CN107349927A - A kind of laurustinus tufted bismuth tungstate/charcoal composite photocatalyst material and its preparation method and application - Google Patents
A kind of laurustinus tufted bismuth tungstate/charcoal composite photocatalyst material and its preparation method and application Download PDFInfo
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- CN107349927A CN107349927A CN201710764588.1A CN201710764588A CN107349927A CN 107349927 A CN107349927 A CN 107349927A CN 201710764588 A CN201710764588 A CN 201710764588A CN 107349927 A CN107349927 A CN 107349927A
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- Prior art keywords
- charcoal
- laurustinus
- tufted
- composite photocatalyst
- photocatalyst material
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- 239000003610 charcoal Substances 0.000 title claims abstract description 82
- 239000000463 material Substances 0.000 title claims abstract description 76
- 239000002131 composite material Substances 0.000 title claims abstract description 62
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 58
- 241000673705 Viburnum tinus Species 0.000 title claims abstract description 39
- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 28
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 28
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 238000006243 chemical reaction Methods 0.000 claims abstract description 47
- 239000007788 liquid Substances 0.000 claims abstract description 25
- 239000002243 precursor Substances 0.000 claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000004094 surface-active agent Substances 0.000 claims abstract description 19
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 16
- 238000005406 washing Methods 0.000 claims abstract description 11
- 238000000227 grinding Methods 0.000 claims abstract description 10
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims abstract description 9
- 229910020350 Na2WO4 Inorganic materials 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 3
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 244000276331 Citrus maxima Species 0.000 claims description 27
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 27
- 239000000975 dye Substances 0.000 claims description 26
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 14
- 238000006555 catalytic reaction Methods 0.000 claims description 13
- PPNKDDZCLDMRHS-UHFFFAOYSA-N dinitrooxybismuthanyl nitrate Chemical compound [Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PPNKDDZCLDMRHS-UHFFFAOYSA-N 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 9
- 229910052724 xenon Inorganic materials 0.000 claims description 9
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 9
- 244000144992 flock Species 0.000 claims description 8
- 235000001759 Citrus maxima Nutrition 0.000 claims description 7
- 238000002336 sorption--desorption measurement Methods 0.000 claims description 7
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 6
- MCPLVIGCWWTHFH-UHFFFAOYSA-L methyl blue Chemical compound [Na+].[Na+].C1=CC(S(=O)(=O)[O-])=CC=C1NC1=CC=C(C(=C2C=CC(C=C2)=[NH+]C=2C=CC(=CC=2)S([O-])(=O)=O)C=2C=CC(NC=3C=CC(=CC=3)S([O-])(=O)=O)=CC=2)C=C1 MCPLVIGCWWTHFH-UHFFFAOYSA-L 0.000 claims description 5
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 claims description 5
- 229940012189 methyl orange Drugs 0.000 claims description 5
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 claims description 5
- 229940043267 rhodamine b Drugs 0.000 claims description 5
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 238000011049 filling Methods 0.000 claims description 3
- 230000005855 radiation Effects 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 239000010919 dye waste Substances 0.000 claims description 2
- -1 polytetrafluoroethylene Polymers 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 11
- 230000001699 photocatalysis Effects 0.000 abstract description 10
- 230000000593 degrading effect Effects 0.000 abstract description 3
- 238000006731 degradation reaction Methods 0.000 description 13
- 230000015556 catabolic process Effects 0.000 description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 11
- 229910052799 carbon Inorganic materials 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 10
- 238000013019 agitation Methods 0.000 description 9
- 239000002994 raw material Substances 0.000 description 8
- 239000002351 wastewater Substances 0.000 description 8
- 239000003054 catalyst Substances 0.000 description 7
- 238000003760 magnetic stirring Methods 0.000 description 7
- 238000007789 sealing Methods 0.000 description 7
- 229920000742 Cotton Polymers 0.000 description 6
- 241000219146 Gossypium Species 0.000 description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 6
- 239000003575 carbonaceous material Substances 0.000 description 6
- 238000012856 packing Methods 0.000 description 6
- 239000011734 sodium Substances 0.000 description 6
- 229910052708 sodium Inorganic materials 0.000 description 6
- 239000003643 water by type Substances 0.000 description 6
- 239000002028 Biomass Substances 0.000 description 5
- 238000001816 cooling Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 229910002651 NO3 Inorganic materials 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000000835 fiber Substances 0.000 description 4
- 238000007146 photocatalysis Methods 0.000 description 4
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 4
- 238000013032 photocatalytic reaction Methods 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 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 description 3
- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 238000001338 self-assembly Methods 0.000 description 3
- 238000000862 absorption spectrum Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- HRHBQGBPZWNGHV-UHFFFAOYSA-N azane;bromomethane Chemical compound N.BrC HRHBQGBPZWNGHV-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000010842 industrial wastewater Substances 0.000 description 2
- 229960003742 phenol Drugs 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 230000009257 reactivity Effects 0.000 description 2
- 230000008929 regeneration Effects 0.000 description 2
- 238000011069 regeneration method Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- AISMNBXOJRHCIA-UHFFFAOYSA-N trimethylazanium;bromide Chemical compound Br.CN(C)C AISMNBXOJRHCIA-UHFFFAOYSA-N 0.000 description 2
- 235000017060 Arachis glabrata Nutrition 0.000 description 1
- 244000105624 Arachis hypogaea Species 0.000 description 1
- 235000010777 Arachis hypogaea Nutrition 0.000 description 1
- 235000018262 Arachis monticola Nutrition 0.000 description 1
- 244000283207 Indigofera tinctoria Species 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003093 cationic surfactant Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- DCAYPVUWAIABOU-UHFFFAOYSA-N hexadecane Chemical class CCCCCCCCCCCCCCCC DCAYPVUWAIABOU-UHFFFAOYSA-N 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical group C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 235000020232 peanut Nutrition 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010792 warming Methods 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
-
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0259—Compounds of N, P, As, Sb, Bi
-
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
-
- 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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
-
- 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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
-
- 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
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- 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
- C02F2101/34—Organic compounds containing oxygen
- C02F2101/345—Phenols
-
- 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 present invention relates to a kind of laurustinus tufted bismuth tungstate/charcoal composite photocatalyst material and its preparation method and application, first by charcoal, Bi (NO3)3·5H2O and Na2WO4·2H2O is added in water and is well mixed, and adds surfactant and is well mixed, obtains reaction precursor liquid；Wherein Bi (NO3)3·5H2O、Na2WO4·2H2O, the ratio between charcoal and surfactant is (3~5) mmol：(1~3) mmol：(0.1~0.3) g：(1.2~1.8) mmol；The pH value of reaction precursor liquid is adjusted to 1~3；The reaction precursor liquid for mixing up pH value is subjected to hydro-thermal reaction；Drying and grinding obtains laurustinus tufted bismuth tungstate/charcoal composite photocatalyst material hydro-thermal reaction takes out product washing after terminating after.The present invention can not only reduce cost by introducing charcoal, simplify technique, the photocatalytic activity of material can also be improved, to the good degrading effect of organic pollution.
Description
Technical field
The invention belongs to inorganic functional material field, and in particular to a kind of laurustinus tufted bismuth tungstate/charcoal complex light
Catalysis material and its preparation method and application.
Background technology
With the development of globalization, climate warming and problem of environmental pollution are the great difficult problems that countries in the world are faced, and are opened
It is environment friendly and pollution-free to send out a kind of, cost is cheap, the depollution of environment treatment technology of reusable edible, and turn into researcher one is important
Problem and research direction.
In numerous semi-conducting materials, bismuth tungstate material, can be purple due to narrower energy gap (~2.7eV)
Outer light and excited by visible light, there is photostability, in the absence of photoetch phenomenon, study it utilization for being favorably improved visible ray
Rate.Further to improve its photocatalysis performance, domestic and international researcher is lived by ion doping, immobilized supported, addition surface
Property agent etc., to regulate and control its appearance structure, narrow forbidden band, expands photoresponse scope, so as to realize bismuth tungstate material light catalysis effect
Enhancing.But raw material used in these methods are expensive, preparation technology is complicated, and degradation efficiency still needs to further improve, so as to
Limit the process of industrialization of material.Therefore, raw material use cost is reduced, simplifies preparation technology, it is to determine to improve degradation efficiency
The fixed material can actual popularization and application effective way.
The content of the invention
It is an object of the invention to overcome problems of the prior art, there is provided a kind of laurustinus tufted bismuth tungstate/life
Thing charcoal composite photocatalyst material and its preparation method and application, cost is reduced, simplify technique, the photocatalysis of material obtained by raising
Activity.
In order to achieve the above object, the present invention adopts the following technical scheme that：
Comprise the following steps：
(1) by charcoal, Bi (NO3)3·5H2O and Na2WO4·2H2O is added in water and is well mixed, and adds surface-active
Agent is well mixed, and obtains reaction precursor liquid；Wherein Bi (NO3)3·5H2O、Na2WO4·2H2O, charcoal and surfactant it
Between ratio be (3~5) mmol：(1~3) mmol：(0.1~0.3) g：(1.2~1.8) mmol；
(2) pH value of reaction precursor liquid is adjusted to 1~3；
(3) the reaction precursor liquid for mixing up pH value is subjected to hydro-thermal reaction；
(4) it is multiple to obtain laurustinus tufted bismuth tungstate/charcoal for drying and grinding after taking-up product washs after hydro-thermal reaction terminates
Closing light catalysis material.
Further, for the charcoal in step (1) using pomelo peel charcoal, pomelo peel charcoal is by pomelo peel
The white flock layer of internal layer is peeled to be placed in and is connected with the vacuum tube furnace of Ar gas, carried out at 500 DEG C~800 DEG C calcining 60min~
What 90min was obtained.
Further, the surfactant in step (1) uses CTAB；Bi(NO3)3·5H2The ratio of O and water for (3~
5)mmol：40ml.
Further, concentration is used to adjust reaction precursor for 0.2mol/L~0.8mol/L NaOH solution in step (2)
The pH value of liquid.
Further, hydro-thermal reaction, reaction-filling ratio are carried out in liner is the water heating kettle of polytetrafluoroethylene (PTFE) in step (3)
40%~50%.
Further, heated in the hydro-thermal reaction of step (3) using microwave；Hydrothermal temperature is 180 DEG C~200 DEG C,
The hydro-thermal reaction time is 60min~90min.
Further, product carries out centrifuge washing several times respectively using deionized water and absolute ethyl alcohol in step (4), so
Afterwards 3h is dried in vacuo at 60~80 DEG C.
One kind utilizes laurustinus tufted bismuth tungstate/charcoal composite photocatalyst material made from preparation method as described above.
Laurustinus tufted bismuth tungstate/application of the charcoal composite photocatalyst material in degradating organic dye as described above,
Laurustinus tufted bismuth tungstate/charcoal composite photocatalyst material is added in organic dye waste water first, carries out dark reaction, its
Middle laurustinus tufted bismuth tungstate/mass ratio between charcoal composite photocatalyst material and organic dyestuff is (50~100)：0.5；
After reaching adsorption-desorption balance, then radiation of visible light is carried out, and react 30min~180min, complete the degraded of organic dyestuff.
Further, dark reaction time is 30min~60min；Visible ray uses 500W xenon source, 1000W xenon
Lamp source or sunshine；Organic dyestuff includes the one or more in rhodamine B, methyl orange, methyl blue and phenol.
Compared with prior art, the present invention has technique effect beneficial below：
In the inventive method, by the bigger serface of biomass carbon, flourishing pore structure, wider light absorbs model
Enclose, stable chemical property, and the features such as its stronger power of regeneration and adsorption capacity, using presoma raw material mutually it
Between self assembly effect, for obtain cheap, economically feasible, simple to operate, the high catalytic activity and stability of function admirable
Visible ray conductor photocatalysis material, it is Bi that wherein charcoal, which serves not only as carbon fiber skeleton,2WO6/ biological carbon composite is more
The growth of pass structure serves support and template action, is also greatly improved absorption of the dye molecule on the catalysis material surface
Behavior, more reacting environment and condition are provided for light-catalyzed reaction, meanwhile, charcoal and Bi2WO6It is compound so that
Light induced electron mobility under illumination condition improves, and these factors are advantageous to improve the photocatalytic activity of the composite.This
Invention preparation method is built a kind of using biomass raw material cheap, can be recycled are enriched in nature by hydro-thermal method
Laurustinus tufted Bi2WO6/ charcoal composite photocatalyst material, simple to operate, reaction is gentle, and controllability is strong.
Further, the biological carbon feedstock in the present invention uses pomelo peel, and pomelo peel is that cost is cheap, can circulate profit
With, with stronger power of regeneration and adsorption capacity, the raw material with flourishing pore structure, closed by introducing pomelo peel charcoal
Into the bismuth tungstate biology carbon composite with multistage mesoporous microsphere structure, to improve absorption and increase specific surface area, so as to carry
Its high Photocatalytic Degradation Property.Identical preparation method and application also extend to it is mutually compound with other semi-conducting materials, not only
It is limited only to bismuth tungstate material.
Composite photocatalyst material of the present invention is acted on using self assembly causes charcoal and Bi2WO6It is combined so as to form one kind
Laurustinus tufted appearance structure, cost is cheap, economically feasible.
The present invention can not only reduce cost by introducing the method for biomass carbon, simplify technique, can also improve material
Photocatalytic activity, laurustinus tufted Bi of the present invention2WO6Degradation effect of/charcoal the composite photocatalyst material to organic pollution
Good, degradation rate is at least up to 96.9%.
Further, the present invention can realize the light to rhodamine B, methyl orange, phenol, methyl blue etc. under visible light
Catalytic degradation, it is applied widely.
Brief description of the drawings
Fig. 1 is the Bi prepared in the embodiment of the present invention 1 and comparative example 12WO6/ charcoal composite photocatalyst material XRD spectrum.
Fig. 2 (a) is Bi prepared by the embodiment of the present invention 12WO6/ charcoal composite photocatalyst material SEM schemes；Fig. 2 (b) is pair
The Bi prepared in ratio 12WO6/ charcoal composite photocatalyst material SEM schemes.
Fig. 3 is the Bi prepared in the embodiment of the present invention 1 and comparative example 12WO6/ charcoal composite photocatalyst material it is ultraviolet-
It can be seen that-diffusing reflection absorption spectrum.
Fig. 4 is the Bi prepared in the embodiment of the present invention and comparative example2WO6The visible ray of/charcoal composite photocatalyst material is urged
Change degradation curve figure.
Embodiment
The present invention is described in further details below in conjunction with the accompanying drawings.
The invention provides a kind of to environment non-secondary pollution, cheap stable, the high laurustinus tufted of photocatalytic activity
Bi2WO6The preparation method of/charcoal composite photocatalyst material, obtained material can enter in being degraded to industrial wastewater dyestuff
Row application.
Preparation method of the present invention comprises the following steps：
(1) the white flock layer of shaddock endo-endothelial layer is peeled to be put into and is connected with the vacuum tube furnace of Ar gas, 500 DEG C~
Calcining 60min~90min is carried out in the range of 800 DEG C, carbonizes pomelo peel, obtains pomelo peel biological carbon materials.
(2) by charcoal, pure bismuth nitrate (Bi (NO are analyzed3)3·5H2) and sodium tungstate (Na O2WO4·2H2O), be dissolved in from
Magnetic agitation makes it fully dissolve in the beaker of sub- water, rear to add surfactant cetyl trimethylammonium bromide (CTAB),
Continue ultrasonic agitation dissolving；Presoma raw material Bi (NO3)3·5H2O、Na2WO4·2H2O, the ratio between charcoal, CTAB
For (3~5) mmol：(1~3) mmol：(0.1~0.3) g：(1.2~1.8) mmol；Bi(NO3)3·5H2The ratio of O and water is
(3~5) mmol：40ml.
(3) NaOH solution for being 0.2mol/L~0.8mol/L with concentration after adjust reaction precursor liquid pH value range to 1~
3。
(4) above-mentioned reaction precursor liquid is fitted into polytetrafluoroethyllining lining, sealing reaction water heating kettle, is put into magnetic stirring
In microwave reaction instrument, reaction-filling, to 40%~50%, reaction 60min~90min is carried out at 180 DEG C~200 DEG C than control.
(5) after naturally cool to room temperature after the completion of reacting, take out sample and carried out respectively using deionized water and absolute ethyl alcohol
Centrifuge washing for several times, 3h is dried in vacuo at 60~80 DEG C, obtains block aggregation, then is obtained after block aggregation is pulverized
To Bi2WO6/ charcoal composite photocatalyst material.
The laurustinus tufted Bi of the present invention2WO6/ charcoal composite photocatalyst material in industrial wastewater to dyestuff purification at
The application of reason, the photocatalytic degradation to rhodamine B, methyl orange, phenol, methyl blue etc. can be realized under visible light.
Its application process is：By 50~100mg Bi2WO6/ charcoal composite photocatalyst material is added to 50ml concentration
In 10mg/L rhdamine B, light-catalyzed reaction is carried out under the irradiation of visible ray, first carry out dark reaction 30min~
60min, after reaching adsorption-desorption balance, Visible Light Induced Photocatalytic reaction is carried out to it, reaction carries out 30min~180min, completion pair
The degraded purified treatment of waste water from dyestuff.Visible ray uses 500W or 1000W xenon source, or is directly put under sunshine and carries out
Irradiation.
Dyestuff in waste water from dyestuff includes a variety of different organic compounds, such as rhodamine B, methyl orange, methyl blue, phenol
Deng.
Embodiment 1
Laurustinus tufted Bi of the present invention2WO6/ charcoal composite photocatalyst material be using pomelo peel as biomass carbon raw material,
With cationic surfactant cetyl trimethylammonium bromide (CTAB) for carrier or template, by with bismuth nitrate (Bi
(NO3)3·5H2) and sodium tungstate (Na O2WO4·2H2O the interaction between) carries out self assembly and formed with abundant porous knot
A kind of laurustinus tufted Bi of structure feature2WO6/ charcoal composite photocatalyst material.
Wherein, the ratio between bismuth nitrate, sodium tungstate, charcoal and CTAB is 4mmol:2mmol:0.2g:1.6mmol.
A kind of laurustinus tufted Bi2WO6The preparation method of/charcoal composite photocatalyst material, comprises the following steps：
(1) it is that internal layer white fiber peels and is put into the vacuum tube furnace for being connected with Ar gas by the white flock layer of shaddock endo-endothelial layer
In 60min is calcined at 800 DEG C, obtain pomelo peel biological carbon materials after cooling.
(2) 0.2g charcoals, 4mmol bismuth nitrates and 2mmol sodium tungstates are weighed respectively, are dissolved in the beaker of 40ml deionized waters
Middle magnetic agitation makes it fully dissolve, and obtains dark brown solution, after add 1.6mmol surfactants cetyl three thereto
Methyl bromide ammonium, continue that abundant dissolving is stirred by ultrasonic.
(3) precursor liquid pH value is adjusted to 2 with 0.5mol/L NaOH solution afterwards.
(4) above-mentioned reaction precursor liquid is fitted into polytetrafluoroethyllining lining, sealing reaction water heating kettle, is put into magnetic stirring
Microwave hydrothermal reaction is carried out in microwave reaction instrument MDS-10, condition is to react 60min, packing ratio 40% at 200 DEG C.
(5) after naturally cool to room temperature after the completion of reacting, take out sample centrifuge washing for several times, be dried in vacuo at 60 DEG C
3h, Bi is obtained after grinding2WO6/ charcoal composite photocatalyst material.
Comparative example 1
A kind of Bi2WO6The preparation method of/charcoal composite photocatalyst material, comprises the following steps：
(1) the white flock layer of shaddock endo-endothelial layer is peeled to be put into be connected with the vacuum tube furnace of Ar gas and forged at 800 DEG C
60min is burnt, obtains pomelo peel biological carbon materials after cooling.
(2) 0.2g charcoals, 4mmol bismuth nitrates and 2mmol sodium tungstates are weighed respectively, are dissolved in the beaker of 40ml deionized waters
Middle magnetic agitation makes it fully dissolve, after be added without any surfactant, continue that abundant dissolving is stirred by ultrasonic.
(3) precursor liquid pH value is adjusted to 2 with 0.5mol/L NaOH solution.
(4) above-mentioned reaction precursor liquid is fitted into polytetrafluoroethyllining lining, sealing reaction water heating kettle, is put into magnetic stirring
Reacted in microwave reaction instrument MDS-10, condition is to react 60min, packing ratio 40% at 200 DEG C.
(5) after naturally cool to room temperature after the completion of reacting, take out sample centrifuge washing for several times, be dried in vacuo at 60 DEG C
3h, Bi is obtained after grinding2WO6/ charcoal composite photocatalyst material.
Comparative example 2
A kind of Bi2WO6The preparation method of/charcoal composite photocatalyst material, comprises the following steps：
(1) put it into be connected with the vacuum tube furnace of Ar gas and calcined at 800 DEG C as biomass carbon source using cotton
60min, cotton charcoal is obtained after grinding to be cooled.
(2) the 0.5g charcoals, 12mmol bismuth nitrates and 5.8mmol sodium tungstates are weighed respectively, are dissolved in 40ml deionized waters
Beaker in magnetic agitation and ultrasonic agitation it is fully dissolved.
(3) precursor liquid pH value is adjusted to 7 with 0.5mol/L NaOH solution.
(4) above-mentioned reaction precursor liquid is fitted into polytetrafluoroethyllining lining, sealing reaction water heating kettle, is put into magnetic stirring
Reacted in microwave reaction instrument MDS-10, condition is to react 60min, packing ratio 40% at 200 DEG C.
(5) after naturally cool to room temperature after the completion of reacting, take out sample centrifuge washing for several times, be dried in vacuo at 60 DEG C
3h, the Bi is obtained after grinding2WO6/ charcoal composite photocatalyst material.
To the laurustinus tufted Bi prepared in embodiment 12WO6Prepared in/charcoal composite photocatalyst material and comparative example 1
Bi2WO6/ charcoal composite photocatalyst material carries out XRD analysis.Reference picture 1, it is pure orthorhombic phase to add CTAB gained samples
Bi2WO6Structure, corresponding with standard card JCPDS Card No.79-2381, diffraction maximum is smooth sharp, good crystallinity.And do not have
Have and add Bi obtained by surfactant2WO6The diffraction peak intensity of/charcoal is weaker, shows the crystallinity of the sample not as adding
The good crystallinity of sample obtained by CTAB.
To the laurustinus tufted Bi prepared in embodiment 12WO6Prepared in/charcoal composite photocatalyst material and comparative example 1
Bi2WO6/ charcoal composite photocatalyst material carries out sem analysis.Reference picture 2 (a), to add laurustinus tufted made from CTAB
Bi2WO6The SEM figures of/charcoal composite photocatalyst material, Fig. 2 (b) are not add Bi made from activating agent2WO6/ charcoal is compound
The SEM of catalysis material schemes, and the pattern of gained sample is porous silk ball floriform appearance after addition CTAB, mutual by many sheets
Staggeredly grow and formed, the petal arrangement of laminated structure is close, forms abundant pore morphology rule, is advantageous to absorbing and storing space
Formation, can for photocatalytic degradation react more reactivity sites are provided.
To the laurustinus tufted Bi prepared in embodiment 12WO6Prepared in/charcoal composite photocatalyst material and comparative example 1
Bi2WO6/ charcoal composite photocatalyst material carries out ultraviolet-visible-diffusing reflection absorption spectrum and analyzed.Reference picture 3, add
Prepared laurustinus tufted Bi after Surfactant CTAB2WO6Absorption of/charcoal the composite photocatalyst material in visible region
Ability strengthens, and uniform pickup phenomenon be present, the Bi without adding surfactant2WO6The visible ray of/biological carbon composite
Absorbability is weaker.
To the laurustinus tufted Bi prepared in embodiment 12WO6/ charcoal composite photocatalyst material, comparative example 1 and comparative example
The Bi prepared in 22WO6It is anti-that/charcoal composite photocatalyst material carries out catalytic degradation under the irradiation of 1000W xenon lamps simulated visible light
Should.
50mg two kinds of composite photocatalyst materials are added separately in the rhdamine B that 50ml concentration is 10mg/L,
Light-catalyzed reaction is carried out under the irradiation of visible ray, first carries out dark reaction 60min, after reaching adsorption-desorption balance, it is carried out
Visible Light Induced Photocatalytic reacts, and reaction carries out 180min, completes the degraded purified treatment to waste water from dyestuff.
Reference picture 4, have 4 degradation curves in figure, represent respectively no added catalyst (i.e. simple organic dyestuff), not plus
Enter the BWO/ pomelo peel biology product chars obtained by surfactant as catalyst, the BWO/ cottons for using cotton to be prepared for carbon source
Peanut thing product char is as laurustinus tufted BWO/ pomelo peels biology resulting after catalyst and addition surfactant CTAB
When product char is as catalyst, the photocatalysis performance of each sample is characterized.Find out in figure：Not degrading substantially without catalyst, adopts
By the use of cotton be BWO/ cotton biology product chars prepared by carbon source and BWO/ pomelo peel biology product chars that pomelo peel is carbon source as
The time of catalyst degradation is longer, less efficient.However, the flower-shaped sample of silk ball obtained by after adding CTAB is through radiation of visible light
After 180min, 96.9% has been reached to the degradation efficiency of rhdamine B, has shown that the material can complete the degraded to waste water from dyestuff
Purified treatment.It is preferably also in the absorption property of the cloudy, turbid phase sample, abundant porous pattern that may be formed is relevant,
The organic dye molecule that exists for of abundant pore morphology rule provides more contact area with catalyst, is carried for light-catalyzed reaction
For more reactivity sites.
Embodiment 2
(1) it is that internal layer white fiber peels and is put into the vacuum tube furnace for being connected with Ar gas by the white flock layer of shaddock endo-endothelial layer
In 90min is calcined at 500 DEG C, obtain pomelo peel biological carbon materials after cooling.
(2) 0.1g charcoals, 3mmol bismuth nitrates and 1mmol sodium tungstates are weighed respectively, are dissolved in the beaker of 40ml deionized waters
Middle magnetic agitation makes it fully dissolve, and obtains dark brown solution, after add 1.2mmol surfactants cetyl three thereto
Methyl bromide ammonium, continue that abundant dissolving is stirred by ultrasonic.
(3) precursor liquid pH value is adjusted to 1 with 0.2mol/L NaOH solution afterwards.
(4) above-mentioned reaction precursor liquid is fitted into polytetrafluoroethyllining lining, sealing reaction water heating kettle, is put into magnetic stirring
Microwave hydrothermal reaction is carried out in microwave reaction instrument MDS-10, condition is to react 90min, packing ratio 45% at 180 DEG C.
(5) after naturally cool to room temperature after the completion of reacting, take out sample centrifuge washing for several times, be dried in vacuo at 70 DEG C
3h, Bi is obtained after grinding2WO6/ charcoal composite photocatalyst material.
(6) by 60mg obtained Bi2WO6/ charcoal composite photocatalyst material is added to the first that 50ml concentration is 10mg/L
In base orange dyestuff, light-catalyzed reaction is carried out under the irradiation of 500W xenon lamp simulated visible lights, dark reaction 40min is first carried out, reaches
After adsorption-desorption balance, Visible Light Induced Photocatalytic reaction is carried out to it, reaction carries out 100min, and the degraded completed to waste water from dyestuff is net
Change is handled, and degradation efficiency has reached 97.2%.
Embodiment 3
(1) it is that internal layer white fiber peels and is put into the vacuum tube furnace for being connected with Ar gas by the white flock layer of shaddock endo-endothelial layer
In 80min is calcined at 600 DEG C, obtain pomelo peel biological carbon materials after cooling.
(2) 0.3g charcoals, 3.5mmol bismuth nitrates and 1.5mmol sodium tungstates are weighed respectively, are dissolved in 40ml deionized waters
Magnetic agitation makes it fully dissolve in beaker, obtains dark brown solution, after add 1.8mmol surfactant hexadecanes thereto
Base trimethylammonium bromide, continue that abundant dissolving is stirred by ultrasonic.
(3) precursor liquid pH value is adjusted to 3 with 0.8mol/L NaOH solution afterwards.
(4) above-mentioned reaction precursor liquid is fitted into polytetrafluoroethyllining lining, sealing reaction water heating kettle, is put into magnetic stirring
Microwave hydrothermal reaction is carried out in microwave reaction instrument MDS-10, condition is to react 75min, packing ratio 50% at 190 DEG C.
(5) after naturally cool to room temperature after the completion of reacting, take out sample centrifuge washing for several times, be dried in vacuo at 80 DEG C
3h, Bi is obtained after grinding2WO6/ charcoal composite photocatalyst material.
(6) by 80mg obtained Bi2WO6/ charcoal composite photocatalyst material is added to the first that 50ml concentration is 10mg/L
In base indigo plant dyestuff, light-catalyzed reaction is carried out under the irradiation of 500W xenon lamp simulated visible lights, dark reaction 35min is first carried out, reaches
After adsorption-desorption balance, Visible Light Induced Photocatalytic reaction is carried out to it, reaction carries out 50min, completes the degraded purification to waste water from dyestuff
Processing, degradation efficiency have reached 98.3%.
Embodiment 4
(1) it is that internal layer white fiber peels and is put into the vacuum tube furnace for being connected with Ar gas by the white flock layer of shaddock endo-endothelial layer
In 70min is calcined at 700 DEG C, obtain pomelo peel biological carbon materials after cooling.
(2) 0.25g charcoals, 5mmol bismuth nitrates and 3mmol sodium tungstates are weighed respectively, are dissolved in the burning of 40ml deionized waters
Cup in magnetic agitation it is fully dissolved, obtain dark brown solution, after add 1.5mmol surfactant cetyls thereto
Trimethylammonium bromide, continue that abundant dissolving is stirred by ultrasonic.
(3) precursor liquid pH value is adjusted to 2.5 with 0.6mol/L NaOH solution afterwards.
(4) above-mentioned reaction precursor liquid is fitted into polytetrafluoroethyllining lining, sealing reaction water heating kettle, is put into magnetic stirring
Microwave hydrothermal reaction is carried out in microwave reaction instrument MDS-10, condition is to react 80min, packing ratio 50% at 185 DEG C.
(5) after naturally cool to room temperature after the completion of reacting, take out sample centrifuge washing for several times, be dried in vacuo at 75 DEG C
3h, Bi is obtained after grinding2WO6/ charcoal composite photocatalyst material.
(6) by 100mg obtained Bi2WO6It is 10mg/L's that/charcoal composite photocatalyst material, which is added to 50ml concentration,
In phenol dyestuff, light-catalyzed reaction is carried out under the irradiation of 1000W xenon lamp simulated visible lights, dark reaction 30min is first carried out, reaches
After adsorption-desorption balance, Visible Light Induced Photocatalytic reaction is carried out to it, reaction carries out 30min, completes the degraded purification to waste water from dyestuff
Processing, degradation efficiency have reached 99.0%.
The present invention has good visible light photocatalytic degradation performance, the party for the organic dyestuff in environmental wastewater of degrading
Method is simple, it is gentle, the cost of raw material can be substantially reduced, improve photocatalytic activity, there is market potential application value.
Above example is only the preferred embodiment of the present invention, and protection scope of the present invention is not restricted to above-mentioned reality
Example is applied, every technical scheme belonged under thinking of the present invention belongs to protection scope of the present invention.It is worthy of note that for this
For the those of ordinary skill of technical field, the improvement done under the premise without departing from the principles of the invention also should be regarded as the present invention
Protection domain.
Claims (10)
- A kind of 1. preparation method of laurustinus tufted bismuth tungstate/charcoal composite photocatalyst material, it is characterised in that：Including following Step：(1) by charcoal, Bi (NO3)3·5H2O and Na2WO4·2H2O is added in water and is well mixed, and adds surfactant and mixes Close uniformly, obtain reaction precursor liquid；Wherein Bi (NO3)3·5H2O、Na2WO4·2H2O, between charcoal and surfactant Ratio is (3~5) mmol：(1~3) mmol：(0.1~0.3) g：(1.2~1.8) mmol；(2) pH value of reaction precursor liquid is adjusted to 1~3；(3) the reaction precursor liquid for mixing up pH value is subjected to hydro-thermal reaction；(4) drying and grinding obtains laurustinus tufted bismuth tungstate/charcoal complex light after product washing is taken out after hydro-thermal reaction terminates Catalysis material.
- 2. a kind of preparation method of laurustinus tufted bismuth tungstate/charcoal composite photocatalyst material according to claim 1, It is characterized in that：For charcoal in step (1) using pomelo peel charcoal, pomelo peel charcoal is by shaddock endo-endothelial layer White flock layer is peeled to be placed in and is connected with the vacuum tube furnace of Ar gas, and carrying out calcining 60min~90min at 500 DEG C~800 DEG C obtains Arrive.
- 3. a kind of preparation method of laurustinus tufted bismuth tungstate/charcoal composite photocatalyst material according to claim 1, It is characterized in that：Surfactant in step (1) uses CTAB；Bi(NO3)3·5H2The ratio of O and water is (3~5) mmol： 40ml。
- 4. a kind of preparation method of laurustinus tufted bismuth tungstate/charcoal composite photocatalyst material according to claim 1, It is characterized in that：Concentration is used to adjust the pH of reaction precursor liquid for 0.2mol/L~0.8mol/L NaOH solution in step (2) Value.
- 5. a kind of preparation method of laurustinus tufted bismuth tungstate/charcoal composite photocatalyst material according to claim 1, It is characterized in that：Hydro-thermal reaction is carried out in liner is the water heating kettle of polytetrafluoroethylene (PTFE) in step (3), reaction-filling ratio is 40% ~50%.
- 6. a kind of preparation method of laurustinus tufted bismuth tungstate/charcoal composite photocatalyst material according to claim 1, It is characterized in that：Heated in the hydro-thermal reaction of step (3) using microwave；Hydrothermal temperature is 180 DEG C~200 DEG C, and hydro-thermal is anti- It is 60min~90min between seasonable.
- 7. a kind of preparation method of laurustinus tufted bismuth tungstate/charcoal composite photocatalyst material according to claim 1, It is characterized in that：Product carries out centrifuge washing several times respectively using deionized water and absolute ethyl alcohol in step (4), then 60 3h is dried in vacuo at~80 DEG C.
- 8. one kind utilizes laurustinus tufted bismuth tungstate made from preparation method described in claim 1/charcoal composite photocatalyst material Material.
- 9. laurustinus tufted bismuth tungstate/charcoal composite photocatalyst material as claimed in claim 8 is in degradating organic dye Using, it is characterised in that：Laurustinus tufted bismuth tungstate/charcoal composite photocatalyst material is added to organic dye waste water first In, carry out the mass ratio of dark reaction, wherein laurustinus tufted bismuth tungstate/between charcoal composite photocatalyst material and organic dyestuff For (50~100)：0.5；After reaching adsorption-desorption balance, then radiation of visible light is carried out, and react 30min~180min, completed The degraded of organic dyestuff.
- 10. laurustinus tufted bismuth tungstate/charcoal composite photocatalyst material is in degradating organic dye according to claim 9 Application, it is characterised in that：Dark reaction time is 30min~60min；Visible ray uses 500W xenon source, 1000W xenon Lamp source or sunshine；Organic dyestuff includes the one or more in rhodamine B, methyl orange, methyl blue and phenol.
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| CN111450819A (en) * | 2020-04-27 | 2020-07-28 | 成都信息工程大学 | Biochar modified bismuth vanadate catalyst, preparation method and application thereof |
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Application publication date: 20171117 |