CN106975478A - The preparation method of bismuth tungstate/attapulgite composite material - Google Patents
The preparation method of bismuth tungstate/attapulgite composite material Download PDFInfo
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- CN106975478A CN106975478A CN201710159870.7A CN201710159870A CN106975478A CN 106975478 A CN106975478 A CN 106975478A CN 201710159870 A CN201710159870 A CN 201710159870A CN 106975478 A CN106975478 A CN 106975478A
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- Prior art keywords
- attapulgite
- composite material
- bismuth
- tungstate
- bismuth tungstate
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- 229960000892 attapulgite Drugs 0.000 title claims abstract description 33
- 229910052625 palygorskite Inorganic materials 0.000 title claims abstract description 33
- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 29
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 239000002131 composite material Substances 0.000 title claims abstract description 26
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000008367 deionised water Substances 0.000 claims abstract description 12
- 229910021641 deionized water Inorganic materials 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 12
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 claims abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000000227 grinding Methods 0.000 claims abstract description 8
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims abstract 2
- 239000002689 soil Substances 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 6
- 239000006185 dispersion Substances 0.000 abstract description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 abstract description 3
- 239000011707 mineral Substances 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 239000000295 fuel oil Substances 0.000 abstract description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 2
- 239000011593 sulfur Substances 0.000 abstract description 2
- 229910052717 sulfur Inorganic materials 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 26
- 238000013019 agitation Methods 0.000 description 15
- 239000002244 precipitate Substances 0.000 description 10
- 239000003054 catalyst Substances 0.000 description 9
- 239000011259 mixed solution Substances 0.000 description 9
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 6
- 238000009413 insulation Methods 0.000 description 6
- 238000011160 research Methods 0.000 description 6
- 230000003197 catalytic effect Effects 0.000 description 5
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 5
- 238000005303 weighing Methods 0.000 description 5
- 230000015556 catabolic process Effects 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 4
- 239000004927 clay Substances 0.000 description 4
- 238000006731 degradation reaction Methods 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- IYYZUPMFVPLQIF-UHFFFAOYSA-N dibenzothiophene Chemical class C1=CC=C2C3=CC=CC=C3SC2=C1 IYYZUPMFVPLQIF-UHFFFAOYSA-N 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- YTPLMLYBLZKORZ-UHFFFAOYSA-N Thiophene Chemical compound C=1C=CSC=1 YTPLMLYBLZKORZ-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 239000010937 tungsten Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000012876 carrier material Substances 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000002153 concerted effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 238000006477 desulfuration reaction Methods 0.000 description 1
- 230000023556 desulfurization Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000012802 nanoclay Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 229930192474 thiophene Natural products 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
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- 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
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- 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—
-
- B01J35/60—
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G27/00—Refining of hydrocarbon oils in the absence of hydrogen, by oxidation
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/20—Characteristics of the feedstock or the products
- C10G2300/201—Impurities
- C10G2300/202—Heteroatoms content, i.e. S, N, O, P
Abstract
The present invention relates to a kind of preparation method of bismuth tungstate/attapulgite composite material, belong to nonmetallic mineral material finishing technology field.A certain amount of bismuth nitrate, sodium tungstate and attapulgite are taken, is added in deionized water and stirs；It is then transferred into reactor, hydro-thermal reaction, and is incubated；Reaction product is washed and alcohol is washed, drying grinding, obtains bismuth tungstate/attapulgite composite material Bi2WO6/ATP.Bi prepared by the present invention2WO6/ ATP composite Load Balanceds, good dispersion, raw material is easy to get, reproducible without complicated equipment, has very high photocatalytic degradation effect to the thiophenic sulfur in fuel oil.
Description
Technical field
The present invention relates to the preparation method of bismuth tungstate/attapulgite composite material, belong to nonmetallic mineral material finishing
Technical field.
Background technology
In recent years, problem of environmental pollution is increasingly serious, and energy scarcity problem is also extremely urgent.Facing above-mentioned two big crises
Situation under, people expand pollution control, the scientific research of environmental protection.Using semiconductor as catalyst, sunshine is utilized
Catalyzing oxidizing degrading polluter is as a kind of effective pollution administration method, the heat studied as environmental protection science
Point.Under research background as above, various countries research worker have developed a variety of semiconductor nano materials, such as TiO2、ZnO、α-
Fe2O3Deng the improvement for pollutant.With TiO2Exemplified by, although nano-TiO2With very high stability, stronger photocatalysis
Ability, the prominent advantage such as nontoxic pollution-free.But, because titanium dioxide energy gap is 3.2 ev, therefore meaning that TiO2
The incident photon that matching wavelength is less than 387 nm can only be absorbed, light absorbs are only limitted to ultraviolet region, the luminous energy of this wave band
Amount accounts for the 5% of the sunshine for being irradiated to ground.The ratio of visible light part accounts for the 45% of solar energy, and is actually reached earth's surface
Solar radiation energy concentrates on 460~500nm wave-length coverages.Therefore how light-catalyzed reaction efficiently is carried out using natural light,
Exploitation just can increasingly aroused people's interest by the photochemical catalyst of excited by visible light.
In recent years, having focused on for research is found the two-phase gold with different crystal morphology by more research workers
Belong on oxide, by expanding light abstraction width to visible region, to develop novel photocatalyst.Nearest many researchs hair
It is existing, bismuth tungstate (Bi2WO6) it is layer structure, with the characteristic such as dielectric, luminous, catalysis, have well in many association areas
Application prospect.Its unique crystal and electronic structure, shows higher photocatalytic activity, particularly to visible light-responded bright
It is aobvious.In addition, bismuth based semiconductor catalysis material also has the unique advantage to hardly degraded organic substance high catalytic activity.Utilize absorption
The nanoclay of excellent performance carrys out the weight that immobilized semiconductor catalyst is the current dispersiveness and reusing for solving catalyst
Method is wanted, active component is combined with the clay-phase of bigger serface turns into an important development direction of catalytic field.It is recessed
Convex rod native (ATP) is a kind of inexpensive natural minerals, microcosmic upper with one-dimensional layer chain nano pore structure, hydrone and one
Determining the organic molecule of size can directly adsorb in its duct, macroscopically show as big specific surface area and stronger absorption
And ion-exchange performance, attapulgite can be used as a kind of excellent catalyst carrier material.In recent years on recessed soil with partly leading
The report of the material of bluk recombination is more, but is also not seen reported at present on bismuth tungstate and the compound document of recessed soil.
The content of the invention
The purpose of the present invention is：A kind of preparation method of bismuth tungstate/attapulgite composite material is provided, the preparation method institute
The Bi obtained2WO6/ ATP composite Load Balanceds, good dispersion, raw material is easy to get, reproducible without complicated equipment, to combustion
Expect that the thiophenic sulfur in oil product has very high photocatalytic degradation effect.
The present invention technical solution be：A certain amount of bismuth nitrate, sodium tungstate and attapulgite are taken, deionization is added to
Stirred in water；It is then transferred into reactor, hydro-thermal reaction, and is incubated；Reaction product is washed and alcohol is washed, drying grinding, obtains tungsten
Sour bismuth/attapulgite composite material Bi2WO6/ATP。
Wherein, the mol ratio of bismuth nitrate and sodium tungstate is 1:3~1:Between 7, quality of the attapulgite relative to bismuth tungstate
Than for 1:3~1:8.
Wherein, hydrothermal temperature is 180~240 DEG C, and the hydro-thermal reaction time is 16~24h.
Wherein, 60~100 DEG C of 12~24h of insulation after hydro-thermal reaction.
It is an advantage of the invention that：
1st, employ a kind of more easy chemical technology and prepare load more uniform, bismuth tungstate/bumps of good dispersion
Rod stone composite material, without complicated equipment, chemical raw material used is cheap, and favorable repeatability has very high commercial introduction
Value.
2nd, attapulgite itself has abundant microcellular structure and larger specific surface area, has very well to organic matter macromolecular
Adsorption capacity in situ；Attapulgite solid-carried catalyst powder, it is to avoid catalyst powder separation is difficult, the problems such as reclaim difficult.
3rd, the composite prepared by the present invention can catalytic degradation organic pollution, fully profit under the conditions of solar irradiation
With solar energy, this kind of composite has very big potential using value in terms of deep desulfurization of gasoline.
4th, strict control mixing time in bismuth tungstate/bumps rod composite material, course of reaction is prepared using the step of hydro-thermal method one
And temperature, it is to avoid cause the generation of accessory substance because of the difference of mixing time and temperature, it is ensured that the photocatalysis of influence material is lived
Property.
5th, on the one hand catalyst is made to be contacted rapidly, fully with organic matter using the excellent adsorption capacity of attapulgite；It is another
Contain in the recessed soil of aspect after a small amount of calcium, magnesium, iron plasma, Material cladding, the foreign ion in recessed soil enters the lattice of bismuth tungstate
In, cause the defect of lattice to increase, promote the transfer of light induced electron, it is to avoid light induced electron itself it is compound, by carrier with
Concerted catalysis effect between active component, and then largely strengthen the catalytic activity of composite.
6th, with attapulgite, sodium tungstate, bismuth nitrate is primary raw material, is synthesized using hydro-thermal method, concavo-convex by optimizing
The technological parameters such as rod soil and mass ratio, hydrothermal temperature and the hydro-thermal time of bismuth nitrate and sodium tungstate control bismuth tungstate/concave convex rod
The pattern and distribution of composite, so as to obtain the product of Load Balanced, good dispersion.
Brief description of the drawings
Fig. 1 is ATP, Bi of embodiment 12WO6And Bi2WO6/ ATP (Bi2WO6The XRD spectra of/ATP=1/2)；
Fig. 2 is the Bi of embodiment 12WO6/ ATP (Bi2WO6The TEM photos of 100 nm scale ranges of/ATP=1/2)；
Fig. 3 is the Bi of embodiment 12WO6/ATP ((Bi2WO6The degradation curve of/ATP=1/2) to dibenzothiophenes.
Embodiment
Technical scheme is described in further detail with reference to embodiment, but is not to be construed as to technical scheme
Limitation.
Embodiment 1：The bismuth nitrate for weighing 0.17g first is dissolved in 50ml deionized water, and magnetic agitation 30min obtains white
Color solution；0.047g sodium tungstate is added into white solution again, it is molten that continuation magnetic agitation 30min is mixed to get white mixing
Liquid；The attapulgite that 0.2g is added into white mixed solution continues magnetic agitation 10min, obtains faint yellow turbid solution；Will
Faint yellow turbid solution is put into 100ml ptfe autoclaves, 180 DEG C of hydro-thermal reaction 24h；After reaction terminates, in reactor
Lower floor's pale yellow precipitate, upper strata settled solution, 60 DEG C of insulation 24h；Pale yellow precipitate is washed with deionized water, absolute ethyl alcohol,
80 DEG C of drying, grinding obtains bismuth tungstate/concave convex rod nanostructure composite material.
To the gained Bi of embodiment 12WO6/ ATP carries out X-ray powder diffraction experiment, and observes under transmission electron microscope its pattern
And structure, ATP, Bi2WO6And Bi2WO6/ ATP (Bi2WO6The XRD spectra of/ATP=1/2) is as shown in figure 1, composite
Bismuth tungstate and the respective characteristic diffraction peak of attapulgite are occurred in that in XRD, illustrates that attapulgite is successfully combined bismuth tungstate.
The gained Bi of embodiment 12WO6/ ATP TEM photos are as shown in Fig. 2 it can be seen that attapulgite and tungsten
Sour bismuth is more uniformly combined with each other, consistent with XRD result.
Using ATP, Bi2WO6And Bi2WO6/ ATP carries out the thiophene in photochemical catalytic oxidation removing fuel oil as catalyst
Sulphur, is obtained to the degradation rate curve of dibenzothiophenes as shown in figure 3, it can be seen that Bi2WO6/ ATP is to dibenzothiophenes
Degradation rate under illumination 4h is up to more than 98%.
Embodiment 2：The bismuth nitrate for weighing 0.17g first is dissolved in 50ml deionized water, and magnetic agitation 30min obtains white
Color solution；0.05g sodium tungstate is added into white solution again, continues magnetic agitation 30min and is mixed to get white mixed solution；
0.3g attapulgite is added into white mixed solution, continues magnetic agitation 10min, obtains faint yellow turbid solution；Will be light
Yellow turbid solution is put into 100ml ptfe autoclaves, 210 DEG C of hydro-thermal reaction 20h；Reaction terminate after, in reactor under
Layer pale yellow precipitate, upper strata settled solution, 80 DEG C of insulation 18h；Pale yellow precipitate is washed with deionized water, absolute ethyl alcohol, 70
DEG C drying, grinding obtain bismuth tungstate/attapulgite clay nano structural composite material.Subsequent detection such as embodiment 1.
Embodiment 3：The bismuth nitrate for weighing 0.17g first is dissolved in 50ml deionized water, and magnetic agitation 30min obtains white
Color solution；0.06g sodium tungstate is added into white solution again, continues magnetic agitation 30min and is mixed to get white mixed solution；
0.4g attapulgite is added into white mixed solution, continues magnetic agitation 10min, obtains faint yellow turbid solution；Will be light
Yellow turbid solution is put into 100ml ptfe autoclaves, 240 DEG C of hydro-thermal reaction 16h；Reaction terminate after, in reactor under
Layer pale yellow precipitate, upper strata settled solution, 100 DEG C of insulation 24h；Pale yellow precipitate is washed with deionized water, absolute ethyl alcohol, 80
DEG C drying, grinding obtain bismuth tungstate/attapulgite clay nano structural composite material.Subsequent detection such as embodiment 1.
Embodiment 4：The bismuth nitrate for weighing 0.17g first is dissolved in 50ml deionized water, and magnetic agitation 30min obtains white
Color solution；0.07g sodium tungstate is added into white solution again, continues magnetic agitation 30min and is mixed to get white mixed solution；
0.5g attapulgite is added into white mixed solution, continues magnetic agitation 10min, obtains faint yellow turbid solution；Will be light
Yellow turbid solution is put into 100ml ptfe autoclaves, 180 DEG C of hydro-thermal reaction 18h；Reaction terminate after, in reactor under
Layer pale yellow precipitate, upper strata settled solution, 70 DEG C of insulation 16h；Pale yellow precipitate is washed with deionized water, absolute ethyl alcohol, 60
DEG C drying, grinding obtain bismuth tungstate/attapulgite clay nano structural composite material.Subsequent detection such as embodiment 1.
Embodiment 5：The bismuth nitrate for weighing 0.17g first is dissolved in 50ml deionized water, and magnetic agitation 30min obtains white
Color solution；0.07g sodium tungstate is added into white solution again, continues magnetic agitation 30min and is mixed to get white mixed solution；
0.6g attapulgite is added into white mixed solution, continues magnetic agitation 10min, obtains faint yellow turbid solution；Will be light
Yellow turbid solution is put into 100ml ptfe autoclaves, 210 DEG C of hydro-thermal reaction 22h；After reaction terminates, reactor lower floor
Pale yellow precipitate, upper strata settled solution, 90 DEG C of insulation 22h；Pale yellow precipitate is washed with deionized water, absolute ethyl alcohol, 80 DEG C
Drying, grinding obtains bismuth tungstate/attapulgite clay nano structural composite material.Subsequent detection such as embodiment 1.
Claims (4)
1. the preparation method of bismuth tungstate/attapulgite composite material, it is characterized in that：Take a certain amount of bismuth nitrate, sodium tungstate and recessed
Convex rod soil, is added in deionized water and stirs；It is then transferred into reactor, hydro-thermal reaction, and is incubated；Reaction product wash and
Alcohol is washed, drying grinding, obtains bismuth tungstate/attapulgite composite material Bi2WO6/ATP。
2. the preparation method of bismuth tungstate/attapulgite composite material according to claim 1, it is characterized in that：Bismuth nitrate and
The mol ratio of sodium tungstate is 1:3~1:Between 7, attapulgite is 1 relative to the mass ratio of bismuth tungstate:3~1:8.
3. the preparation method of bismuth tungstate/attapulgite composite material according to claim 1, it is characterized in that：Hydro-thermal reaction
Temperature is 180~240 DEG C, and the hydro-thermal reaction time is 16~24h.
4. the preparation method of bismuth tungstate/attapulgite composite material according to claim 1, it is characterized in that：Hydro-thermal reaction
60~100 DEG C are incubated 12~24h afterwards.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN108014799A (en) * | 2017-12-14 | 2018-05-11 | 盱眙县中材凹凸棒石粘土有限公司 | The preparation method of nickel titanate/attapulgite composite material |
| CN114904521A (en) * | 2021-02-09 | 2022-08-16 | 中国建筑材料科学研究总院有限公司 | Au/Bi 2 WO 6 Mineral ternary composite material and preparation method and application thereof |
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| CN105797712A (en) * | 2016-04-07 | 2016-07-27 | 常州大学 | Preparation method of Mo-doped Bi2WO6/MMT (montmorillonite) composite material and application of Mo-doped Bi2WO6/MMT composite material in photocatalytic desulfurization |
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| CN105582909A (en) * | 2015-12-23 | 2016-05-18 | 常州大学 | Preparation method and application of bismuth tungstate/expanded graphite sheet nanocomposite |
| CN105797712A (en) * | 2016-04-07 | 2016-07-27 | 常州大学 | Preparation method of Mo-doped Bi2WO6/MMT (montmorillonite) composite material and application of Mo-doped Bi2WO6/MMT composite material in photocatalytic desulfurization |
Cited By (5)
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| 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 |
| CN108014799A (en) * | 2017-12-14 | 2018-05-11 | 盱眙县中材凹凸棒石粘土有限公司 | The preparation method of nickel titanate/attapulgite composite material |
| CN114904521A (en) * | 2021-02-09 | 2022-08-16 | 中国建筑材料科学研究总院有限公司 | Au/Bi 2 WO 6 Mineral ternary composite material and preparation method and application thereof |
| CN114904521B (en) * | 2021-02-09 | 2024-01-16 | 中国建筑材料科学研究总院有限公司 | Au/Bi 2 WO 6 Mineral ternary composite material, preparation method and application thereof |
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