CN102125832B - Visible light responsive pucherite-graphene composite photocatalyst and preparation method thereof - Google Patents
Visible light responsive pucherite-graphene composite photocatalyst and preparation method thereof Download PDFInfo
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- CN102125832B CN102125832B CN 201110021160 CN201110021160A CN102125832B CN 102125832 B CN102125832 B CN 102125832B CN 201110021160 CN201110021160 CN 201110021160 CN 201110021160 A CN201110021160 A CN 201110021160A CN 102125832 B CN102125832 B CN 102125832B
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- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 41
- 239000002131 composite material Substances 0.000 title claims abstract description 37
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 9
- 239000010439 graphite Substances 0.000 claims abstract description 9
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims abstract description 9
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 5
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract 3
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000005119 centrifugation Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 5
- 238000001035 drying Methods 0.000 abstract 1
- 239000011259 mixed solution Substances 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 239000010865 sewage Substances 0.000 abstract 1
- 230000001699 photocatalysis Effects 0.000 description 8
- 238000000634 powder X-ray diffraction Methods 0.000 description 4
- 238000001069 Raman spectroscopy Methods 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 238000012512 characterization method Methods 0.000 description 3
- 229910002915 BiVO4 Inorganic materials 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000000502 dialysis Methods 0.000 description 1
- YWEUIGNSBFLMFL-UHFFFAOYSA-N diphosphonate Chemical compound O=P(=O)OP(=O)=O YWEUIGNSBFLMFL-UHFFFAOYSA-N 0.000 description 1
- 239000000383 hazardous chemical Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229960000907 methylthioninium chloride Drugs 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- DLYUQMMRRRQYAE-UHFFFAOYSA-N phosphorus pentoxide Inorganic materials O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 239000012286 potassium permanganate Substances 0.000 description 1
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 1
- 235000019394 potassium persulphate Nutrition 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 238000004627 transmission electron microscopy Methods 0.000 description 1
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Abstract
The invention discloses a visible light responsive pucherite-graphene composite photocatalyst and a preparation method thereof. The composite photocatalyst is prepared by compositing pucherite and graphene according to the mass ratio of (1:2)-(1:5). The preparation method comprises the following steps of: putting graphite oxide into a mixed solution of water and ethanol for ultrasonic dispersion, respectively adding bismuth nitrate and ammonium metavanadate into ethanol for stirring, and finally mixing the three systems and regulating the pH to be greater than 7; then, transferring the mixed system into a hydrothermal kettle for reacting; and after the reaction is finished, centrifugally separating, washing and drying the product to obtain a leaf-shaped pucherite-graphene composite photocatalyst. In the invention, by using graphene as a template, the leaf-shaped pucherite-graphene composite photocatalyst is prepared by a hydrothermal synthesis method. The pucherite-graphene composite photocatalyst prepared by the method disclosed by the invention has better application prospect and economic benefit in the aspect of sewage treatment.
Description
Technical field
The invention belongs to take Graphene as template, and in the technology of preparing, particularly a kind of visible light-responded pucherite-graphene composite photocatalyst and preparation method thereof of its surface deposition leaf shape bismuth nitrate composite photo-catalyst.
Background technology
Along with global ecological deterioration problem becomes increasingly conspicuous, oneself becomes the significant problem that the countries in the world government faces and solves effective control of environmental pollution and improvement.Many new technology are attempted being applied to the control of environmental pollution, and Photocatalitic Technique of Semiconductor is exactly one of them.In photocatalysis research process in the past, titanium dioxide research the most extensive, but it has response to ultraviolet light, from taking full advantage of the angle of sunshine, preparing a kind ofly has the catalyst of photocatalytic activity to have and major and immediate significance under visible light.
The band gap of pucherite is narrow, only has 2.4eV, is considered to a kind of desirable visible light catalyst, but because its absorption property is poor, light induced electron can not effectively separate with the hole, has limited again its photocatalytic activity.Up to the present, people improve its photocatalytic activity (Preparation by the method for doping metals or metal oxide, characterization and photocatalytic properties of Cu-loaded BiVO4. Journal of Hazardous Materials 2008,153,877-884; Enhanced photocatalytic activity for degradation of methylene blue over V2O5/BiVO4 composite. Journal of Alloys and Compounds 2009,479,821-827.).
Summary of the invention
The object of the present invention is to provide a kind of long-pending visible light-responded pucherite-graphene composite photocatalyst of photocatalytic activity and particle surface and preparation method thereof that improves.
The technical solution that realizes the object of the invention is: a kind of visible light-responded pucherite-graphene composite photocatalyst is characterized in that: the pucherite and the Graphene that are 1:2 ~ 1:5 by mass ratio are composited.Preparation method's step is as follows:
The first step is with graphite oxide ultrasonic dispersion in water and ethanol system;
Second step stirs bismuth nitrate and ammonium metavanadate respectively in isopyknic ethanol;
The 3rd step, first step gained system is mixed with second step gained mixture, regulate this mixed system and be alkalescence, and stir;
In the 4th step, the 3rd reaction system that goes on foot is transferred to carries out hydro-thermal reaction in water heating kettle;
The 5th step, with the products therefrom centrifugation of the 4th step, with the deionized water washing, the dry rear pucherite-graphene composite photocatalyst that obtains.
The present invention compared with prior art, its remarkable advantage: (1) adopts Graphene is template, at its surface deposition leaf shape bismuth nitrate composite photo-catalyst, provide than large surface area and more activated centre, improve the absorption property of catalyst, light induced electron can effectively be separated with the hole, thereby improve its photocatalytic activity; (2) by hydro-thermal reaction, graphite oxide is reduced into Graphene, has avoided using other reducing agents.
Description of drawings
Fig. 1 is the XRD figure of embodiment 1 obtained pucherite-graphene composite photocatalyst.
Fig. 2 is the Raman spectrogram of embodiment 1 obtained pucherite-graphene composite photocatalyst.
Fig. 3 is the TEM figure of embodiment 1 obtained pucherite-graphene composite photocatalyst.
Fig. 4 is the preparation method's of the visible light-responded pucherite-graphene composite photocatalyst of the present invention schematic diagram.
The specific embodiment
Below in conjunction with accompanying drawing, the present invention is described in further detail.
In conjunction with Fig. 4, pucherite-graphene composite photocatalyst that the present invention is visible light-responded, the pucherite and the Graphene that are 1:2 ~ 1:5 by mass ratio are composited.
The preparation method of pucherite-graphene composite photocatalyst that the present invention is visible light-responded comprises the following steps:
The first step, with graphite oxide ultrasonic dispersion in water and ethanol system, the volume ratio of second alcohol and water is 1:1;
Second step stirs bismuth nitrate and ammonium metavanadate 20-50 minute in isopyknic ethanol respectively;
The 3rd step, first step gained system is mixed with second step gained mixture, regulate this mixed system and be alkalescence, and stirred 30-60 minute;
The 4th step was transferred to the 3rd reaction system that goes on foot and carries out hydro-thermal reaction in water heating kettle, and reaction temperature is 180-200 ° of C, and the reaction time is 5-8 hour;
The 5th step, with the products therefrom centrifugation of the 4th step, with the deionized water washing, the dry rear pucherite-graphene composite photocatalyst that obtains, baking temperature is 60 ° of C, the time is 12 hours.
The preparation method of pucherite-graphene composite photocatalyst that the present invention is visible light-responded, the volume ratio of second alcohol and water is 3:1 in whole reaction system.
Below in conjunction with embodiment, the present invention is described in further details.
Embodiment 1: the preparation method of pucherite-graphene composite photocatalyst that the present invention is visible light-responded comprises the following steps:
The first step, the preparation of graphite oxide.10 g graphite powders are joined the potassium peroxydisulfate (5 g) of 80 ℃, in the concentrated sulfuric acid solution (15mL) of phosphorus pentoxide (5g), pre-oxidation 6 hours, cool to room temperature, filter afterwards, and washing is to neutral.The graphite powder (10 g) of pre-oxidation is joined in the 230 mL concentrated sulfuric acid solutions of 0 ℃, the careful potassium permanganate that adds 30g afterwards, afterwards in 35 ℃ of reactions 2 hours, add 30% the hydrogen peroxide of 1L deionized water and 25mL to make reaction terminating in the most backward reactant liquor, filter, washing, dialysis makes graphite oxide.
Second step is placed in 10mL ethanol with the graphite oxide of 40mg and the 10mL deionized water for ultrasonic was disperseed 2 hours.
In the 3rd step, 0.1796g bismuth nitrate and 0.0430g ammonium metavanadate were stirred 20 minutes in 10mL ethanol respectively.
The 4th step, second step was mixed with the 3rd step, regulate pH=7, and stirred 30 minutes.
The 5th step was transferred to the 4th reaction system that goes on foot in the 50mL water heating kettle, 180 ℃ of reactions 6 hours.
The 6th step, with the product centrifugation of the 5th step, with the deionized water washing, the dry rear pucherite-graphene composite photocatalyst that obtains.
Characterize through X-ray powder diffraction (XRD), prepared product is monoclinic system pucherite (JCPDS 14-0688), and Fig. 1 is the XRD figure of obtained pucherite-graphene composite photocatalyst.Through the Raman spectral characterization, prepared product is pucherite-graphene composite photocatalyst, and Fig. 2 is the Raman spectrogram of obtained pucherite-graphene composite photocatalyst.(TEM) carries out morphology characterization to prepared pucherite-graphene composite photocatalyst through the transmission electron microscopy Electronic Speculum, and the present invention has made leaf shape pucherite-graphene composite photocatalyst.Fig. 3 is the TEM figure of obtained pucherite-graphene composite photocatalyst.
Embodiment 2: the preparation method of pucherite-graphene composite photocatalyst that the present invention is visible light-responded comprises the following steps:
The first step is with the step 1 in embodiment 1.
Second step is with the step 2 in embodiment 1.
In the 3rd step, 0.1796g bismuth nitrate and 0.0430g ammonium metavanadate were stirred 30 minutes in 10mL ethanol respectively.
The 4th step, second step was mixed with the 3rd step, regulate pH=8, and stirred 40 minutes.
The 5th step was transferred to the 4th reaction system that goes on foot in the 50mL water heating kettle, 190 ℃ of reactions 7 hours.
The 6th step is with the step 6 in embodiment 1.
Embodiment 3: the preparation method of pucherite-graphene composite photocatalyst that the present invention is visible light-responded comprises the following steps:
The first step is with the step 1 in embodiment 1.
Second step is with the step 2 in embodiment 1.
In the 3rd step, 0.1796g bismuth nitrate and 0.0430g ammonium metavanadate were stirred 50 minutes in 10mL ethanol respectively.
The 4th step, second step was mixed with the 3rd step, regulate pH=10, and stirred 60 minutes.
The 5th step was transferred to the 4th reaction system that goes on foot in the 50mL water heating kettle, 200 ℃ of reactions 8 hours.
The 6th step is with the step 6 in embodiment 1.
Claims (3)
1. the preparation method of a visible light-responded pucherite-graphene composite photocatalyst, it is characterized in that, be that preparation method's the step of the pucherite of 1:2 ~ 1:5 and visible light-responded pucherite-graphene composite photocatalyst that Graphene is composited is as follows by mass ratio:
The first step is with graphite oxide ultrasonic dispersion in water and ethanol system; The volume ratio of second alcohol and water is 1:1;
Second step stirs bismuth nitrate and ammonium metavanadate respectively in isopyknic ethanol;
The 3rd step, first step gained system is mixed with second step gained mixture, regulate this mixed system and be alkalescence, and stir;
In the 4th step, the 3rd reaction system that goes on foot is transferred to carries out hydro-thermal reaction in water heating kettle; Reaction temperature is 180-200 ℃, and the reaction time is 5-8 hour;
The 5th step, with the products therefrom centrifugation of the 4th step, with the deionized water washing, the dry rear pucherite-graphene composite photocatalyst that obtains;
The volume ratio of second alcohol and water is 3:1 in whole reaction system.
2. the preparation method of visible light-responded pucherite-graphene composite photocatalyst according to claim 1, it is characterized in that: the mixing time in second step is 20-50 minute.
3. the preparation method of visible light-responded pucherite-graphene composite photocatalyst according to claim 1, it is characterized in that: the mixing time in the 3rd step is 30-60 minute.
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