay that to use as composite be also a good selection.
Clay has powerful adsorption capacity, good heat endurance, resistance to acids and bases, rheological characteristic, fillibility, and hasThe functions such as good ion-exchange, anti-salt, antigelation, pulping and high-temperature phase-change are very promising carrier materials. But orderBefore, the clay application of China is also in lower level.
The problem existing in application with regard to clay, major embodiment is dispersion problem, for example, if the particle diameter of loaded article particle isGreatly, even also can cause on optimum carrier, distribution meeting is inhomogeneous, generation is reunited, affect combination.
Summary of the invention
Technical problem to be solved by this invention is: first a kind of bismuth tungstate/expanded graphite lamella nanostructured composite wood is providedThe preparation method of material, concrete technology is:
Bismuth nitrate, sodium tungstate and expanded graphite are joined to deionized water for stirring, then transfer in reactor at hydrothermal conditionLower insulation reaction, after through washing, alcohol wash, oven dry, grinding, obtain bismuth tungstate/expanded graphite lamella nanostructured composite woodMaterial, this composite, is taking expanded graphite nanometer sheet as carrier, at expanded graphite area load bismuth tungstate, composite wood of the present inventionThe composition general formula of material is expressed as: Bi2WO6/ EG, wherein Bi2WO6Represent bismuth tungstate, EG represents that expanded graphite nanometer sheet carriesBody,
Wherein, the mol ratio of bismuth nitrate and sodium tungstate is 1:3~1:8,
The addition of expanded graphite is that 1:2~1:8 calculates according to the mass ratio of expanded graphite and bismuth tungstate,
Product after hydro-thermal need to be through repeatedly washing and alcohol wash to eliminate impurity, and insulation oven dry 12 at 60~100 DEG C~24h,
Under hydrothermal condition, in insulation reaction, hydrothermal temperature is 180~240 DEG C, and hydro-thermal temperature retention time is 16~24h.
The present invention also provides a kind of application of bismuth tungstate/expanded graphite lamella nanostructure composite material of above-mentioned preparation: be about toThis composite is as the application of catalysis material,
The present invention adopts one step hydro thermal method to prepare bismuth tungstate/expanded graphite lamella nanostructure composite material, expanded graphite toolThere is larger specific area can make above bismuth tungstate loads on comparatively uniformly, can improve the catalytic performance of this composite;
In addition, the present invention also provides a kind of application of bismuth tungstate/expanded graphite lamella nanostructure composite material of preparing:
Bismuth tungstate/expanded graphite lamella nanostructure composite material, as for expanded graphite being removed under high temperature, is then passed through to two stepsThe method of modification loads to above clay bismuth tungstate, and concrete steps are:
Bismuth tungstate/expanded graphite lamella nanostructure composite material of above-mentioned preparation is fired to constant weight under 900 DEG C of hot environments,Obtain bismuth tungstate (bismuth tungstate is high temperature resistant, 900 DEG C of variations on can recurring structure), by the bismuth tungstate acidifying of gained, then logicalCross sol-gal process, the bismuth tungstate after acidifying and clay are joined in 100ml deionized water by the mass ratio of 1:5, andUnder 70 DEG C of water bath condition, continue to stir until form gel, then 80 DEG C of dry 12h, 520 DEG C of calcining 2h, obtain bismuth tungstate/glutinousSoil composite material (Bi2WO6/ATP),
Wherein, above-mentioned souring operation is, adopts the hydrochloric acid 5ml that solute mass fraction is 10%, under normal temperature (25 DEG C) to tungstenAcid bismuth carries out modification, uses absolute ethanol washing 3 times after modification, 80 DEG C of oven dry,
Clay is attapulgite.
Beneficial effect of the present invention is embodied in:
1, expanded graphite not only can promote effective dispersion of product bismuth tungstate as carrier, and the present invention fully recognizes and profitWith expanded graphite the template effect that provides of space structure is provided has effectively controlled the particle diameter of single bismuth tungstate particle and diminish, then willWhen prepared small particle diameter bismuth tungstate is carried on other clay carriers, just can make its equably load get on, avoided reunion;
2, the loose structure of expanded graphite and stronger absorption property can maintain the photocatalysis efficiency that bismuth tungstate suspension system is higher.
3, the electric conductivity of graphite can shift photo-generated carrier and avoid compound, thereby has improved bismuth tungstate/expanded graphite lamella nanometerThe light-catalysed activity of structural composite material;
4, the present invention, by the hydro-thermal of proper temperature, disperses the bismuth tungstate sheet that loads to expanded graphite surface relatively, obtains wolframic acidBismuth/expanded graphite lamella nanostructure composite material, with respect to pure bismuth tungstate, the catalytic activity of this composite increases;
5, the inventive method is simple, easy to control, and cost is low.
Brief description of the drawings
Fig. 1 is Bi2WO6, EG and the prepared Bi of embodiment 12WO6/EG(Bi2WO6/ EG=1/2) XRD spectra of sample;
Fig. 2 is the prepared Bi of embodiment 12WO6/EG(Bi2WO6/ EG=1/2) sample 100nm scale scope TEM shineSheet;
Fig. 3 is the prepared Bi of embodiment 12WO6/EG(Bi2WO6/ EG=1/2) the concentration degradation curve of sample to methylene blue.
Fig. 4 is the bismuth tungstate/attapulgite composite material (Bi preparing respectively in embodiment 1 and comparative example 12WO6/ATP)To the concentration degradation curve of methylene blue.
Detailed description of the invention
The preparation of expanded graphite:
Press crystalline flake graphite, the mass ratio of the concentrated sulfuric acid, hydrogen peroxide and potassium bichromate is 10:30:5:1 sample thief, 40 DEG C of perseverancesIn tepidarium, be oxidized, intercalation 12h, then press crystalline flake graphite 1:0.9HNO3Amount add nitric acid, secondary intercalation, continue reaction 30min,Washing, dries, and instantaneous expansion in 900 DEG C of Muffle furnaces, obtains expanded graphite.
Embodiment 1
First the bismuth nitrate that takes 0.17g is dissolved in the deionized water of 50ml, and magnetic agitation 30min, obtains white solution; Again toIn white solution, add the sodium tungstate of 0.047g, continue magnetic agitation 30min and be mixed to get white mixed solution, to described solutionIn add the expanded graphite of 0.2g to continue magnetic agitation 10min, obtain black turbid solution; Above-mentioned solution is put into 100ml poly-Tetrafluoroethene reactor, then 180 DEG C of hydro-thermal reaction 24h; Reaction finishes rear taking-up reactor and obtains lower black precipitation, upper strataSettled solution; By black precipitate deionized water, absolute ethanol washing, then 80 DEG C of oven dry, grind and obtain bismuth tungstate/expansion stoneInk sheet layer nanostructure composite material.
Gained sample is carried out to X-ray powder diffraction experiment, and observe its pattern and structure under transmission electron microscope, according to embodimentThe XRD collection of illustrative plates of bismuth tungstate/expanded graphite lamella nanostructure composite material that 1 technological parameter makes and bismuth tungstate, expanded graphiteAs shown in Figure 1. In the XRD of composite, there is bismuth tungstate and expanded graphite characteristic diffraction peak separately, expanded graphite has been describedThe compound sodium tungstate of success.
EG/Bi2WO6The TEM photo of sample as shown in Figure 2. As can be seen from the figure, expanded graphite nanometer sheet and bismuth tungstateSheet is comparatively evenly combined with each other, consistent with the result of XRD.
Bi2WO6、EG/Bi2WO6Sample to the degradation curve of methylene blue as shown in Figure 3, as can be seen from the figure, Bi2WO6Clearance to methylene blue is about 70%, EG/Bi2WO6Sample reaches more than 97% the clearance of methylene blue.
Again bismuth tungstate/expanded graphite lamella the nanostructure composite material obtaining in the present embodiment is calcined under 900 DEG C of hot environmentsTo constant weight, obtain bismuth tungstate (bismuth tungstate is high temperature resistant, 900 DEG C of variations on can recurring structure), by the bismuth tungstate of gained and 5mlIt is acidified modified that solute mass fraction is that hydrochloric acid mix and blend at 25 DEG C of 10% carries out for 2 hours, after filtration, washes with absolute ethyl alcohol againWash bismuth tungstate 3 times, 80 DEG C of oven dry; Then by sol-gal process, the bismuth tungstate after acidifying and 1g attapulgite are joinedIn 100ml deionized water, and under 70 DEG C of water bath condition, continue to stir until form gel, then 80 DEG C of dry 12h, 520 DEG CCalcining 2h, obtains bismuth tungstate/attapulgite composite material (Bi2WO6/ ATP), this material to the degradation rate curve of methylene blue asShown in accompanying drawing 4.
Comparative example 1:
First the bismuth nitrate that takes 0.17g is dissolved in the deionized water of 50ml, and magnetic agitation 30min, obtains white solution; Again toIn white solution, add the sodium tungstate of 0.047g, continue magnetic agitation 30min and be mixed to get white mixed solution, to described solutionIn add 1g attapulgite to continue magnetic agitation 10min, obtain grey turbid solution; Above-mentioned solution is put into 100ml polytetrafluoroEthylene reaction still, then 180 DEG C of hydro-thermal reaction 24h; Reaction finishes rear taking-up reactor and obtains lower floor's gray precipitate, upper strata clarificationSolution; By gray precipitate deionized water, absolute ethanol washing, then 80 DEG C of oven dry, grinding obtains bismuth tungstate/attapulgite and receivesRice structural composite material. This material to the degradation rate curve of methylene blue as shown in curve A in accompanying drawing 4.
By more visible: in the present invention by the introducing of expanded graphite, fully refinement the particle diameter of bismuth tungstate, then by its loadAfter on attapulgite, more even than growth in situ bismuth tungstate dispersion out, avoid better reunion.
Embodiment 2:
The bismuth nitrate that takes 0.17g is dissolved in the deionized water of 50ml, and magnetic agitation 30min, obtains white solution; Again to whiteIn solution, add the sodium tungstate of 0.05g, continuation magnetic agitation 30min is mixed to get white mixed solution and adds in described solutionThe expanded graphite of 0.3g continues magnetic agitation 10min, obtains black turbid solution; Above-mentioned solution is put into 100ml polytetrafluoroethyl-neAlkene reaction still, then 170 DEG C of hydro-thermal reaction 18h; Reaction finishes rear taking-up reactor and obtains lower black precipitation, and upper strata clarification is moltenLiquid; By black precipitate deionized water, absolute ethanol washing, then 70 DEG C of oven dry, grind and obtain bismuth tungstate/expanded graphite lamellaNanostructure composite material, subsequent detection is as embodiment 1.
Embodiment 3:
The bismuth nitrate that takes 0.17g is dissolved in the deionized water of 50ml, and magnetic agitation 30min, obtains white solution; Again to whiteIn solution, add the sodium tungstate of 0.06g, continuation magnetic agitation 30min is mixed to get white mixed solution and adds in described solutionThe expanded graphite of 0.4g continues magnetic agitation 10min, obtains black turbid solution; Above-mentioned solution is put into 100ml polytetrafluoroethyl-neAlkene reaction still, then 160 DEG C of hydro-thermal reaction 16h; Reaction finishes rear taking-up reactor and obtains lower black precipitation, and upper strata clarification is moltenLiquid; By black precipitate deionized water, absolute ethanol washing, then 60 DEG C of oven dry, grind and obtain bismuth tungstate/expanded graphite lamellaNanostructure composite material, subsequent detection is as embodiment 1.
Embodiment 4:
The bismuth nitrate that takes 0.17g is dissolved in the deionized water of 50ml, and magnetic agitation 30min, obtains white solution; Again to whiteIn solution, add the sodium tungstate of 0.07g, continuation magnetic agitation 30min is mixed to get white mixed solution and adds in described solutionThe expanded graphite of 0.5g continues magnetic agitation 10min, obtains black turbid solution; Above-mentioned solution is put into 100ml polytetrafluoroethyl-neAlkene reaction still, then 160 DEG C of hydro-thermal reaction 14h; Reaction finishes rear taking-up reactor and obtains lower black precipitation, and upper strata clarification is moltenLiquid; By black precipitate deionized water, absolute ethanol washing, then 60 DEG C of oven dry, grind and obtain bismuth tungstate/expanded graphite lamellaNanostructure composite material, subsequent detection is as embodiment 1.
Embodiment 5:
The bismuth nitrate that takes 0.17g is dissolved in the deionized water of 50ml, and magnetic agitation 30min, obtains white solution; Again to whiteIn solution, add the sodium tungstate of 0.07g, continuation magnetic agitation 30min is mixed to get white mixed solution and adds in described solutionThe expanded graphite of 0.6g continues magnetic agitation 10min, obtains black turbid solution; Above-mentioned solution is put into 100ml polytetrafluoroethyl-neAlkene reaction still, then 140 DEG C of hydro-thermal reaction 12h; Reaction finishes rear taking-up reactor and obtains lower black precipitation, and upper strata clarification is moltenLiquid; By black precipitate deionized water, absolute ethanol washing, then 60 DEG C of oven dry, grind and obtain bismuth tungstate/expanded graphite lamellaNanostructure composite material, subsequent detection is as embodiment 1.
Claims (9)
1. a preparation method for bismuth tungstate/expanded graphite lamella nanostructure composite material, is characterized in that: described preparationMethod is, bismuth nitrate, sodium tungstate and expanded graphite are joined to deionized water for stirring, then transfers in reactor in hydro-thermalInsulation reaction under condition, after through washing, alcohol wash, oven dry, grinding, obtain bismuth tungstate/expanded graphite lamella nanostructured compoundMaterial.
2. the preparation method of bismuth tungstate/expanded graphite lamella nanostructure composite material as claimed in claim 1, its feature existsIn: the mol ratio of bismuth nitrate and sodium tungstate is 1:3~1:8.
3. the preparation method of bismuth tungstate/expanded graphite lamella nanostructure composite material as claimed in claim 1, its feature existsIn: the addition of expanded graphite is that 1:2~1:8 calculates according to the mass ratio of expanded graphite and bismuth tungstate.
4. the preparation method of bismuth tungstate/expanded graphite lamella nanostructure composite material as claimed in claim 1, its feature existsIn: under hydrothermal condition, in insulation reaction, hydrothermal temperature is 180~240 DEG C, and hydro-thermal temperature retention time is 16~24h.
5. the preparation method of bismuth tungstate/expanded graphite lamella nanostructure composite material as claimed in claim 1, its feature existsIn: after washing, alcohol wash, at 60~100 DEG C, 12~24h is dried in insulation.
6. the application of bismuth tungstate/expanded graphite lamella nanostructure composite material as prepared in claim 1, is characterized in that:Described composite is used as catalysis material.
7. the application of bismuth tungstate/expanded graphite lamella nanostructure composite material as prepared in claim 1, is characterized in that:By bismuth tungstate/expanded graphite lamella nanostructure composite material as for expanded graphite being removed under high temperature, then by two step modificationsMethod loads to above clay bismuth tungstate.
8. the application of bismuth tungstate/expanded graphite lamella nanostructure composite material as prepared in claim 7, is characterized in that:Bismuth tungstate/expanded graphite lamella nanostructure composite material is fired to constant weight under 900 DEG C of hot environments, obtains bismuth tungstate, willAfter the bismuth tungstate acidifying of gained, under water bath condition, continue to stir until formation gel is then dry by sol-gal process and clayDry calcining obtains bismuth tungstate/clay composite.
9. the application of bismuth tungstate/expanded graphite lamella nanostructure composite material as prepared in claim 8, is characterized in that:Described clay is attapulgite.
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CN106076422A (en) * | 2016-06-13 | 2016-11-09 | 湘潭大学 | A kind of sepiolite supported porphyrin sensitization Bi2wO6the preparation method of visible light catalyst |
CN106975478A (en) * | 2017-03-17 | 2017-07-25 | 江苏省华源矿业有限公司 | The preparation method of bismuth tungstate/attapulgite composite material |
CN107649117A (en) * | 2017-10-27 | 2018-02-02 | 盛世园林集团股份有限公司 | A kind of bismuth molybdate/attapulgite clay compounded visible light catalytic material and preparation method thereof, application |
CN108620061A (en) * | 2018-06-21 | 2018-10-09 | 常州大学 | A kind of mesoporous tungsten oxide(WO3)Adulterate bismuth tungstate(Bi2WO6)The preparation method of composite photo-catalyst |
CN110586149A (en) * | 2019-09-24 | 2019-12-20 | 湖南大学 | Bismuth molybdate/titanium carbide heterojunction two-dimensional photocatalytic material and preparation method and application thereof |
CN112371113A (en) * | 2020-12-05 | 2021-02-19 | 常州大学 | Bi2WO6Preparation method and application of-rGO visible light catalyst |
WO2021072818A1 (en) * | 2019-10-15 | 2021-04-22 | 中山大学 | Preparation method for and application of bismuth tungstate-graphene-conductive hydrogel |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20070142223A1 (en) * | 2003-11-18 | 2007-06-21 | Basf Akiengesellschaft | Heterogeneous catalyst for the preparation of acrolein by partial gas phase oxidation of propene |
CN104971720A (en) * | 2015-06-11 | 2015-10-14 | 西北师范大学 | Bismuth tungstate nanocomposite, and preparation method and application thereof |
-
2015
- 2015-12-23 CN CN201510979059.4A patent/CN105582909B/en active Active
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20070142223A1 (en) * | 2003-11-18 | 2007-06-21 | Basf Akiengesellschaft | Heterogeneous catalyst for the preparation of acrolein by partial gas phase oxidation of propene |
CN104971720A (en) * | 2015-06-11 | 2015-10-14 | 西北师范大学 | Bismuth tungstate nanocomposite, and preparation method and application thereof |
Non-Patent Citations (2)
Title |
---|
ZHILIANG WANG等: "A sensitive o-aminophenol sensor based on a modified montmorillonite-modified expanded graphite electrode", 《APPLIED CLAY SCIENCE》 * |
马宏伟: "MnO2,Bi2WO6纳米材料及石墨烯复合物制备和性能研究", 《中国博士学位论文全文数据库工程科技Ⅰ辑》 * |
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CN106076422B (en) * | 2016-06-13 | 2018-04-20 | 湘潭大学 | A kind of sepiolite supported porphyrin sensitization Bi2WO6The preparation method of visible light catalyst |
CN106975478A (en) * | 2017-03-17 | 2017-07-25 | 江苏省华源矿业有限公司 | The preparation method of bismuth tungstate/attapulgite composite material |
CN107649117A (en) * | 2017-10-27 | 2018-02-02 | 盛世园林集团股份有限公司 | A kind of bismuth molybdate/attapulgite clay compounded visible light catalytic material and preparation method thereof, application |
CN107649117B (en) * | 2017-10-27 | 2020-06-30 | 盛世生态环境股份有限公司 | Bismuth molybdate/attapulgite composite visible light catalytic material, and preparation method and application thereof |
CN108620061A (en) * | 2018-06-21 | 2018-10-09 | 常州大学 | A kind of mesoporous tungsten oxide(WO3)Adulterate bismuth tungstate(Bi2WO6)The preparation method of composite photo-catalyst |
CN108620061B (en) * | 2018-06-21 | 2019-12-06 | 常州大学 | preparation method of mesoporous tungsten oxide (WO3) doped bismuth tungstate (Bi2WO6) composite photocatalyst |
CN110586149A (en) * | 2019-09-24 | 2019-12-20 | 湖南大学 | Bismuth molybdate/titanium carbide heterojunction two-dimensional photocatalytic material and preparation method and application thereof |
CN110586149B (en) * | 2019-09-24 | 2020-09-04 | 湖南大学 | Bismuth molybdate/titanium carbide heterojunction two-dimensional photocatalytic material and preparation method and application thereof |
WO2021072818A1 (en) * | 2019-10-15 | 2021-04-22 | 中山大学 | Preparation method for and application of bismuth tungstate-graphene-conductive hydrogel |
CN112371113A (en) * | 2020-12-05 | 2021-02-19 | 常州大学 | Bi2WO6Preparation method and application of-rGO visible light catalyst |
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