CN105562040A - Preparation and application of BiOCl-(001)/GO nano-composite photocatalyst - Google Patents
Preparation and application of BiOCl-(001)/GO nano-composite photocatalyst Download PDFInfo
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- CN105562040A CN105562040A CN201610021421.1A CN201610021421A CN105562040A CN 105562040 A CN105562040 A CN 105562040A CN 201610021421 A CN201610021421 A CN 201610021421A CN 105562040 A CN105562040 A CN 105562040A
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- 239000002114 nanocomposite Substances 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title claims abstract description 45
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 29
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 36
- 238000003756 stirring Methods 0.000 claims abstract description 36
- 239000013078 crystal Substances 0.000 claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- 239000008367 deionised water Substances 0.000 claims abstract description 20
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 20
- 239000011780 sodium chloride Substances 0.000 claims abstract description 18
- 230000000694 effects Effects 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000005406 washing Methods 0.000 claims abstract description 6
- 239000002131 composite material Substances 0.000 claims abstract description 5
- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 claims abstract 2
- 239000000463 material Substances 0.000 claims description 30
- 239000003054 catalyst Substances 0.000 claims description 18
- 239000004567 concrete Substances 0.000 claims description 13
- 239000002055 nanoplate Substances 0.000 claims description 10
- 239000013049 sediment Substances 0.000 claims description 9
- 150000001875 compounds Chemical class 0.000 claims description 8
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 6
- 238000005119 centrifugation Methods 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 6
- 239000005457 ice water Substances 0.000 claims description 6
- 239000012265 solid product Substances 0.000 claims description 4
- 238000007865 diluting Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 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 3
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 3
- 239000006228 supernatant Substances 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 239000000376 reactant Substances 0.000 claims description 2
- 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 abstract description 18
- 229940012189 methyl orange Drugs 0.000 abstract description 18
- 230000003197 catalytic effect Effects 0.000 abstract description 8
- 238000005516 engineering process Methods 0.000 abstract description 8
- 230000000593 degrading effect Effects 0.000 abstract description 2
- 229910021389 graphene Inorganic materials 0.000 abstract description 2
- BCKXLBQYZLBQEK-KVVVOXFISA-M Sodium oleate Chemical compound [Na+].CCCCCCCC\C=C/CCCCCCCC([O-])=O BCKXLBQYZLBQEK-KVVVOXFISA-M 0.000 abstract 2
- 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 abstract 2
- 238000001816 cooling Methods 0.000 abstract 1
- 230000015556 catabolic process Effects 0.000 description 13
- 238000006731 degradation reaction Methods 0.000 description 13
- 230000001699 photocatalysis Effects 0.000 description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 11
- 238000000034 method Methods 0.000 description 8
- 239000007864 aqueous solution Substances 0.000 description 7
- 238000007146 photocatalysis Methods 0.000 description 7
- 239000000243 solution Substances 0.000 description 6
- -1 fully stir Chemical compound 0.000 description 5
- 239000002244 precipitate Substances 0.000 description 5
- 239000010410 layer Substances 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 230000001678 irradiating effect Effects 0.000 description 2
- 239000002159 nanocrystal Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 238000000103 photoluminescence spectrum Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 230000003595 spectral effect Effects 0.000 description 2
- 239000002344 surface layer Substances 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 125000001309 chloro group Chemical group Cl* 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000002355 dual-layer Substances 0.000 description 1
- 230000005685 electric field effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 238000001782 photodegradation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/06—Halogens; Compounds thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/20—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state
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- 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
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- 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
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract
The invention discloses preparation and application of a BiOCl-(001)/GO nano-composite photocatalyst and belongs to the field of photocatalysts. The active component of the composite photocatalyst is BiOCl-(001)/GO. The BiOCl-(001)/GO composite photocatalyst is characterized in that the crystal surface engineering technology and an electronic extracting effect are combined, GO and a BiOCl monocrystal nano-piece of an exposure face (001) are recombined, and the BiOCl-(001)/GO nano-composite photocatalyst is prepared. The preparation method comprises the steps that NaCl and sodium oleate are put into a round-bottom flask, deionized water is added, sufficient stirring is conducted to enable sodium oleate and NaCl to be dissolved fully, graphene is added, constant-temperature stirring is conducted, Bi(NO3)3 is added slowly, cooling, washing and drying are conducted after a reaction is carried out for a certain time, and then the target product is obtained. The prepared nano-composite photocatalyst can be applied to a reaction of degrading methyl orange, and a good catalytic effect and stability are achieved.
Description
Technical field
The invention belongs to photochemical catalyst field, be specifically related to a kind of technology of preparing containing bismoclite (BiOCl) and Graphene (GO) composite photo-catalyst, particularly one contains the technology of preparing of composite photo-catalyst BiOCl-(the 001)/GO of the BiOCl single crystal nanoplate (BiOCl-(001)) in GO and exposure (001) face.The present invention utilizes plane of crystal engineering and electronics stripping effect to combine, and has prepared nano composite photo-catalyst BiOCl-(001)/GO, and achieves good catalytic effect for Photodegradation of Methyl Orange (MO).
Background technology
Environmental problem and energy problem are 21 century two challenging greatly of facing of human kind sustainable development.The Photocatalitic Technique of Semiconductor of clean solar energy resources can be utilized to become one of this two important means challenged greatly of reply (H.Wang, etal.Semiconductorheterojunctionphotocatalysts:design, construction, andphotocatalyticperformances, Chem.Soc.Rev., 2014,43,5234-5244.).Wherein BiOCl shows very excellent photocatalysis performance owing to itself having unique layer structure and suitable energy gap, its higher stability and the excellent characteristic such as nontoxic determine that it has great application prospect in photocatalysis field (S.Bai, etal.TowardEnhancedPhotocatalyticOxygenEvolution:Synerge ticUtilizationofPlasmonicEffectandSchottkyJunctionviaInt erfacingFacetSelection, Adv.Mater.2015,27,3444 – 3452.).
The atomic structure of plane of crystal and crystals phase and electronic structure ubiquity difference, and then produce different physicochemical properties, and the surface characteristic of crystal (such as the character such as Surface Layer Atomic Structure, surface state), plays vital effect usually in the physical and chemical performance of performance crystal self.The surface of photochemical catalyst is the main place of carrying out light-catalyzed reaction, and some microdefects on its surface can affect the transport of surface electronic.In addition, surface state is usually present in the outer surface of semiconductor functional material, especially there is highdensity all kinds of surface state in nano material, its surface state plays by catching photogenerated charge the window role (B.Klahr being separated photo-generate electron-hole and realizing photoelectric activity in photoelectrocatalysis process, etal.WaterOxidationatHematitePhotoelectrodes:TheRoleofSu rfaceStates, J.Am.Chem.Soc., 2012,134,4294-4302.).The crystal structure of BiOCl is the two Cl along c-axis direction
-sheath and [Bi
2o
2]
2+the layer structure that layer is staggered, and closed by more weak Van der Waals bond by Cl atom between the Cl atomic layer of dual layer arrangement, crystal is easily caused to dissociate on [001] direction, thus can prepare and there is the BiOCl that different crystal face is master, such as (the J.Jiang such as Jiang, etal., SynthesisandFacet-DependentPhotoreactivityofBiOClSingle-CrystallineNanosheets, J.Am.Chem.Soc., 2012, 134, water heat transfer 4473-4476) is utilized to expose the BiOCl single crystal nanoplate in (001) face and (010) face, and the reason of (010) crystal face is better than from the photocatalysis performance that Surface Layer Atomic Structure and internal electric field effect two aspect explain BiOCl (001) face.Correlative study is thought (S.Bai, etal., Steeringchargekineticsinphotocatalysis:intersectionofmat erialssyntheses, characterizationtechniquesandtheoreticalsimulations, Chem.Soc.Rev., 2015, 44, BiOCl nanocrystal inside 2893-2939.) exposing (001) face exists between magnetic field and different crystal face and there is potential difference, play the effect being separated photo-generate electron-hole, namely electronics flows to electronegative potential, vacancy flows to high potential, thus be conducive to the photocatalytic activity improving BiOCl.But the gathering of electronics can weaken the potential difference between the magnetic field of nanocrystal inside and different crystal face, thus is unfavorable for the separation of electron-hole, therefore, only relies on the surface engineering technology of crystal to be limited to improve the photocatalytic activity of BiOCl.In order to improve the photocatalytic activity of BiOCl further, the electronics of above-mentioned gathering just must be made to consume rapidly.
GO is one of important material with carbon element, has much excellent character, and such as specific area is large, and heat endurance is high, and conductive capability is strong, is widely used in the various fields comprising photocatalysis.This patent is attempted to introduce GO in the process of preparation BiOCl-(001), due to the electric conductivity that GO is good, the electronics of gathering is extracted out in time, thus promote that electric charge is separated with hole, namely plane of crystal engineering and electronics stripping effect is utilized to combine, prepare nano composite photo-catalyst BiOCl-(001)/GO, improve its photocatalysis performance further.
Summary of the invention
For overcoming the deficiencies in the prior art, the object of the invention is to provide a kind of method utilizing plane of crystal engineering and electronics stripping effect to combine, prepare nano composite photo-catalyst BiOCl-(001)/GO, obtain good effect to BiOCl-(the 001)/GO nano composite material prepared with the present invention as photocatalyst for degrading MO.
In order to realize above-mentioned technical purpose, the present invention is achieved by the following technical programs.
The invention provides a kind of BiOCl-(001)/GO nano composite material, its active component is BiOCl-(001)/GO, be characterized in the method utilizing plane of crystal engineering and electronics stripping effect to combine, GO is introduced in the process of preparation BiOCl-(001) single crystal nanoplate, BiOCl-(001) single crystal nanoplate is grown in GO nanometer sheet, form compound nanometer photocatalyst, its concrete preparation process is as follows:
(1) 0.5g graphite powder and 1.5gKMnO
4join in the round-bottomed flask that the 12mL concentrated sulfuric acid is housed, ice-water bath condition lower magnetic force stirs 4h, is heated to 35 DEG C, constant temperature stirs 30min, dropwise adds 23mL distilled water, is warming up to 98 DEG C, stir 15min, this mixture is transferred in ice-water bath, adds 70mL distilled water diluting, add the hydrogen peroxide of 10mL30% again, stir 30min, solution becomes yellow, centrifugation, lower sediment thing, to supernatant liquor pH=7, is drying to obtain GO by abundant washing.
(2) take sodium chloride 116mg, enuatrol 0-200mg, add 30mL deionized water, abundant stirring, makes enuatrol and NaCl fully dissolve, and adds the GO that 0-40mg step (1) obtains, stir 2h, in round-bottomed flask, slowly add the 0.1-0.5mol/LBi (NO of 2mL
3)
3, and in the lower reaction of 95 DEG C of degree 3 hours, reactant is cooled to room temperature, centrifugation, washing, obtain solid product after drying, this solid product was BiOCl-(001)/GO nano composite material.
By adjustment NaOA, GO and Bi (NO
3)
3the preparation conditions such as the consumption of solution can the pattern of control BiOCl-(001)/GO nano composite material, dispersiveness and size.Be 15mg, Bi (NO when enuatrol is 200mg, GO
3)
3during for 0.5mol/L, BiOCl-(001) nanometer sheet can be dispersed in GO nanometer sheet uniformly, the nano-photocatalyst of formation sheet-sheet compound.
BiOCl-(001)/GO nano composite material prepared by the present invention can be used as photochemical catalyst for the MO that degrades, and shows good catalytic effect.BiOCl-prepared by the present invention (001)/GO nano-composite catalyst for reaction condition during light degradation MO is: concentration is 10mgmL
-1mO aqueous solution 10mL, catalyst amount is 30mg, and LED (30W) is light source, and when irradiation time is 120min, the degradation rate of MO reaches 87%.In addition, this catalyst also has good stability, and the above-mentioned MO aqueous solution of catalytic degradation, continuous circulation 3 times, degradation rate still can reach about 82%.
Compared with prior art, the present invention has following technique effect:
(1) take water as solvent, the preparation method of catalyst is simple, and preparation temperature is low.
BiOCl-(001)/GO Nano-composite materials process is simple.Be solvent with water, being raw material with NaCl, take NaOA as surfactant, makes the two be dissolved in water first at a certain temperature, then adds GO, Bi (NO
3)
3, at 90 DEG C, react 3h, just obtain BiOCl-(001)/GO nano composite material.
(2) combine with plane of crystal engineering and electronics stripping effect, catalytic efficiency is high, and catalytic stability is good.
For the reaction of degraded MO, when catalyst amount is 30mg, LED is light source, and when irradiation time is 120min, the degradation rate of rhodamine is 87%.The catalytic degradation MO aqueous solution, continuous circulation 3 times, degradation rate does not significantly reduce.
Accompanying drawing explanation
BiOCl-(001) prepared by Fig. 1 the present invention, the XRD curve of BiOCl-(001)/GO and GO;
The XRD curve of the BiOCl-of Fig. 1 prepared by the present invention (001), BiOCl-(001)/GO and GO.As can be seen from the figure, the crystal face of prepared BiOCl-(001), based on (001) face, illustrates the BiOCl that can prepare exposure (001) face by technology of the present invention.And GO is based on (002) face, after BiOCl-(001) and GO compound, the peak in (001) face diminishes, and broadens, and illustrates that (001) face of BiOCl and (002) face of GO there occurs compound.
Fig. 2 is the projection electromicroscopic photograph of BiOCl-(001)/GO nano composite material prepared by the embodiment of the present invention 1;
Fig. 2 is the projection electromicroscopic photograph of BiOCl-(001)/GO nano composite material prepared by the embodiment of the present invention 1, as can be seen from the figure, the growth of BiOCl-(001) nanometer sheet is in GO nanometer sheet, the nano material of formation sheet-sheet compound, BiOCl-(001) is dispersed relatively good, and its thickness is 20-30nm.
The PL spectrum of BiOCl-(the 001)/GO nano composite material prepared by Fig. 3 embodiment of the present invention 1;
Fig. 3 is the PL spectrum of BiOCl-(the 001)/GO nano composite material prepared by the embodiment of the present invention 1.As can be seen from the figure, the PL spectral intensity of BiOCl-(001)/GO is significantly less than the PL spectral intensity of BiOCl-(001), illustrate that the light induced electron in light nano composite photo-catalyst BiOCl-(001)/GO is transferred, namely be gathered in electronics quilt " extraction " on BiOCl-(001), thus effectively inhibit the compound in light induced electron and hole, extend the life-span in light induced electron and hole, improve photocatalysis effect, this can photocatalysis data from behind find out.
BiOCl-(001) prepared by Fig. 4 embodiment of the present invention 1 and the photocurrent curve of BiOCl-(001)/GO nano composite material;
Fig. 4 is the photocurrent curve of BiOCl-(001) prepared by the embodiment of the present invention 1 and BiOCl-(001)/GO nano composite material, as can be seen from curve: the photo-current intensity of BiOCl-(001)/GO nano composite material is 1.3 times of BiOCl-(001) photo-current intensity, this illustrates that the introducing of GO adds separation of charge and efficiency of transmission, really the electronics " extraction " being accumulated in BiOCl-(001), namely " stripping effect " can be there is in the namely existence of GO.The present invention make use of the surface engineering technology of crystal and the stripping effect of electronics just, has prepared BiOCl-(001)/GO nano composite photo-catalyst.
Detailed description of the invention
Below by example, feature of the present invention is described further, but the present invention is not limited to following embodiment.
One, the preparation of BiOCl-(001)
Embodiment 1
The concrete preparation process of 1#BiOCl-(001) is as follows:
First use Bi (NO
3)
35H
2o is configured to 0.5mol/LBi (NO
3)
3solution for standby: measure 100mLH at normal temperatures
2o, adds the HNO of 20mL65%
3, take 0.06molBi (NO
3)
35H
2o, stirs with glass bar and makes it dissolve completely, obtain 0.5mol/LBi (NO
3)
3solution.
Take 116mgNaCl and 100mg enuatrol (NaOA) and put into round-bottomed flask, add 30mL deionized water, fully stir, NaOA and NaCl is fully dissolved, in round-bottomed flask, slowly add the 0.5mol/LBi (NO of 2mL
3)
3, and in the lower reaction of 95 DEG C of degree three hours, the white precipitate absolute ethyl alcohol obtained repeatedly is washed rear drying, obtain 1#BiOCl-(001) single crystal nanoplate.
Embodiment 2
The concrete preparation process of 2#BiOCl-(001) is as follows:
Take 116mgNaCl and 0mgNaOA and put into round-bottomed flask, add 30mL deionized water, fully stir, NaCl is fully dissolved, in round-bottomed flask, slowly add the 0.5mol/LBi (NO of 2mL
3)
3, and in the lower reaction of 95 DEG C of degree three hours, the white precipitate absolute ethyl alcohol obtained repeatedly is washed rear drying, obtain 2#BiOCl-(001) single crystal nanoplate.
Embodiment 3
The concrete preparation process of 3#BiOCl-(001) is as follows:
Take 116mgNaCl and 200mgNaOA and put into round-bottomed flask, add 30mL deionized water, fully stir, NaCl is fully dissolved, in round-bottomed flask, slowly add the 0.5mol/LBi (NO of 2mL
3)
3, and in the lower reaction of 95 DEG C of degree three hours, the white precipitate absolute ethyl alcohol obtained repeatedly is washed rear drying, obtain 3#BiOCl-(001) single crystal nanoplate.
Embodiment 4
The concrete preparation process of 4#BiOCl-(001) is as follows:
Take 116mgNaCl and 100mgNaOA and put into round-bottomed flask, add 30mL deionized water, fully stir, NaCl is fully dissolved, in round-bottomed flask, slowly add the 0.1mol/LBi (NO of 2mL
3)
3, and in the lower reaction of 95 DEG C of degree three hours, the white precipitate absolute ethyl alcohol obtained repeatedly is washed rear drying, obtain 4#BiOCl-(001) single crystal nanoplate.
Embodiment 5
The concrete preparation process of 5#BiOCl-(001) is as follows:
Take 116mgNaCl and 100mgNaOA and put into round-bottomed flask, add 30mL deionized water, fully stir, NaCl is fully dissolved, in round-bottomed flask, slowly add the 0.3mol/LBi (NO of 2mL
3)
3, and in the lower reaction of 95 DEG C of degree three hours, the white precipitate absolute ethyl alcohol obtained repeatedly is washed rear drying, obtain 5#BiOCl-(001) single crystal nanoplate.
Two, the preparation of BiOCl-(001)/GO nano composite material
Embodiment 6
The concrete preparation process of 1#BiOCl-(001)/GO nano composite material is as follows:
(1) preparation of GO
0.5g graphite powder and 1.5gKMnO
4join in the round-bottomed flask that the 12mL concentrated sulfuric acid is housed, ice-water bath condition lower magnetic force stirs 4h, is heated to 35 DEG C, constant temperature stirs 30min, dropwise adds 23mL distilled water, is warming up to 98 DEG C, stir 15min, this mixture is transferred in ice-water bath, adds 70mL distilled water diluting, add the hydrogen peroxide of 10mL30% again, stir 30min, solution becomes yellow, centrifugation, lower sediment thing, to supernatant liquor pH=7, is drying to obtain GO by abundant washing.
(2) preparation of BiOCl-(001)/GO nano composite material
Take 116mgNaCl, 200mgNaOA, add 30mL deionized water, fully stir, NaOA and NaCl is fully dissolved, adds 15mgGO, stir 2h, in round-bottomed flask, slowly add the 0.5mol/LBi (NO of 2mL
3)
3, and in the lower reaction of 95 DEG C of degree three hours, after the sediment priority deionized water obtained and absolute ethyl alcohol are repeatedly washed, dry, obtain 1#BiOCl-(001)/GO nano composite photo-catalyst.Embodiment 7
The concrete preparation process of 2#BiOCl-(001)/GO nano composite material is as follows:
(1) preparation of GO
With the preparation method of GO in embodiment 6.
(2) preparation of BiOCl-(001)/GO nano composite material
Take 116mgNaCl, 100mgNaOA, add 30mL deionized water, fully stir, NaOA and NaCl is fully dissolved, adds 15mgGO, stir 2h, in round-bottomed flask, slowly add the 0.5mol/LBi (NO of 2mL
3)
3, and in the lower reaction of 95 DEG C of degree three hours, after the sediment priority deionized water obtained and absolute ethyl alcohol are repeatedly washed, dry, obtain 2#BiOCl-(001)/GO nano composite photo-catalyst.Embodiment 8
The concrete preparation process of 3#BiOCl-(001)/GO nano composite material is as follows:
(1) preparation of GO
With the preparation method of GO in embodiment 6.
(2) preparation of BiOCl-(001)/GO nano composite material
Take 116mgNaCl, 0mgNaOA, add 30mL deionized water, fully stir, NaCl is fully dissolved, adds 15mgGO, stir 2h, in round-bottomed flask, slowly add the 0.5mol/LBi (NO of 2mL
3)
3, and in the lower reaction of 95 DEG C of degree three hours, after the sediment priority deionized water obtained and absolute ethyl alcohol are repeatedly washed, dry, obtain 3#BiOCl-(001)/GO nano composite photo-catalyst.
Embodiment 9
The concrete preparation process of 4#BiOCl-(001)/GO nano composite material is as follows:
(1) preparation of GO
With the preparation method of GO in embodiment 6.
(2) preparation of BiOCl-(001)/GO nano composite material
Take 116mgNaCl, 200mgNaOA, add 30mL deionized water, fully stir, NaOA and NaCl is fully dissolved, adds 5mgGO, stir 2h, in round-bottomed flask, slowly add the 0.5mol/LBi (NO of 2mL
3)
3, and in the lower reaction of 95 DEG C of degree three hours, after the sediment priority deionized water obtained and absolute ethyl alcohol are repeatedly washed, dry, obtain 4#BiOCl-(001)/GO nano composite photo-catalyst.Embodiment 10
The concrete preparation process of 5#BiOCl-(001)/GO nano composite material is as follows:
(1) preparation of GO
With the preparation method of GO in embodiment 6.
(2) preparation of BiOCl-(001)/GO nano composite material
Take 116mgNaCl, 200mgNaOA, add 30mL deionized water, fully stir, NaOA and NaCl is fully dissolved, adds 25mgGO, stir 2h, in round-bottomed flask, slowly add the 0.5mol/LBi (NO of 2mL
3)
3, and in the lower reaction of 95 DEG C of degree three hours, after the sediment priority deionized water obtained and absolute ethyl alcohol are repeatedly washed, dry, obtain 5#BiOCl-(001)/GO nano composite photo-catalyst.Embodiment 11
The concrete preparation process of 6#BiOCl-(001)/GO nano composite material is as follows:
(1) preparation of GO
With the preparation method of GO in embodiment 6.
(2) preparation of BiOCl-(001)/GO nano composite material
Take 116mgNaCl, 200mgNaOA, add 30mL deionized water, fully stir, NaOA and NaCl is fully dissolved, adds 40mgGO, stir 2h, in round-bottomed flask, slowly add the 0.5mol/LBi (NO of 2mL
3)
3, and in the lower reaction of 95 DEG C of degree three hours, after the sediment priority deionized water obtained and absolute ethyl alcohol are repeatedly washed, dry, obtain 6#BiOCl-(001)/GO nano composite photo-catalyst.Three, BiOCl-(001) and BiOCl-(001)/GO photocatalytic activity evaluation
BiOCl-(001) prepared by table 1 the embodiment 1 and BiOCl-prepared by embodiment 6 (001)/GO photocatalytic degradation MO
(a)reaction condition: degraded concentration is 10mgL
-1mO aqueous solution 10mL
Measure 10mL10mgL
-1mO solution puts into conical flask, add 30mgBiOCl-(001)/GO nano-composite catalyst, at dark place, ultrasonic disperse 30min makes it reach adsorption equilibrium, then under the condition stirred, LED (30W) conduct irradiates 120min, every the concentration of 40min with MO in the 722S spectrophotometer measurement aqueous solution.
Table 1 is BiOCl-(001) prepared by the present invention and BiOCl-(001)/GO, degrade respectively MO time the different light time degradation rate.As can be seen from Table 1, under the irradiation of LED, BiOCl-(001)/GO nano-composite catalyst shows good catalytic activity to degraded MO.When irradiating 40min, the degradation rate of MO is 68%, when light application time is 120min, degradation rate reaches 87%, and under the same conditions, BiOCl-(001) is as photochemical catalyst, when irradiating 40min, the degradation rate of MO is 43%, when light application time is 120min, degradation rate is only 48%, and as can be seen here, the photocatalytic activity of BiOCl-(the 001)/GO nano-composite catalyst utilizing the surface engineering technology of crystal and the stripping effect of electronics to prepare has had and increases substantially.
The stability of BiOCl-(the 001)/GO nano composite photo-catalyst prepared by table 2 embodiment 6
Table 2 is stability tests of catalyst B iOCl-(001)/GO.Degraded 10mL concentration is 10mgL
-1the MO aqueous solution, during first time degraded, catalyst amount is 30mg, light application time 2h, and after completion of the reaction, centrifugation, reclaim catalyst, then to add 10mL concentration is 10mgL
-1the rhodamine aqueous solution, carries out exposure experiments to light, and catalyst so recycles 3 times, and as can be seen from Table 2, the degradation rate of MO still can reach 85%, and this shows: having good stability of BiOCl-(001)/GO nano-composite catalyst.
Claims (3)
1. the preparation method of BiOCl-(001)/GO nano composite photo-catalyst, it is characterized in that, the active component of this composite photo-catalyst is BiOCl-(001)/GO, plane of crystal engineering and electronics stripping effect is utilized to combine, by the BiOCl single crystal nanoplate phase compound in GO and exposure (001) face, photochemical catalyst BiOCl-(the 001)/GO of preparation nanometer sheet-sheet compound; Its concrete preparation process is as follows:
(1) 0.5g graphite powder and 1.5gKMnO
4join in the round-bottomed flask that the 12mL concentrated sulfuric acid is housed, ice-water bath condition lower magnetic force stirs 4h, is heated to 35 DEG C, constant temperature stirs 30min, dropwise adds 23mL distilled water, is warming up to 98 DEG C, stir 15min, this mixture is transferred in ice-water bath, adds 70mL distilled water diluting, add the hydrogen peroxide of 10mL30% again, stir 30min, solution becomes yellow, centrifugation, lower sediment thing, to supernatant liquor pH=7, is drying to obtain GO by abundant washing;
(2) take sodium chloride 116mg, enuatrol 0-200mg, add 30mL deionized water, abundant stirring, makes enuatrol and NaCl fully dissolve, and adds the GO that 0-40mg step (1) obtains, stir 2h, in round-bottomed flask, slowly add the 0.1-0.5mol/LBi (NO of 2mL
3)
3, and in the lower reaction of 95 DEG C of degree 3 hours, reactant is cooled to room temperature, centrifugation, washing, obtain solid product after drying, this solid product was BiOCl-(001)/GO nano composite material.
2. the preparation method of BiOCl-(001)/GO nano composite photo-catalyst as claimed in claim 1, is characterized in that, in described step (2): enuatrol is 200mg, GO is 15mg, Bi (NO
3)
3for 0.5mol/L.
3. the application of BiOCl-(001)/GO nano composite photo-catalyst of obtaining of preparation method in the reaction of degraded rhodamine as claimed in claim 1.
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