CN106890657A - A kind of graphene oxide/silver phosphate/composite photo-catalyst and preparation and application - Google Patents
A kind of graphene oxide/silver phosphate/composite photo-catalyst and preparation and application Download PDFInfo
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- CN106890657A CN106890657A CN201710010214.0A CN201710010214A CN106890657A CN 106890657 A CN106890657 A CN 106890657A CN 201710010214 A CN201710010214 A CN 201710010214A CN 106890657 A CN106890657 A CN 106890657A
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- graphene oxide
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- phosphate
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- 229910000161 silver phosphate Inorganic materials 0.000 title claims abstract description 54
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 43
- 239000002131 composite material Substances 0.000 title claims abstract description 40
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 40
- FJOLTQXXWSRAIX-UHFFFAOYSA-K silver phosphate Chemical compound [Ag+].[Ag+].[Ag+].[O-]P([O-])([O-])=O FJOLTQXXWSRAIX-UHFFFAOYSA-K 0.000 title claims abstract description 23
- 229940019931 silver phosphate Drugs 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000006185 dispersion Substances 0.000 claims abstract description 41
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000007788 liquid Substances 0.000 claims abstract description 31
- 238000003756 stirring Methods 0.000 claims abstract description 28
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000007864 aqueous solution Substances 0.000 claims abstract description 15
- 238000005406 washing Methods 0.000 claims abstract description 14
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 13
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 11
- 230000015556 catabolic process Effects 0.000 claims abstract description 10
- 238000005119 centrifugation Methods 0.000 claims abstract description 10
- 238000006731 degradation reaction Methods 0.000 claims abstract description 10
- 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 abstract description 9
- 229940043267 rhodamine b Drugs 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- 230000003197 catalytic effect Effects 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims description 7
- 238000002604 ultrasonography Methods 0.000 claims description 7
- 230000035484 reaction time Effects 0.000 claims description 4
- 238000004821 distillation Methods 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 238000001291 vacuum drying Methods 0.000 claims 1
- 239000003054 catalyst Substances 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract description 7
- 230000001699 photocatalysis Effects 0.000 abstract description 5
- 238000006555 catalytic reaction Methods 0.000 abstract description 3
- 238000005286 illumination Methods 0.000 abstract description 3
- 229910019142 PO4 Inorganic materials 0.000 description 13
- 239000000243 solution Substances 0.000 description 12
- 238000001556 precipitation Methods 0.000 description 10
- 230000015572 biosynthetic process Effects 0.000 description 7
- 101710134784 Agnoprotein Proteins 0.000 description 6
- 239000012153 distilled water Substances 0.000 description 6
- 230000001133 acceleration Effects 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 238000006552 photochemical reaction Methods 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000004593 Epoxy Chemical group 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006065 biodegradation reaction Methods 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000002189 fluorescence spectrum Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 150000002500 ions Chemical group 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000012286 potassium permanganate Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000006862 quantum yield reaction Methods 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Inorganic materials [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/16—Phosphorus; Compounds thereof containing oxygen, i.e. acids, anhydrides and their derivates with N, S, B or halogens without carriers or on carriers based on C, Si, Al or Zr; also salts of Si, Al and Zr
- B01J27/18—Phosphorus; Compounds thereof containing oxygen, i.e. acids, anhydrides and their derivates with N, S, B or halogens without carriers or on carriers based on C, Si, Al or Zr; also salts of Si, Al and Zr with metals other than Al or Zr
- B01J27/1802—Salts or mixtures of anhydrides with compounds of other metals than V, Nb, Ta, Cr, Mo, W, Mn, Tc, Re, e.g. phosphates, thiophosphates
- B01J27/1817—Salts or mixtures of anhydrides with compounds of other metals than V, Nb, Ta, Cr, Mo, W, Mn, Tc, Re, e.g. phosphates, thiophosphates with copper, silver or gold
-
- B01J35/39—
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
-
- 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 belongs to catalysis material technical field, a kind of graphene oxide/silver phosphate/composite photo-catalyst and preparation and application are disclosed.Methods described is：(1) graphene oxide ultrasonic disperse is obtained into graphene oxide dispersion in water；(2) aqueous solution of silver nitrate is dropped in the graphene oxide dispersion of step (1), lucifuge stirring obtains mixed dispersion liquid；(3) to the aqueous solution that disodium hydrogen phosphate is added dropwise in mixed dispersion liquid, lucifuge stirring reaction, centrifugation, washing is dried, and obtains graphene oxide/silver phosphate/composite photo-catalyst.Catalyst photocatalytic activity of the invention is high, has good stability；Preparation method is simple, it is easy to produce in batches；Under visible light illumination, can be used for the catalytic degradation of the materials such as organic pollution such as rhodamine B.
Description
Technical field
The invention belongs to catalysis material technical field, and in particular to a kind of graphene oxide/silver phosphate/composite photocatalyst
Agent and preparation and application.
Background technology
Photocatalysis technology is that, using illumination and catalyst collective effect, photochemical reaction occurs, for being difficult to biodegradation
Organic matter removal have certain advantage.Conventional Ti O2Photochemical catalyst possesses non-toxic inexpensive, stable chemical nature, anti-light corrosivity
The advantage such as strong and oxidability is high, is widely used, but it can only absorb purple of the sunshine medium wavelength less than 380nm
Outer light, the utilization rate to sunshine is very low.
Silver orthophosphate (Ag3PO4) used as a kind of visible-light photocatalyst of latest find in recent years, it can be small with absorbing wavelength
In the sunshine of 530nm, and quantum yield under visible light is up to more than 90%, shows under visible light illumination powerful
Oxidability.Yet with Ag3PO4It is slightly soluble in water and photoetch phenomenon easily occurs, reduces the stability of its structure.
Graphene oxide (GO) is a kind of material with quasi- two-dimensional layered structure, and it introduces many in graphenic surface
The oxygen-containing functional groups such as carboxyl, hydroxyl, epoxy radicals.With good electric conductivity, big specific surface area and high mechanical properties so that GO
Composite photocatalyst material has obtained extensive concern.Therefore, GO/Ag is prepared3PO4Composite, improve photocatalytic activity turn into grind
The focus studied carefully.
The content of the invention
In order to solve the shortcoming and defect part of above prior art, primary and foremost purpose of the invention is to provide a kind of oxidation
The preparation method of Graphene/silver phosphate composite photocatalyst.
Urged another object of the present invention is to provide the graphene oxide/silver phosphate/complex light prepared by the above method
Agent.
It is still another object of the present invention to provide the application of above-mentioned graphene oxide/silver phosphate/composite photo-catalyst.It is described
Graphene oxide/silver phosphate/composite photo-catalyst is in catalytic degradation organic pollution, such as application in rhodamine B material.
The object of the invention is achieved through the following technical solutions：
A kind of preparation method of graphene oxide/silver phosphate/composite photo-catalyst, including following preparation process：
(1) graphene oxide ultrasonic disperse is obtained into graphene oxide dispersion in water；
(2) lucifuge is stirred in silver nitrate aqueous solution being dropped into graphene oxide dispersion, obtains mixed dispersion liquid；
(3) to dropwise addition disodium hydrogen phosphate (Na in mixed dispersion liquid2HPO4·12H2O) aqueous solution lucifuge stirring reaction, from
The heart, washing is dried, and obtains graphene oxide/silver phosphate/composite photo-catalyst.
The concentration of graphene oxide dispersion described in step (1) is (0.2~1.5) mg/mL；The graphene oxide is excellent
Choosing is dispersed in water in the form of graphene oxide water solution, and the concentration of graphene oxide water solution is (0.5~1.5) mg/mL；
The power of the ultrasound is 100~200W, and ultrasonic time is 20~40min.
The temperature of the stirring of lucifuge described in step (2) is room temperature, and the time of stirring is 0.5~1h；The rotating speed of the stirring
It is 300~500rpm；Silver nitrate and the molal volume ratio of water are (0.05~0.08) in silver nitrate aqueous solution described in step (2)
mol：100mL.The speed being added dropwise described in step (2) is 20~30 drops/min；Graphene oxide dispersion described in step (2)
Middle graphene oxide is (3~30) mg with the mass ratio of silver nitrate in silver nitrate aqueous solution:1.02g.
Disodium hydrogen phosphate (Na described in step (3)2HPO4·12H2O) in the aqueous solution disodium hydrogen phosphate and water mole body
Product is than being (0.01~0.03) mol：200mL；Silver nitrate and the disodium hydrogen phosphate aqueous solution in mixed dispersion liquid described in step (3)
The mol ratio of middle disodium hydrogen phosphate is 3:1；The speed being added dropwise described in step (3) is 20~30 drops/min；Described in step (3)
The temperature of lucifuge stirring reaction is room temperature, 3~5h of lucifuge stirring reaction time；The rotating speed of the stirring is 300~500rpm；
Washing described in step (3) refers to use distillation water washing, and the drying is to be vacuum dried under the conditions of 60~80 DEG C
10~14h.
Graphene oxide described in step (1) is prepared using improved Hummers oxidizing process.
A kind of graphene oxide/silver phosphate/composite photo-catalyst, is prepared by above method,
Application of the above-mentioned graphene oxide/silver phosphate/composite photo-catalyst in catalytic degradation organic pollution.
Preparation principle of the invention is：Ag is prepared by liquid-phase precipitation method3PO4Photochemical catalyst；With the GO of 1mg/mL as load
Body, GO/Ag is prepared by ion exchange-precipitation method3PO4Composite photo-catalyst.Using the efficient electron transfer efficiencies of GO, machine high
Tool intensity and the compound of electron hole pair can be effectively prevented as electron acceptor, suppress the generation of photoetch phenomenon, improve
The photocatalytic activity and stability of catalyst.
Preparation method of the invention and the product for obtaining have the following advantages that and beneficial effect：
(1) present invention can just prepare GO/Ag using the simple precipitation method3PO4Composite photo-catalyst, it is easy to relatively high-volume
Production；
(2) the obtained GO/Ag of the present invention3PO4Composite photo-catalyst has good photocatalytic degradation characteristic to rhodamine B,
There is very big exploitation and application prospect in terms of degraded organic dye pollutant under visible light conditions；
(3) GO/Ag obtained in the inventive method3PO4Composite photo-catalyst has good stability, is Ag3PO4It is compound
Catalyst preparation extends new direction.
Brief description of the drawings
Fig. 1 is GO/Ag prepared by embodiment 1~63PO4Composite photo-catalyst and Ag3PO4Under visible light to rhodamine B
Degradation curve figure；GO/Ag in figure3PO4(1%)~GO/Ag3PO4(10%) embodiment 1~6 is corresponded to respectively；
Fig. 2 is GO/Ag prepared by embodiment 43PO4Composite photo-catalyst and Ag3PO4Rhodamine B is followed under visible light
Ring degradation curve figure；
Fig. 3 is GO/Ag prepared by embodiment 43PO4Composite photo-catalyst and Ag3PO4Fluorescence spectra (PL).
Specific embodiment
With reference to embodiment, the present invention is described in further detail, but embodiments of the present invention not limited to this.
The graphene oxide is prepared using improved Hummers oxidizing process, is concretely comprised the following steps：1. it is by specification
The beaker of 500mL is placed in ice bath environment, adds the concentrated sulfuric acid of 230mL98%, then to being slowly added to 5.0g in the concentrated sulfuric acid
NaNO3Powder, and be stirred continuously；2. 10.0g crystalline flake graphites are weighed to be slowly added in above-mentioned solution and be stirred continuously, is then weighed
30.0g KMnO4It is slowly added into above-mentioned mixed liquor, and notes maintaining the temperature at less than 20 DEG C, the stirring reaction time is 1h；③
Ice bath is removed, 35 DEG C is warming up to and is stirred continuously 2h, now mixture becomes sticky, generate taupe material；4. 45mL is added
Pure water, is continuously heating to 90 DEG C, and the reaction time keeps 15min, mixture to be changed into brown；5. it is 1 to add volume ratio:2 peroxide
Change the mixed liquor 100mL of hydrogen (30%) and pure water, until bubble-free is emerged, terminate reaction；6. the yellow suspension for now generating
Washed with the hydrochloric acid that concentration is 1mol/L, be centrifuged, filtered, to remove sulfate ion；7. finally pure water cyclic washing is used
Precipitation, centrifugation, are diluted to concentration for 1mg/mL, deposit in standby in 4 DEG C of refrigerators.
Embodiment 1
(1) the GO solution of 3mL concentration 1mg/mL is measured in 10mL water, the ultrasonic disperse in the ultrasonic device of P=100W
30min, obtains GO dispersion liquids；
(2) 1.02g AgNO are weighed3It is dissolved in 10mL water, then drops in the GO dispersion liquids of step (1), speed is added dropwise
It is 25 drops/min to spend, and lucifuge stirs 1h (400r/min) under room temperature condition, obtains mixed dispersion liquid；
(3) 0.716g Na are weighed2HPO4·12H2O is dissolved in 20mL water, then drops to the mixing dispersion of step (2)
In liquid, rate of addition is 25 drops/min, and lucifuge stirs 4h (400r/min) under room temperature condition, forms precipitation；
(4) pelleting centrifugation that will be obtained in step (3), with distilled water cyclic washing 3 times, 12h is vacuum dried at 60 DEG C,
Obtain GO/Ag3PO4(it is Ag by the weight for calculating GO due to having mass loss in actual preparation3PO4The 1% of weight is
W=1%) composite photo-catalyst is GO/Ag3PO4(1%).
Embodiment 2
(1) the GO solution of 9mL concentration 1mg/mL is measured in 10mL water, the ultrasound 40min in the ultrasonic device of P=100W,
It is fully dispersed in water to GO, obtains GO dispersion liquids；
(2) 1.02g AgNO are weighed3It is dissolved in 10mL water, then drops in the GO dispersion liquids of step (1), speed is added dropwise
It is 25 drops/min to spend, and lucifuge stirs 1h (400r/min) under room temperature condition, obtains mixed dispersion liquid；
(3) 0.716g Na are weighed2HPO4·12H2O is dissolved in 20mL water, then drops to the mixing dispersion of step (2)
In liquid, rate of addition is 25 drops/min, and lucifuge stirs 4h (400r/min) under room temperature condition, forms precipitation；
(4) pelleting centrifugation that will be obtained in step (3), with distilled water cyclic washing 4 times, 12h is vacuum dried at 65 DEG C,
Obtain GO/Ag3PO4(weight of GO is Ag3PO4The 3% of weight is w=3%) composite photo-catalyst is GO/Ag3PO4(3%).
Embodiment 3
(1) the GO solution of 15mL concentration 1mg/mL is measured in 10mL water, the ultrasound 40min in the ultrasonic device of P=100W,
It is fully dispersed in water to GO, obtains GO dispersion liquids；
(2) 1.02g AgNO are weighed3It is dissolved in 10mL water, then drops in the GO dispersion liquids of step (1), speed is added dropwise
It is 25 drops/min to spend, and lucifuge stirs 1h (400r/min) under room temperature condition, obtains mixed dispersion liquid；
(3) 0.716g Na are weighed2HPO4·12H2O is dissolved in 20mL water, then drops to the mixing of step (2) formation
In dispersion liquid, rate of addition is 25 drops/min, and lucifuge stirs 4h (400r/min) under room temperature condition, forms precipitation；
(4) pelleting centrifugation that will be obtained in step (3), with distilled water cyclic washing 5 times, 12h is vacuum dried at 60 DEG C,
Obtain GO/Ag3PO4(weight of GO is Ag3PO4The 5% of weight is w=5%) composite photo-catalyst is GO/Ag3PO4(5%).
Embodiment 4
(1) the GO solution of 21mL concentration 1mg/mL is measured in 10mL water, the ultrasound 40min in the ultrasonic device of P=100W,
It is fully dispersed in water to GO, obtains GO dispersion liquids；
(2) 1.02g AgNO are weighed3It is dissolved in 10mL water, then drops in the GO dispersion liquids of step (1) formation, drips
Acceleration is 25 drops/min, and lucifuge stirs 1h (400r/min) under room temperature condition, obtains mixed dispersion liquid；
(3) 0.716g Na are weighed2HPO4·12H2O is dissolved in 20mL water, then drops to the mixing of step (2) formation
In dispersion liquid, rate of addition is 25 drops/min, and lucifuge stirs 4h (400r/min) under room temperature condition, forms precipitation；
(4) pelleting centrifugation that will be obtained in step (3), with distilled water cyclic washing 5 times, 12h is vacuum dried at 60 DEG C,
Obtain GO/Ag3PO4(weight of GO is Ag3PO4The 7% of weight is w=7%) composite photo-catalyst is GO/Ag3PO4(7%).
Embodiment 5
(1) the GO solution of 27mL concentration 1mg/mL is measured in 10mL water, the ultrasound 30min in the ultrasonic device of P=100W,
It is fully dispersed in water to GO, obtains GO dispersion liquids；
(2) 1.02g AgNO are weighed3It is dissolved in 10mL water, then drops in the GO dispersion liquids of step (1) formation, drips
Acceleration is 25 drops/min, and lucifuge stirs 1h (400r/min) under room temperature condition；
(3) 0.716g Na are weighed2HPO4·12H2O is dissolved in 20mL water, then drops to the mixing of step (2) formation
In dispersion liquid, rate of addition is 25 drops/min, and lucifuge stirs 4h (400r/min) under room temperature condition, forms precipitation；
(4) pelleting centrifugation that will be obtained in step (3), with distilled water cyclic washing 4 times, 12h is vacuum dried at 60 DEG C,
Obtain GO/Ag3PO4(weight of GO is Ag3PO4The 9% of weight is w=9%) composite photo-catalyst is GO/Ag3PO4(9%).
Embodiment 6
(1) the GO solution of 30mL concentration 1mg/mL is measured in 10mL water, the ultrasound 40min in the ultrasonic device of P=100W,
It is fully dispersed in water to GO, obtains GO dispersion liquids；
(2) 1.02g AgNO are weighed3It is dissolved in 10mL water, then drops in the GO dispersion liquids of step (1) formation, drips
Acceleration is 25 drops/min, and lucifuge stirs 1h (400r/min) under room temperature condition, obtains mixed dispersion liquid；
(3) 0.716g Na are weighed2HPO4·12H2O is dissolved in 20mL water, then drops to the mixing of step (2) formation
In dispersion liquid, rate of addition is 25 drops/min, and lucifuge stirs 4h (400r/min) under room temperature condition, forms precipitation；
(4) pelleting centrifugation that will be obtained in step (3), with distilled water cyclic washing 5 times, 12h is vacuum dried at 60 DEG C,
Obtain GO/Ag3PO4(weight of GO is Ag3PO4The 10% of weight is w=10%) composite photo-catalyst is GO/Ag3PO4
(10%).
Embodiment 1~6 is the GO/Ag for preparing3PO4Composite photo-catalyst and Ag3PO4To the degradation curve such as figure of rhodamine B
Shown in 1.As can be seen that as the mass fraction w=7% of GO, catalyst is optimal to the degradation effect of rhodamine B.Embodiment 4 is made
Standby GO/Ag3PO4Composite photo-catalyst and Ag3PO4Circulation degradation curve figure to rhodamine B is as shown in Fig. 2 by 5 drops
After solution, degradation efficiency is still up to 90% or so.GO/Ag prepared by embodiment 43PO4Composite photo-catalyst and Ag3PO4It is glimmering
Light spectrogram (PL) figure is as shown in Figure 3.As can be seen from Figure 3 strong diffraction maximum is occurred in that at 373nm, this be due to
Ag3PO4Middle electronics is in O 2p tracks and Ag+Transfer causes between d tracks.Compare Ag3PO4And GO/Ag3PO4The fluorescence of sample
Spectrum discovery, GO/Ag3PO4The diffraction peak intensity of sample is relatively low, because the addition of GO inhibits the compound of photo-generated carrier,
So as to the GO/Ag in PL collection of illustrative plates3PO4The diffraction peak intensity of sample is relatively low.Therefore, the addition of GO can make to be located at Ag3PO4Surface
Electronics be quickly transferred to GO surfaces and stored, efficiently separate photo-generate electron-hole pair, extend the life-span of photo-generated carrier,
Further improve photocatalytic activity.
The test condition of composite photocatalyst for degrading rhodamine B：Photocatalytic degradation Rh B are tested than bright photochemical reaction
Carried out in instrument (BL-GHX-V).Using the xenon lamp of 500W as light source, obtained through 420nm cutoff wavelengths optical filter and remove ultraviolet light
Visible ray.0.1g photochemical catalysts, dark adsorption 30min is added to reach absorption flat in the Rh B aqueous solution of the 10mg/L of 100mL
Weighing apparatus.Turning on light carries out photocatalytic degradation experiment, and 3mL solution, centrifugation removal catalysis are drawn with dropper every 15min in experimentation
Agent, its absorbance is determined using ultraviolet-uisible spectrophotometer under λ=554nm.
Above-described embodiment is the present invention preferably implementation method, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from Spirit Essence of the invention and the change, modification, replacement made under principle, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (9)
1. a kind of preparation method of graphene oxide/silver phosphate/composite photo-catalyst, it is characterised in that：Comprise the following steps：
(1) graphene oxide ultrasonic disperse is obtained into graphene oxide dispersion in water；
(2) aqueous solution of silver nitrate is dropped in the graphene oxide dispersion of step (1), lucifuge stirring obtains mixing point
Dispersion liquid；
(3) to the aqueous solution that disodium hydrogen phosphate is added dropwise in mixed dispersion liquid, lucifuge stirring reaction, centrifugation, washing is dried, obtained
Graphene oxide/silver phosphate/composite photo-catalyst.
2. the preparation method of graphene oxide/silver phosphate/composite photo-catalyst according to claim 1, it is characterised in that step
(3) silver nitrate and the mol ratio of disodium hydrogen phosphate in the disodium hydrogen phosphate aqueous solution are 3 in mixed dispersion liquid described in:1；Step
(3) temperature of lucifuge stirring reaction described in is room temperature, 3~5h of lucifuge stirring reaction time.
3. the preparation method of graphene oxide/silver phosphate/composite photo-catalyst according to claim 1, it is characterised in that：Step
Suddenly described in (2) in graphene oxide dispersion in graphene oxide and silver nitrate aqueous solution silver nitrate mass ratio for (3~
30)mg:1.02g；The temperature of the stirring of lucifuge described in step (2) is room temperature, and the time of stirring is 0.5~1h.
4. the preparation method of graphene oxide/silver phosphate/composite photo-catalyst according to claim 1, it is characterised in that：Step
Suddenly the concentration of graphene oxide dispersion described in (1) is (0.2~1.5) mg/mL；
Silver nitrate and the molal volume ratio of water are (0.05~0.08) mol in silver nitrate aqueous solution described in step (2)：100mL；
Disodium hydrogen phosphate and the molal volume ratio of water are (0.01~0.03) in the disodium hydrogen phosphate aqueous solution described in step (3)
mol：200mL.
5. the preparation method of graphene oxide/silver phosphate/composite photo-catalyst according to claim 1, it is characterised in that：Step
Suddenly the rotating speed for being stirred described in (2) is 300~500rpm；The speed being added dropwise described in step (2) is 20~30 drops/min；
The speed being added dropwise described in step (3) is 20~30 drops/min；The rotating speed stirred described in step (3) for 300~
500rpm；
The power of ultrasound described in step (1) is 100~200W, and ultrasonic time is 20~40min.
6. the preparation method of graphene oxide/silver phosphate/composite photo-catalyst according to claim 1, it is characterised in that：Step
Suddenly washing described in (3) refers to use distillation water washing, and the drying is 10~14h of vacuum drying under the conditions of 60~80 DEG C.
7. a kind of graphene oxide/silver phosphate/composite photo-catalyst, is prepared by the method described in any one of claim 1~6
Obtain.
8. the graphene oxide/silver phosphate/composite photo-catalyst described in claim 7 in catalytic degradation organic pollution should
With.
9. the application described in claim 8, it is characterised in that：Described organic pollution refers to rhodamine B.
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