CN105562040B - A kind of preparation and application of BiOCl- (001)/GO nano composite photo-catalysts - Google Patents
A kind of preparation and application of BiOCl- (001)/GO nano composite photo-catalysts Download PDFInfo
- Publication number
- CN105562040B CN105562040B CN201610021421.1A CN201610021421A CN105562040B CN 105562040 B CN105562040 B CN 105562040B CN 201610021421 A CN201610021421 A CN 201610021421A CN 105562040 B CN105562040 B CN 105562040B
- Authority
- CN
- China
- Prior art keywords
- biocl
- added
- composite photo
- nano composite
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 43
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 26
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 58
- 239000013078 crystal Substances 0.000 claims abstract description 31
- 239000011780 sodium chloride Substances 0.000 claims abstract description 29
- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000003756 stirring Methods 0.000 claims abstract description 21
- 239000003054 catalyst Substances 0.000 claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- 230000015556 catabolic process Effects 0.000 claims abstract description 17
- 238000006731 degradation reaction Methods 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 230000000694 effects Effects 0.000 claims abstract description 15
- 238000005516 engineering process Methods 0.000 claims abstract description 14
- 238000005406 washing Methods 0.000 claims abstract description 10
- 239000002055 nanoplate Substances 0.000 claims abstract description 9
- 150000001875 compounds Chemical class 0.000 claims abstract description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000002131 composite material Substances 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 4
- 239000003643 water by type Substances 0.000 claims description 13
- 239000013049 sediment Substances 0.000 claims description 9
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 6
- 239000005457 ice water Substances 0.000 claims description 6
- 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 4
- 238000010790 dilution Methods 0.000 claims description 3
- 239000012895 dilution Substances 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 3
- 239000010439 graphite Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000012286 potassium permanganate Substances 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid group Chemical class S(O)(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
- 239000007788 liquid Substances 0.000 claims description 2
- 239000000376 reactant Substances 0.000 claims description 2
- 239000012265 solid product 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 17
- 230000003197 catalytic effect Effects 0.000 abstract description 8
- 239000008367 deionised water Substances 0.000 abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 abstract description 7
- 229910021389 graphene Inorganic materials 0.000 abstract description 2
- 230000001699 photocatalysis Effects 0.000 description 16
- 229940073609 bismuth oxychloride Drugs 0.000 description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 11
- 238000007146 photocatalysis Methods 0.000 description 9
- 239000007864 aqueous solution Substances 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 239000002244 precipitate Substances 0.000 description 5
- 239000010410 layer Substances 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 238000004220 aggregation Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 230000000593 degrading effect Effects 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 230000001678 irradiating effect Effects 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 238000000103 photoluminescence spectrum Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 230000003595 spectral effect Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 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
- 230000005611 electricity 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
- 238000001595 flow curve Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910052595 hematite Inorganic materials 0.000 description 1
- 239000011019 hematite Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- LIKBJVNGSGBSGK-UHFFFAOYSA-N iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Fe+3].[Fe+3] LIKBJVNGSGBSGK-UHFFFAOYSA-N 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000001782 photodegradation Methods 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
Classifications
-
- B01J35/39—
-
- 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
-
- B01J35/23—
-
- 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
- C02F1/30—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
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
The invention discloses the preparations and application of a kind of BiOCl (001)/GO nano composite photo-catalysts, belong to photochemical catalyst field.The active component of the composite photo-catalyst is BiOCl (001)/GO, feature is combined using plane of crystal engineering technology and electronics stripping effect, GO and the BiOCl single crystal nanoplates in exposure (001) face is mutually compound, prepare nano composite photo-catalyst BiOCl (001)/GO；Preparation method is：NaCl and enuatrol are put into round-bottomed flask, deionized water is added, is sufficiently stirred, enuatrol and NaCl is made fully to dissolve, graphene is added, constant temperature stirring is then slowly added into Bi (NO3)3, reaction certain time postcooling, washing, drying to obtain target product.Nano composite photo-catalyst prepared by the present invention can be used for the reaction of degradation methyl orange, have good catalytic effect and stability.
Description
Technical field
The invention belongs to photochemical catalyst fields, and in particular to one kind is multiple containing bismuth oxychloride (BiOCl) and graphene (GO)
The technology of preparing of closing light catalyst, more particularly to a kind of BiOCl single crystal nanoplates (BiOCl- containing GO and exposure (001) face
(001)) technology of preparing of composite photo-catalyst BiOCl- (001)/GO.The present invention utilizes plane of crystal engineering technology and electronics
Stripping effect is combined, and is prepared for nano composite photo-catalyst BiOCl- (001)/GO, and take for Photodegradation of Methyl Orange (MO)
Obtained good catalytic effect.
Background technology
Environmental problem and energy problem are the two big challenges that 21 century human kind sustainable development faces.The clean sun can be utilized
The Photocatalitic Technique of Semiconductor of energy resource, which becomes, copes with one of the important means of this two big challenge (H.Wang, et
al.Semiconductor heterojunction photocatalysts:design,construction,and
photocatalytic performances,Chem.Soc.Rev.,2014,43,5234-5244.).Wherein BiOCl is due to this
Body has unique layer structure and suitable energy gap and shows very excellent photocatalysis performance, higher stabilization
Property and nontoxic equal excellent characteristics determine its (S.Bai, et al.Toward that has great application prospect in photocatalysis field
Enhanced Photocatalytic Oxygen Evolution:Synergetic Utilization of Plasmonic
Effect and Schottky Junction via Interfacing Facet Selection,Adv.Mater.2015,
27,3444–3452.)。
The atomic structure and electronic structure generally existing difference of plane of crystal and crystals phase, and then generate different physics
Chemical property, and the surface characteristic (such as the properties such as Surface Layer Atomic Structure, surface state) of crystal, usually in performance crystal itself
Physical and chemical performance in terms of play the role of it is vital.The surface of photochemical catalyst is the main field for carrying out light-catalyzed reaction
Institute, some microdefects on surface can influence the transport of surface electronic.In addition, surface state is usually present in semiconductor function
There are highdensity all kinds of surface states, surface states can lead to during photoelectrocatalysis for the outer surface of material, especially nano material
Capture photogenerated charge is crossed to play separation photo-generate electron-hole and realize window role (B.Klahr, the et of photoelectric activity
al.Water Oxidation at Hematite Photoelectrodes:The Role of Surface States,
J.Am.Chem.Soc.,2012,134,4294-4302.).The crystal structure of BiOCl is double Cl along c-axis direction-Sheath and
[Bi2O2]2+Layer structure made of layer is staggered, and weaker model is passed through by Cl atoms between the Cl atomic layers of dual layer arrangement
Moral China bond is closed, and is easy to cause crystal and is dissociated on [001] direction, thus can be prepared with based on different crystal faces
BiOCl, (J.Jiang, et al., Synthesis the and Facet-Dependent such as such as Jiang
Photoreactivity of BiOCl Single-Crystalline Nanosheets,J.Am.Chem.Soc.,2012,
Hydro-thermal method 134,4473-4476) is utilized to synthesize the BiOCl single crystal nanoplates in exposure (001) face and (010) face, and former from surface
The reason of photocatalysis performance that minor structure explains BiOCl (001) face with two aspect of internal electric field effect is better than (010) crystal face.
(S.Bai, et al., Steering charge kinetics in photocatalysis are thought in correlative study:
intersection of materials syntheses,characterization techniques and
Theoretical simulations, Chem.Soc.Rev., 2015,44,2893-2939.) exposure (001) face BiOCl receive
There are, there are potential difference, play the role of detaching photo-generate electron-hole, i.e. electricity between magnetic field and different crystal faces for rice crystals
Son is flowed to low potential, and vacancy is flowed to high potential, to be conducive to improve the photocatalytic activity of BiOCl.But electronics is poly-
Rally weakens the potential difference between the magnetic field and different crystal faces of nanocrystal interior, to be unfavorable for the separation of electron-hole,
Therefore, the photocatalytic activity for relying solely on the surface engineering technology of crystal to improve BiOCl is limited.In order to further carry
The photocatalytic activity of high BiOCl just must be such that the electronics of above-mentioned aggregation consumes rapidly.
GO is important one of carbon material, has many excellent properties, such as large specific surface area, thermal stability is high, leads
Electric energy power is strong etc., is widely used in the various fields including photocatalysis.This patent attempts in the mistake for preparing (001) BiOCl-
GO is introduced in journey, due to the good electric conductivity of GO, the electronics of aggregation is extracted out in time, to promote charge and hole to detach, i.e.,
It is combined using plane of crystal engineering technology and electronics stripping effect, prepares nano composite photo-catalyst BiOCl- (001)/GO,
Further increase its photocatalysis performance.
Invention content
In order to overcome the deficiencies of the prior art, it is taken out using plane of crystal engineering technology and electronics it is an object of the present invention to provide a kind of
Go out the method that effect is combined, prepare nano composite photo-catalyst BiOCl- (001)/GO, to what is prepared with the present invention
BiOCl- (001)/GO nanocomposites obtain good effect as photocatalyst for degrading MO.
In order to achieve the above technical purposes, the present invention is achieved by the following technical programs.
The present invention provides a kind of BiOCl- (001)/GO nanocomposites, active component be BiOCl- (001)/
GO, its main feature is that the method being combined using plane of crystal engineering technology and electronics stripping effect, single preparing BiOCl- (001)
GO is introduced during brilliant nanometer sheet, BiOCl- (001) single crystal nanoplate is made to be grown in GO nanometer sheets, forms composite Nano light
Catalyst, specific preparation process are as follows：
(1) 0.5g graphite powders and 1.5g KMnO4It is added in the round-bottomed flask equipped with the 12mL concentrated sulfuric acids, ice-water bath condition
Lower magnetic agitation 4h is heated to 35 DEG C, and constant temperature stirs 30min, and 23mL distilled water is added dropwise, and is warming up to 98 DEG C, stirring
The mixture is transferred in ice-water bath by 15min, and the dilution of 70mL distilled water is added, adds the hydrogen peroxide of 10mL 30%, stirs
30min is mixed, solution becomes yellow, centrifuges, and fully washing is until supernatant liquor pH=7, by lower sediment thing drying
Obtain GO.
(2) weigh sodium chloride 116mg, enuatrol 0-200mg, 30mL deionized waters be added, are sufficiently stirred, make enuatrol and
NaCl fully dissolves, and the GO that 0-40mg steps (1) obtain is added, and stirs 2h, the 0.1- of 2mL is slowly added into round-bottomed flask
0.5mol/L Bi(NO3)3, and in the lower reaction of 95 DEG C of degree 3 hours, reactant is cooled to room temperature, is centrifuged, is washed, it is dry
After obtain solid product, which is BiOCl- (001)/GO nanocomposites.
By adjusting NaOA, GO and Bi (NO3)3The preparation conditions such as the dosage of solution can control BiOCl- (001)/GO and receive
Pattern, dispersibility and the size of nano composite material.When enuatrol is 200mg, GO 15mg, Bi (NO3)3For 0.5mol/L
When, BiOCl- (001) nanometer sheet can be uniformly dispersed in GO nanometer sheets, form the compound nano-photocatalyst of piece-piece.
BiOCl- (001)/GO nanocomposites prepared by the present invention can be used as photochemical catalyst for the MO that degrades, and show
Good catalytic effect.BiOCl- prepared by the present invention (001)/GO nano-composite catalysts are used to react item when light degradation MO
Part is：A concentration of 10mg mL-1MO aqueous solution 10mL, catalyst amount 30mg, LED light (30W) is light source, irradiation time
For 120min when, the degradation rate of MO reaches 87%.In addition, the catalyst is also with good stability, the above-mentioned MO of catalytic degradation
Aqueous solution, continuous cycle 3 times, degradation rate remains able to reach 82% or so.
Compared with prior art, the present invention has the following technical effects：
(1) using water as solvent, the preparation method of catalyst is simple, and preparation temperature is low.
BiOCl- (001)/GO nanocomposite preparation process is simple.Using water as solvent, using NaCl as raw material, with NaOA
It for surfactant, is first dissolved in water at a certain temperature the two, GO, Bi (NO is then added3)3, reacted at 90 DEG C
3h just obtains BiOCl- (001)/GO nanocomposites.
(2) it is combined with plane of crystal engineering technology and electronics stripping effect, high catalytic efficiency, catalytic stability is good.
Reaction for the MO that degrades, when catalyst amount is 30mg, LED light is light source, when irradiation time is 120min,
The degradation rate of MO is 87%.Catalytic degradation MO aqueous solutions, continuous cycle 3 times, degradation rate does not reduce significantly.
Description of the drawings
The XRD curves of BiOCl- (001), BiOCl- (001)/GO and GO prepared by Fig. 1 present invention；
Fig. 1 be the present invention prepared by BiOCl- (001), BiOCl- (001)/GO and GO XRD curves.It can be with from figure
Find out, the crystal face of prepared BiOCl- (001) illustrates that the technology with the present invention can prepare exposure based on (001) face
(001) BiOCl in face.And GO is based on (002) face, after BiOCl- (001) and GO is compound, the peak in (001) face becomes smaller, and broadens,
(002) face in (001) face and GO that illustrate BiOCl has occurred compound.
Fig. 2 is the projection electromicroscopic photograph of BiOCl- (001)/GO nanocomposites prepared by the embodiment of the present invention 1；
Fig. 2 is the projection electromicroscopic photograph of BiOCl- (001)/GO nanocomposites prepared by the embodiment of the present invention 1, from figure
In as can be seen that BiOCl- (001) nanometer sheet is grown in GO nanometer sheets, form the compound nano material of piece-piece, BiOCl-
(001) relatively good, the thickness 20-30nm of dispersibility.
The PL spectrum of BiOCl- (001)/GO nanocomposites prepared by Fig. 3 embodiment of the present invention 1；
Fig. 3 is the PL spectrum of BiOCl- (001)/GO nanocomposites prepared by the embodiment of the present invention 1.It can from figure
To find out, the PL spectral intensities of BiOCl- (001)/GO are significantly less than the PL spectral intensities of BiOCl- (001), illustrate in light nanometer
Light induced electron in composite photo-catalyst BiOCl- (001)/GO is transferred, that is, the electronics being gathered on BiOCl- (001)
By " extraction ", to effectively inhibit the compound of light induced electron and hole, the service life in light induced electron and hole is extended, raising
Photocatalysis effect, this can find out from subsequent photocatalysis data.
The photoelectricity of BiOCl- (001) and BiOCl- (001)/GO nanocomposites prepared by Fig. 4 embodiment of the present invention 1
Flow curve；
Fig. 4 is the light of the BiOCl- (001) and BiOCl- (001)/GO nanocomposites prepared by the embodiment of the present invention 1
Current curve can be seen that from curve：The photo-current intensity of BiOCl- (001)/GO nanocomposites is (001) BiOCl-
1.3 times of photo-current intensity, this illustrates that the introducing of GO increases separation of charge and efficiency of transmission, that is, the presence of GO really can
, that is, there is " stripping effect " in the enough electronics " extraction " for being accumulated in (001) BiOCl-.The present invention is exactly that the surface of crystal is utilized
The stripping effect of engineering technology and electronics is prepared for BiOCl- (001)/GO nano composite photo-catalysts.
Specific implementation mode
The feature of the present invention is described further below by example, but the present invention is not limited to following embodiments.
One, the preparation of BiOCl- (001)
Embodiment 1
The specific preparation process of 1#BiOCl- (001) is as follows：
First use Bi (NO3)3·5H2O is configured to 0.5mol/L Bi (NO3)3Solution for standby：100mL is measured at normal temperatures
H2The HNO of 20mL 65% is added in O3, weigh 0.06mol Bi (NO3)3·5H2O is made it completely dissolved with glass bar stirring, is obtained
To 0.5mol/L Bi (NO3)3Solution.
It weighs 116mg NaCl and 100mg enuatrol (NaOA) to be put into round-bottomed flask, 30mL deionized waters is added, fully
Stirring, makes NaOA and NaCl fully dissolve, the 0.5mol/L Bi (NO of 2mL is slowly added into round-bottomed flask3)3, and in 95 DEG C
The lower reaction of degree three hours, it is dry after obtained white precipitate is repeatedly washed with absolute ethyl alcohol, obtain 1#BiOCl- (001) monocrystalline
Nanometer sheet.
Embodiment 2
The specific preparation process of 2#BiOCl- (001) is as follows：
It weighs 116mg NaCl and 0mg NaOA to be put into round-bottomed flask, 30mL deionized waters is added, is sufficiently stirred, makes
NaCl fully dissolves, and the 0.5mol/L Bi (NO of 2mL are slowly added into round-bottomed flask3)3, and it is small in the lower reaction three of 95 DEG C of degree
When, it is dry after obtained white precipitate is repeatedly washed with absolute ethyl alcohol, obtain 2#BiOCl- (001) single crystal nanoplate.
Embodiment 3
The specific preparation process of 3#BiOCl- (001) is as follows：
It weighs 116mg NaCl and 200mg NaOA to be put into round-bottomed flask, 30mL deionized waters is added, is sufficiently stirred, makes
NaCl fully dissolves, and the 0.5mol/L Bi (NO of 2mL are slowly added into round-bottomed flask3)3, and it is small in the lower reaction three of 95 DEG C of degree
When, it is dry after obtained white precipitate is repeatedly washed with absolute ethyl alcohol, obtain 3#BiOCl- (001) single crystal nanoplate.
Embodiment 4
The specific preparation process of 4#BiOCl- (001) is as follows：
It weighs 116mg NaCl and 100mg NaOA to be put into round-bottomed flask, 30mL deionized waters is added, is sufficiently stirred, makes
NaCl fully dissolves, and the 0.1mol/L Bi (NO of 2mL are slowly added into round-bottomed flask3)3, and it is small in the lower reaction three of 95 DEG C of degree
When, it is dry after obtained white precipitate is repeatedly washed with absolute ethyl alcohol, obtain 4#BiOCl- (001) single crystal nanoplate.
Embodiment 5
The specific preparation process of 5#BiOCl- (001) is as follows：
It weighs 116mg NaCl and 100mg NaOA to be put into round-bottomed flask, 30mL deionized waters is added, is sufficiently stirred, makes
NaCl fully dissolves, and the 0.3mol/L Bi (NO of 2mL are slowly added into round-bottomed flask3)3, and it is small in the lower reaction three of 95 DEG C of degree
When, it is dry after obtained white precipitate is repeatedly washed with absolute ethyl alcohol, obtain 5#BiOCl- (001) single crystal nanoplate.
Two, the preparation of BiOCl- (001)/GO nanocomposites
Embodiment 6
The specific preparation process of 1#BiOCl- (001)/GO nanocomposites is as follows：
(1) preparation of GO
0.5g graphite powders and 1.5g KMnO4It is added in the round-bottomed flask equipped with the 12mL concentrated sulfuric acids, magnetic under the conditions of ice-water bath
Power stirs 4h, is heated to 35 DEG C, and constant temperature stirs 30min, and 23mL distilled water is added dropwise, and is warming up to 98 DEG C, stirs 15min, will
The mixture is transferred in ice-water bath, and the dilution of 70mL distilled water is added, adds the hydrogen peroxide of 10mL 30%, stirs 30min,
Solution becomes yellow, centrifuges, and fully washing is until supernatant liquor pH=7, by lower sediment thing drying to obtain GO.
(2) preparation of BiOCl- (001)/GO nanocomposites
116mg NaCl, 200mg NaOA are weighed, 30mL deionized waters are added, is sufficiently stirred, keeps NaOA and NaCl abundant
15mg GO are added in dissolving, stir 2h, the 0.5mol/L Bi (NO of 2mL are slowly added into round-bottomed flask3)3, and in 95 DEG C of degree
Lower reaction three hours, it is dry after obtained sediment priority deionized water and absolute ethyl alcohol repeatedly washing, obtain 1#
BiOCl- (001)/GO nano composite photo-catalysts.
Embodiment 7
The specific preparation process of 2#BiOCl- (001)/GO nanocomposites is as follows：
(1) preparation of GO
With the preparation method of GO in embodiment 6.
(2) preparation of BiOCl- (001)/GO nanocomposites
116mg NaCl, 100mg NaOA are weighed, 30mL deionized waters are added, is sufficiently stirred, keeps NaOA and NaCl abundant
15mg GO are added in dissolving, stir 2h, the 0.5mol/L Bi (NO of 2mL are slowly added into round-bottomed flask3)3, and in 95 DEG C of degree
Lower reaction three hours, it is dry after obtained sediment priority deionized water and absolute ethyl alcohol repeatedly washing, obtain 2#
BiOCl- (001)/GO nano composite photo-catalysts.
Embodiment 8
The specific preparation process of 3#BiOCl- (001)/GO nanocomposites is as follows：
(1) preparation of GO
With the preparation method of GO in embodiment 6.
(2) preparation of BiOCl- (001)/GO nanocomposites
116mg NaCl, 0mg NaOA are weighed, 30mL deionized waters are added, is sufficiently stirred, NaCl is made fully to dissolve, is added
15mg GO stir 2h, the 0.5mol/L Bi (NO of 2mL are slowly added into round-bottomed flask3)3, and it is small in the lower reaction three of 95 DEG C of degree
When, it is dry after obtained sediment priority deionized water and absolute ethyl alcohol repeatedly washing, obtain 3#BiOCl- (001)/GO
Nano composite photo-catalyst.
Embodiment 9
The specific preparation process of 4#BiOCl- (001)/GO nanocomposites is as follows：
(1) preparation of GO
With the preparation method of GO in embodiment 6.
(2) preparation of BiOCl- (001)/GO nanocomposites
116mg NaCl, 200mg NaOA are weighed, 30mL deionized waters are added, is sufficiently stirred, keeps NaOA and NaCl abundant
5mg GO are added in dissolving, stir 2h, the 0.5mol/L Bi (NO of 2mL are slowly added into round-bottomed flask3)3, and under 95 DEG C of degree
Reaction three hours, it is dry after obtained sediment priority deionized water and absolute ethyl alcohol repeatedly washing, obtain 4#BiOCl-
(001)/GO nano composite photo-catalysts.
Embodiment 10
The specific preparation process of 5#BiOCl- (001)/GO nanocomposites is as follows：
(1) preparation of GO
With the preparation method of GO in embodiment 6.
(2) preparation of BiOCl- (001)/GO nanocomposites
116mg NaCl, 200mg NaOA are weighed, 30mL deionized waters are added, is sufficiently stirred, keeps NaOA and NaCl abundant
25mg GO are added in dissolving, stir 2h, the 0.5mol/L Bi (NO of 2mL are slowly added into round-bottomed flask3)3, and in 95 DEG C of degree
Lower reaction three hours, it is dry after obtained sediment priority deionized water and absolute ethyl alcohol repeatedly washing, obtain 5#
BiOCl- (001)/GO nano composite photo-catalysts.
Embodiment 11
The specific preparation process of 6#BiOCl- (001)/GO nanocomposites is as follows：
(1) preparation of GO
With the preparation method of GO in embodiment 6.
(2) preparation of BiOCl- (001)/GO nanocomposites
116mg NaCl, 200mg NaOA are weighed, 30mL deionized waters are added, is sufficiently stirred, keeps NaOA and NaCl abundant
40mg GO are added in dissolving, stir 2h, the 0.5mol/L Bi (NO of 2mL are slowly added into round-bottomed flask3)3, and in 95 DEG C of degree
Lower reaction three hours, it is dry after obtained sediment priority deionized water and absolute ethyl alcohol repeatedly washing, obtain 6#
BiOCl- (001)/GO nano composite photo-catalysts.
Three, BiOCl- (001) and BiOCl- (001)/GO photocatalytic activity evaluations
The BiOCl- (001) prepared by BiOCl- (001) and embodiment 6/GO photocatalysis drop prepared by 1 embodiment 1 of table
Solve MO
(a)Reaction condition：Degrade a concentration of 10mg L-1MO aqueous solutions 10mL
Measure 10mL 10mg L-1MO solution is put into conical flask, and 30mg BiOCl- (001)/GO is nano combined are added and urge
Agent, ultrasonic disperse 30min reaches adsorption equilibrium at dark, then under stirring conditions, LED light (30W) conduct
120min is irradiated, every the 40min concentration of MO in 722S spectrophotometer measurement aqueous solutions.
Table 1 is the BiOCl- (001) and BiOCl- (001)/GO prepared by the present invention, respectively when degradation MO when difference illumination
Between degradation rate.From table 1 it follows that under the irradiation of LED light, BiOCl- (001)/GO nano-composite catalysts are to degradation
MO shows good catalytic activity.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 used as photochemical catalyst, when irradiating 40min, the degradation of MO
Rate is 43%, and when light application time is 120min, degradation rate is only 48%, it can be seen that, utilize the surface engineering technology of crystal
The photocatalytic activity of BiOCl- (the 001)/GO nano-composite catalysts prepared with the stripping effect of electronics, which has, to be increased substantially.
The stability of BiOCl- (001)/GO nano composite photo-catalysts prepared by 2 embodiment 6 of table
Table 2 is the stability test of catalyst BiOCl- (001)/GO.Degrade a concentration of 10mg L of 10mL-1MO it is water-soluble
Liquid, catalyst amount is that 30mg, light application time 2h are centrifuged after completion of the reaction when degrading for the first time, recycles catalyst, then
A concentration of 10mg L of 10mL are added-1MO aqueous solutions carry out exposure experiments to light, and catalyst so recycles 3 times, can be with from table 2
Find out, the degradation rate of MO still can reach 85%, this shows：The stability of BiOCl- (001)/GO nano-composite catalysts is good
It is good.
Claims (3)
1. a kind of preparation method of BiOCl- (001)/GO nano composite photo-catalysts, which is characterized in that the composite photo-catalyst
Active component be BiOCl- (001)/GO, be combined using plane of crystal engineering technology and electronics stripping effect, by GO and sudden and violent
The BiOCl single crystal nanoplates for revealing (001) face are mutually compound, prepare compound photochemical catalyst BiOCl- (the 001)/GO of nanometer sheet-piece；Its
Specific preparation process is as follows：
(1) 0.5g graphite powders and 1.5g KMnO4It is added in the round-bottomed flask equipped with the 12mL concentrated sulfuric acids, magnetic force under the conditions of ice-water bath
4h is stirred, is heated to 35 DEG C, constant temperature stirs 30min, and 23mL distilled water is added dropwise, and is warming up to 98 DEG C, 15min is stirred, by this
Mixture is transferred in ice-water bath, and the dilution of 70mL distilled water is added, adds the hydrogen peroxide of 10mL 30%, stirs 30min, molten
Liquid becomes yellow, centrifuges, and fully washing is until supernatant liquor pH=7, by lower sediment thing drying to obtain GO；
(2) weigh sodium chloride 116mg, enuatrol 100-200mg, 30mL deionized waters be added, are sufficiently stirred, make enuatrol and
NaCl fully dissolves, and the GO that 0-40mg steps (1) obtain is added, and stirs 2h, the 0.1- of 2mL is slowly added into round-bottomed flask
0.5mol/L Bi(NO3)3, and in the lower reaction of 95 DEG C of degree 3 hours, reactant is cooled to room temperature, is centrifuged, is washed, it is dry
After obtain solid product, which is BiOCl- (001)/GO nanocomposites.
2. the preparation method of BiOCl- (001)/GO nano composite photo-catalysts as described in claim 1, which is characterized in that institute
It states in step (2)：Enuatrol is 200mg, GO 15mg, Bi (NO3)3For 0.5mol/L.
3. BiOCl- (001)/GO nano composite photo-catalysts that preparation method as described in claim 1 obtains are in degradation MO reactions
In application.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610021421.1A CN105562040B (en) | 2016-01-11 | 2016-01-11 | A kind of preparation and application of BiOCl- (001)/GO nano composite photo-catalysts |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610021421.1A CN105562040B (en) | 2016-01-11 | 2016-01-11 | A kind of preparation and application of BiOCl- (001)/GO nano composite photo-catalysts |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105562040A CN105562040A (en) | 2016-05-11 |
| CN105562040B true CN105562040B (en) | 2018-08-07 |
Family
ID=55872993
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610021421.1A Active CN105562040B (en) | 2016-01-11 | 2016-01-11 | A kind of preparation and application of BiOCl- (001)/GO nano composite photo-catalysts |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105562040B (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107824202A (en) * | 2017-10-19 | 2018-03-23 | 哈尔滨理工大学 | A kind of chlorine bismuth oxybromide (010)/graphene hetero-junctions and its preparation method and application |
| CN108355684B (en) * | 2018-03-02 | 2020-06-02 | 广州大学 | Nanorod-shaped BiOI photocatalyst and preparation method thereof |
| CN109158118B (en) * | 2018-07-24 | 2021-05-18 | 南昌航空大学 | Preparation method of treatment-free tetracycline degradation photocatalyst capable of being repeatedly used |
| CN109078654A (en) * | 2018-08-03 | 2018-12-25 | 沈阳理工大学 | PVP modified graphene loads BiOCl photochemical catalyst and preparation method thereof |
| CN109261171A (en) * | 2018-11-14 | 2019-01-25 | 哈尔滨理工大学 | A kind of chlorine bismuth oxyiodide (010)/graphene hetero-junctions and its preparation method and application |
| CN111701602B (en) * | 2020-06-09 | 2022-10-28 | 华东师范大学 | Composite catalyst, preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103537303A (en) * | 2013-09-24 | 2014-01-29 | 合肥工业大学 | High-performance micro-nano multi-level structure BiOCl photocatalytic material and preparation method thereof |
| CN103623849A (en) * | 2013-11-05 | 2014-03-12 | 江苏大学 | Graphene/BiOCl<x>Br<1-x> micro-nano compound photocatalyst and preparation method thereof |
| CN104001495A (en) * | 2014-06-06 | 2014-08-27 | 河南师范大学 | Preparation method of bismuth oxychloride/graphene composite visible light catalyst |
| CN104353472A (en) * | 2014-11-26 | 2015-02-18 | 安徽工业大学 | Preparation method of BiOBr/RGO nanometer composite and application thereof in reaction of degrading rhodamine |
-
2016
- 2016-01-11 CN CN201610021421.1A patent/CN105562040B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103537303A (en) * | 2013-09-24 | 2014-01-29 | 合肥工业大学 | High-performance micro-nano multi-level structure BiOCl photocatalytic material and preparation method thereof |
| CN103623849A (en) * | 2013-11-05 | 2014-03-12 | 江苏大学 | Graphene/BiOCl<x>Br<1-x> micro-nano compound photocatalyst and preparation method thereof |
| CN104001495A (en) * | 2014-06-06 | 2014-08-27 | 河南师范大学 | Preparation method of bismuth oxychloride/graphene composite visible light catalyst |
| CN104353472A (en) * | 2014-11-26 | 2015-02-18 | 安徽工业大学 | Preparation method of BiOBr/RGO nanometer composite and application thereof in reaction of degrading rhodamine |
Non-Patent Citations (1)
| Title |
|---|
| BiOCl基光催化材料的制备与性能表征;黄永吉;《兰州大学研究生学位论文》;20131215;第32页第4.2节,第38-39页第4.3.5.2节,图4.6 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105562040A (en) | 2016-05-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105562040B (en) | A kind of preparation and application of BiOCl- (001)/GO nano composite photo-catalysts | |
| Liu et al. | Boron doped C3N4 nanodots/nonmetal element (S, P, F, Br) doped C3N4 nanosheets heterojunction with synergistic effect to boost the photocatalytic hydrogen production performance | |
| Tian et al. | Carbon quantum dots/hydrogenated TiO2 nanobelt heterostructures and their broad spectrum photocatalytic properties under UV, visible, and near-infrared irradiation | |
| Xiao et al. | A novel hollow-hierarchical structured Bi2WO6 with enhanced photocatalytic activity for CO2 photoreduction | |
| Ma et al. | Effective photoinduced charge separation and photocatalytic activity of hierarchical microsphere-like C60/BiOCl | |
| CN105709782B (en) | A kind of preparation and application of Ag/AgBr/BiOCl- (001) nanocomposite | |
| Fang et al. | Facile synthesis of CeO2 hollow structures with controllable morphology by template-engaged etching of Cu2O and their visible light photocatalytic performance | |
| Ke et al. | In situ photochemical synthesis noble-metal-free NiS on CdS-diethylenetriamine nanosheets for boosting photocatalytic H2 production activity | |
| Sun et al. | Template-free self-assembly of three-dimensional porous graphitic carbon nitride nanovesicles with size-dependent photocatalytic activity for hydrogen evolution | |
| Shui et al. | Green sonochemical synthesis of cupric and cuprous oxides nanoparticles and their optical properties | |
| Mageshwari et al. | Photocatalytic activity of hierarchical CuO microspheres synthesized by facile reflux condensation method | |
| CN107149932B (en) | Synthesis of bismuth vanadate photocatalyst with controllable crystal face proportion, catalyst and application | |
| CN107349937A (en) | A kind of preparation method of graphene-based bimetallic sulfide nano composite photo-catalyst | |
| Li et al. | Hollow SnO2 nanotubes decorated with ZnIn2S4 nanosheets for enhanced visible-light photocatalytic activity | |
| Li et al. | The in-built bionic “MoFe cofactor” in Fe-doped two-dimensional MoTe 2 nanosheets for boosting the photocatalytic nitrogen reduction performance | |
| CN106824248A (en) | A kind of pattern and the controllable WO of composition3Nanometer sheet/g C3N4The preparation method of nano composite material | |
| CN106268902B (en) | A kind of preparation method of g-C3N4 quantum dot, the quantum dot sensitized BiVO4 photochemical catalyst of Ag | |
| CN103240073B (en) | Zn<2+>-doped BiVO4 visible-light-driven photocatalyst and preparation method thereof | |
| Ma et al. | Construction of dual Z-scheme NiO/NiFe2O4/Fe2O3 photocatalyst via incomplete solid state chemical combustion reactions for organic pollutant degradation with simultaneous hydrogen production | |
| Shi et al. | Synthesis and characterization of porous platelet-shaped α-Bi 2 O 3 with enhanced photocatalytic activity for 17α-ethynylestradiol | |
| CN105879884A (en) | One-dimensional ZnS (zinc sulfide)/CdS-C nanocomposite material and preparation method thereof | |
| Zhang et al. | Facile synthesis of hollow p-Cu2O/n-ZnO microspheres with enhanced photocatalytic H2 production | |
| Zhao et al. | Rose-like CuS microflowers and their enhanced visible-light photocatalytic performance | |
| CN108479777A (en) | A kind of preparation method and applications of attapulgite composite photo-catalyst | |
| Xiong et al. | Unique multi-hierarchical Z-scheme heterojunction of branching SnIn4S8 nanosheets on ZnIn2S4 nanopetals for boosted photocatalytic performance |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |