CN110280295A - A kind of g-C3N4Base composite photocatalyst material and preparation method thereof - Google Patents
A kind of g-C3N4Base composite photocatalyst material and preparation method thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 34
- 239000002131 composite material Substances 0.000 title claims abstract description 20
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 20
- 229910003145 α-Fe2O3 Inorganic materials 0.000 claims abstract description 66
- 238000003756 stirring Methods 0.000 claims abstract description 18
- 239000000725 suspension Substances 0.000 claims abstract description 11
- 230000001699 photocatalysis Effects 0.000 claims abstract description 9
- 238000007146 photocatalysis Methods 0.000 claims abstract description 7
- 238000006555 catalytic reaction Methods 0.000 claims abstract description 6
- 150000001875 compounds Chemical class 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 26
- 239000008367 deionised water Substances 0.000 claims description 19
- 229910021641 deionized water Inorganic materials 0.000 claims description 19
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 14
- 239000004202 carbamide Substances 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 14
- 239000000843 powder Substances 0.000 claims description 11
- 239000000243 solution Substances 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 230000001376 precipitating effect Effects 0.000 claims description 7
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 235000019441 ethanol Nutrition 0.000 claims description 6
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 5
- 238000001354 calcination Methods 0.000 claims description 4
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 4
- 238000010792 warming Methods 0.000 claims description 4
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 3
- 239000012467 final product Substances 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- 238000003837 high-temperature calcination Methods 0.000 claims description 2
- 229910021382 natural graphite Inorganic materials 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 239000013049 sediment Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 6
- 230000015556 catabolic process Effects 0.000 abstract description 5
- 238000006731 degradation reaction Methods 0.000 abstract description 5
- 230000003287 optical effect Effects 0.000 abstract description 3
- 230000004044 response Effects 0.000 abstract description 3
- 239000000975 dye Substances 0.000 abstract description 2
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- 238000010586 diagram Methods 0.000 description 8
- 239000002585 base Substances 0.000 description 7
- 238000010521 absorption reaction Methods 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 239000012153 distilled water Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 229910000859 α-Fe Inorganic materials 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 239000004570 mortar (masonry) Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000001291 vacuum drying Methods 0.000 description 3
- 206010013786 Dry skin Diseases 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 238000013019 agitation Methods 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 230000005281 excited state Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 238000010907 mechanical stirring Methods 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 238000003911 water pollution Methods 0.000 description 2
- JYEUMXHLPRZUAT-UHFFFAOYSA-N 1,2,3-triazine Chemical compound C1=CN=NN=C1 JYEUMXHLPRZUAT-UHFFFAOYSA-N 0.000 description 1
- 229910017135 Fe—O Inorganic materials 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 244000178870 Lavandula angustifolia Species 0.000 description 1
- 235000010663 Lavandula angustifolia Nutrition 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000001491 aromatic compounds Chemical class 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 238000000502 dialysis Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- YWEUIGNSBFLMFL-UHFFFAOYSA-N diphosphonate Chemical compound O=P(=O)OP(=O)=O YWEUIGNSBFLMFL-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 239000008236 heating water Substances 0.000 description 1
- 239000005457 ice water Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000001102 lavandula vera Substances 0.000 description 1
- 235000018219 lavender Nutrition 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000001473 noxious 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
- 230000037361 pathway Effects 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
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 239000000049 pigment Substances 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
- 239000002244 precipitate Substances 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 239000002699 waste material Substances 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
- B01J27/24—Nitrogen compounds
-
- B01J35/33—
-
- B01J35/39—
Abstract
The present invention relates to a kind of g-C3N4Base composite photocatalyst material comprising following material: g-C3N4、α‑Fe2O3And RGO, the α-Fe2O3It is dispersed in g-C3N4Surface, the α-Fe2O3With g-C3N4Between be interspersed with RGO；And it is related to g-C3N4The preparation method of base composite photocatalyst material, this method is by g-C3N4With α-Fe2O3It mixes by stirring, obtains g-C3N4/α‑Fe2O3The suspension of binary complex；GO is dispersed in suspension later；GO is finally reduced into RGO to get g-C3N4/α‑Fe2O3/ RGO tri compound catalysis material.The g-C provided in above-mentioned technical proposal3N4Base composite photocatalyst material, optical response range is wide, high to organic dyestuff RhB degradation efficiency, and photocatalysis performance is excellent；Preparation method is easy to operate, low in cost, few using equipment, green and pollution-free, it can be achieved that large-scale production.
Description
Technical field
The present invention relates to catalysis material technical fields, and in particular to a kind of g-C3N4/α-Fe2O3/ RGO composite photocatalyst
Material and preparation method thereof.
Background technique
With economic continuous development, environment and problem of energy crisis become to be on the rise, environmental pollution can be divided into
Under several classes: water pollution, air pollution, noxious waste pollution and noise pollution etc., wherein water pollution situation is the severeest.Too
It is positive to be used as clean energy resource, not only can freely using, exempt to transport, but also it is environmentally friendly, be the base of realization sustainable development
Plinth.From TiO in 19722Since the phenomenon that semi-conducting electrode photochemical catalyzing, finds, application of the semiconductor in photocatalysis field
Extensive research is obtained.It is also most widely used catalysis material that conductor photocatalysis material, which is instantly most stable, generally may be used
It is divided into following a few classes: metal oxide；Multi-component oxide；Nitrogen oxides；Metal sulfide；Bismuth system oxide；Laminated metal
Oxide；Silverbased compound；Organic matter semiconductor material.
In recent years, g-C3N4(carboritride of graphite-phase) because excellent properties in terms of photocatalytic degradation and by
It welcomes.Firstly, g-C3N4Semiconductor material be it is visible light-responded, band gap is relatively narrow, about 2.7ev (energy position of CB and VB difference
- 1.1ev and 1.6ev).In addition, g-C3N4Also with strong heat resistance, resistance to acid and alkali, itself is nontoxic, low in cost and easy
The features such as acquisition, but since the photo-generate electron-hole of single semiconductor material is fast to recombination velocity, quantum efficiency is low and to light
Utilization rate it is low, cause its photocatalytic activity lower.
α-Fe2O3Due to cheap price, stronger resistance to corrosion, stable chemical property and environmental-friendly etc.
Advantage is usually applied to the fields such as pigment, catalyst.α-Fe2O3Band-gap energy is about 2.2eV, is less than or equal to wave-length coverage
The light of 564nm has sink effect, and this wave-length coverage is in sunlight wave band, so iron oxide has good absorption to sunlight
Effect is a kind of efficient photochemical catalyst.However, α-the Fe of one-component2O3There are hole diffusion lengths short, photo-generated carrier
Transmittability is weak, the excited state lower service life is short and it is poor to the absorbability of light the defects of.
Summary of the invention
The object of the present invention is to provide a kind of g-C3N4Base composite photocatalyst material and preparation method thereof, can effectively solve
Existing single semiconductor material photocatalytic activity is lower, and the single photochemical catalyst excited state lower service life is short and suction to light
The problems such as receipts ability is poor.
In order to solve the above technical problems, the invention adopts the following technical scheme:
A kind of g-C3N4Base composite photocatalyst material, including following material: g-C3N4、α-Fe2O3And RGO, the α-Fe2O3
It is dispersed in g-C3N4Surface, the α-Fe2O3With g-C3N4Between be interspersed with RGO.
Preferably, the g-C3N4For loose irregular sheet；α-the Fe2O3For side length is 0.5~1.5 μm six
It is angular；The RGO is film-form.
Preferably, the g-C3N4With α-Fe2O3Weight ratio be 38:3.
Preferably, the weight of the RGO accounts for g-C3N4/α-Fe2O3The 5% of binary complex weight.
And provide above-mentioned g-C3N4The preparation method of base composite photocatalyst material, comprising the following steps:
(1)g-C3N4Preparation
Weigh urea and deionized water, urea be dissolved in deionized water, stirring to forming homogeneous aqueous solution of urea,
Aqueous solution of urea is transferred in crucible later and is put into Muffle furnace high-temperature calcination, after muffle furnace cooled to room temperature,
The block in crucible is taken out, grinding obtains faint yellow g-C3N4Powder；
(2)α-Fe2O3Preparation
It weighs ferric nitrate and sodium hydroxide is dissolved in deionized water, gained suspension is transferred to reaction vessel after stirring
In 148~152 DEG C, heat preservation 10~12h washed repeatedly after reaction vessel cooled to room temperature with deionized water and ethyl alcohol
It precipitates and dries, the powder after drying is calcined in Muffle furnace, after muffle furnace cooled to room temperature, i.e. acquisition α-
Fe2O3；
(3)g-C3N4/α-Fe2O3Preparation
By the above-mentioned g-C prepared3N4With α-Fe2O3Mixing ultrasonic disperse filters out precipitating in deionized water, after stirring
And it is dry, the blocks of solid after mill-drying is later up to g-C3N4/α-Fe2O3；
(4) preparation of GO
Using natural graphite as raw material, GO is prepared using improved Hummers method；GO obtained is added in deionized water and is surpassed
Sound disperses to obtain GO suspension；
(5)g-C3N4/α-Fe2O3The preparation of/RGO
By the g-C of above-mentioned preparation3N4/α-Fe2O3It is dispersed in GO suspension, hydrazine hydrate is added after stirring, continue to stir,
The solution after stirring is filtered out into precipitating later, washing, alcohol are dry after washing, and the blocks of solid after mill-drying is to get to finally
Product g-C3N4/α-Fe2O3/RGO。
In step (1), the mass ratio of urea and deionized water is 3:4；Muffle furnace calcining temperature schedule be with 15 DEG C/
The heating rate of min keeps the temperature 1h after being warming up to 400 DEG C, then rises to 500 DEG C with same heating rate, keeps the temperature naturally cold after 2h
But.
In step (2), the temperature schedule of Muffle furnace calcining is that 280 DEG C are warming up to the heating rate of 5 DEG C/min, heat preservation
Natural cooling after 0.5h；Mixing time is 30~40min, and drying condition is dry 24~36h at 60 DEG C.
Mixing time is 10~12h in step (3), and drying condition is dry 24~36h at 60 DEG C.
Stirring condition is that 10~12h is stirred at 95 DEG C in step (5), and drying condition is dry 24~36h at 60 DEG C.
The g-C provided in above-mentioned technical proposal3N4Base composite photocatalyst material, optical response range is wide, to organic dyestuff RhB
Degradation efficiency is high, and photocatalysis performance is excellent；And the g-C of its offer3N4The preparation method of base composite photocatalyst material, by by g-
C3N4With α-Fe2O3It is compound, hetero-junctions is formed, the optical response range of photochemical catalyst has effectively been widened, has made g-C3N4Under visible light
Photocatalysis efficiency enhancing；On this basis by RGO and g-C3N4/α-Fe2O3Compound, film-form RGO is interspersed in α-Fe2O3With g-
C3N4Between, electron transfer pathways are provided, the quantum efficiency of catalysis material is effectively improved, inhibit the compound of electron hole pair,
To improve its light-catalyzed reaction rate.
Detailed description of the invention
Fig. 1 a is g-C single in the embodiment of the present invention3N4XRD diagram；
Fig. 1 b is α-Fe in the embodiment of the present invention2O3XRD diagram；
Fig. 1 c is g-C in the embodiment of the present invention3N4/α-Fe2O3XRD diagram；
Fig. 1 d is g-C in the embodiment of the present invention3N4/α-Fe2O3The XRD diagram of/RGO；
Fig. 2 a is single g-C in the embodiment of the present invention3N4Infrared spectrogram；
Fig. 2 b is g-C in the embodiment of the present invention3N4/α-Fe2O3Infrared spectrogram；
Fig. 2 c is g-C in the embodiment of the present invention3N4/α-Fe2O3The infrared spectrogram of/RGO；
Fig. 3 a, 3b are g-C in the embodiment of the present invention3N4/α-Fe2O3The SEM of/RGO schemes；
Fig. 3 c, 3d are g-C in the embodiment of the present invention3N4/α-Fe2O3The EDS of/RGO schemes；
Fig. 4 is g-C in the embodiment of the present invention3N4/α-Fe2O3The ultraviolet spectrogram of/RGO.
Specific embodiment
In order to which objects and advantages of the present invention are more clearly understood, the present invention is carried out specifically with reference to embodiments
It is bright.It should be appreciated that following text is only used to describe one or more of specific embodiments of the invention, not to the present invention
The protection scope specifically requested carries out considered critical.
With the following Examples, to g-C3N4The preparation method of base composite photocatalyst material is described in detail.
(1)g-C3N4Preparation
12g urea and 16ml deionized water (mass ratio 3:4) are weighed, load weighted urea is dissolved in deionized water
In, homogeneous aqueous solution of urea is formed after magnetic agitation half an hour；Muffle is put into after above-mentioned aqueous solution of urea is transferred to crucible
In furnace, crucible cover is warming up to after 400 DEG C with the heating rate of 15 DEG C/min after covering tightly and keeps the temperature 1h, then with same heating rate liter
To 500 DEG C, and keep the temperature 2h；After muffle furnace cooled to room temperature, the block in crucible is taken out, is ground with agate mortar
Mill, obtains the faint yellow g-C of fluffy lightweight3N4Powder.
(2)α-Fe2O3Preparation
It is that 1:50 weighs 1.212g ferric nitrate respectively and 10.0g sodium hydroxide is dissolved in 150ml deionization according to molar ratio
In water, after magnetic agitation 30min, gained suspension is transferred in the polytetrafluoroethyllining lining of 250ml, lid closes reaction under high pressure
Kettle is heated to 150 DEG C (rate of heat addition is 1.5 DEG C/min), keeps the temperature 12h；After reaction vessel cooled to room temperature, spend from
Sub- water and ethyl alcohol wash precipitating repeatedly, later in a vacuum drying oven at 60 DEG C it is dry for 24 hours, it is dry after powder in Muffle furnace
280 DEG C are raised to the heating rate of 5 DEG C/min, and keeps the temperature 0.5h, after muffle furnace cooled to room temperature, that is, is obtained red
Porous α-the Fe of brown2O3Nanometer rods.
(3)g-C3N4/α-Fe2O3Preparation
Weigh the g-C of 3.8g respectively according to mass ratio 38:33N4With the α-Fe of 0.3g2O3, the two is mixed into ultrasonic disperse and is existed
In deionized water solution.After vigorous magnetic stirs 12h, precipitating is filtered out, 60 DEG C of dryings are for 24 hours, dry in a vacuum drying oven
Blocks of solid afterwards is ground with agate mortar, obtains lavender g-C3N4/α-Fe2O3。
(4) preparation of GO
By the graphite powder of 3.0g, the potassium peroxydisulfate of 2.5g and the phosphorus pentoxide of 2.5g are added sequentially to the concentrated sulfuric acid of 12ml
In, 6h is kept the temperature under conditions of 80 DEG C of heating water baths, solution is diluted with 200ml distilled water.After standing 12h, is filtered and be used in combination
A large amount of distillation water washings to filtrate is neutrality, and product is dried at 40 DEG C to constant weight.The dense sulphur of 120ml is added in above-mentioned powder
30min is stirred in acid to be allowed to uniformly, and 30g potassium permanganate (being gradually added into, control time 30min) is slowly added under ice-water bath
Control system temperature is no more than 20 DEG C in the whole process.200ml distilled water is then slowly added into system with constant pressure funnel,
Then 2h is reacted, control system temperature is no more than 50 DEG C, switchs to cyan again when liquid upper air switchs to brown from red.Again plus
Enter the distilled water of 500ml and 30% hydrogen peroxide of 30ml is added dropwise and terminate reaction, solution switchs to bright brown at this time.Product centrifugation
It is washed afterwards with dilute hydrochloric acid solution, finally removes remaining metal ion and acid with distilled water dialysis.Finally, GO solution is freezed dry
It is dry at GO powder.
(5)g-C3N4/α-Fe2O3The preparation of/RGO
Weigh the g-C of the above-mentioned preparation of 4g3N4/α-Fe2O3Powder and 0.2g GO powder ultrasonic are dispersed in deionized water solution
In, it is added after mechanical stirring 1h hydrazine hydrate (quality is the 80% of GO powder quality), mechanical stirring 12h at 95 DEG C, after stirring
Solution filters out precipitating, washs precipitating repeatedly with deionized water and ethyl alcohol, in a vacuum drying oven 60 DEG C of dryings for 24 hours, after dry
Blocks of solid ground with agate mortar, obtain final product g-C3N4/α-Fe2O3/RGO。
Fig. 1 a is g-C single in embodiment3N4XRD diagram, have apparent feature at 13.11 ° and 27.31 °
Peak respectively corresponds (100) and (002) crystal face, the two characteristic diffraction peaks and g-C3N4Standard pdf card (JCPDS NO.87-
1526) characteristic diffraction peak matches；Fig. 1 b is the α-Fe in embodiment2O3XRD diagram, characteristic peak and α-Fe in figure2O3Mark
The characteristic diffraction peak of quasi- card (JCPDS NO.33-0664) matches, and peak shape is sharp, without miscellaneous peak, shows in embodiment
α-Fe2O3It is successfully prepared and crystallinity is good；Fig. 1 c is the g-C in embodiment3N4/α-Fe2O3XRD diagram, feature in figure
Peak and the characteristic peak of Fig. 1 a and Fig. 1 b can correspond, and without miscellaneous peak, show g-C in embodiment3N4/α-Fe2O3By success
There is no miscellaneous phases for preparation；Fig. 1 d is the g-C in embodiment3N4/α-Fe2O3The XRD diagram of/RGO, since the volume of RGO is seldom, and
Its characteristic peak and g-C3N4Characteristic peak at 27.31 ° is overlapped, and leads to the characteristic peak for failing to show RGO in figure.
Fig. 2 a is single g-C in embodiment3N4Infrared spectrogram, from the figure, it can be seen that 3419.07cm-1Neighbouring
Broad absorption band is attributed to the stretching vibration of N-H key, 254.82cm-1、1329.77cm-1And 1422.80cm-1Corresponding aromatic compound
In sp3C-N key stretching vibration, 1630.62cm-1Absorption peak corresponds to sp2The stretching vibration of C=N, 811.01cm-1Absorption peak pair
What is answered is skeleton stretching vibration outside the face of triazine；Fig. 2 b is g-C in embodiment3N4/α-Fe2O3Infrared spectrogram, with Fig. 2 a phase
Than the 536.86cm of appearance-1And 462.48cm-1Two absorption peaks are attributed to the stretching vibration of Fe-O key；Fig. 2 c is in embodiment
g-C3N4/α-Fe2O3The infrared spectrogram of/RGO, 1602.88cm in figure-1The absorption peak of enhancing is attributed to graphene oxide also
Former process can not repair oxidation process defect caused by graphene sheet layer, and the RGO after reduction can not be restored to the original of graphite
Beginning state.
Fig. 3 a and Fig. 3 b are g-C in embodiment3N4/α-Fe2O3The SEM of/RGO schemes, and Fig. 3 c and Fig. 3 d are g- in embodiment
C3N4/α-Fe2O3The EDS of/RGO schemes, visible g-C in figure3N4Show porous loose laminated structure, hexagon α-Fe2O3Dispersion
In the g-C of sheet3N4Surface, between the two with the RGO fragment of film-form, by g-C3N4With α-Fe2O3It spreads out, plays anti-
The only effect of reunion and transmission electronics；Region a certain on sample a little sweep with the energy disperse spectroscopy in scanning electron microscope, to sample
Product carry out qualitative elementary, as a result as shown in Figure 3d, it is seen that contain C element, N element, Fe element, O element in sample, each element is equal
It is detected, while occurring without other impurities, match with the result of XRD.
Weigh the g-C in 0.015g embodiment3N4/α-Fe2O3/ RGO is dispersed in 50ml RhB solution (10mg/L), secretly
After reacting 30min, degradation experiment is carried out under the irradiation of 400W Metal halogen lamp.A sample was taken at interval of 10 minutes in experiment, until
Solution becomes colorless transparent, and the sample of acquirement is centrifuged (6000r/min, 3min), takes supernatant liquor.Use uv-spectrophotometric
Meter is tested, g-C3N4/α-Fe2O3The catalytic performance of/RGO is as shown in figure 4, Fig. 4 is g-C3N4/α-Fe2O3The ultraviolet light of/RGO
Spectrogram, it can be seen that with the growth of time, in g-C3N4/α-Fe2O3Under the degradation of/RGO catalyst, RhB concentration continues
It reduces, after the 50min that degrades, RhB degradation rate has reached 95.8%.
Above in conjunction with embodiment, the embodiments of the present invention are described in detail, but the present invention is not limited to above-mentioned realities
Mode is applied, for those skilled in the art, in knowing the present invention after contents, is not departing from this hair
Under the premise of bright principle, several same transformation and substitution can also be made to it, these convert and substitute on an equal basis and also should be regarded as belonging to
In protection scope of the present invention.
Claims (10)
1. a kind of g-C3N4Base composite photocatalyst material, which is characterized in that including following material: g-C3N4、α-Fe2O3And RGO, institute
State α-Fe2O3It is dispersed in g-C3N4Surface, the α-Fe2O3With g-C3N4Between be interspersed with RGO.
2. g-C according to claim 13N4Base composite photocatalyst material, it is characterised in that: the g-C3N4For it is loose not
Regular sheet；α-the Fe2O3The hexagon for being 0.5~1.5 μm for side length；The RGO is film-form.
3. g-C according to claim 13N4Base composite photocatalyst material, it is characterised in that: the g-C3N4With α-Fe2O3
Weight ratio be 38:3.
4. g-C according to claim 13N4Base composite photocatalyst material, it is characterised in that: the weight of the RGO accounts for g-
C3N4/α-Fe2O3The 5% of binary complex weight.
5. g-C according to any one of claims 1 to 43N4The preparation method of base composite photocatalyst material, it is characterised in that:
By g-C3N4With α-Fe2O3It mixes by stirring, obtains g-C3N4/α-Fe2O3The suspension of binary complex；It is later that GO is uniform
It is scattered in suspension；GO is finally reduced into RGO to get g-C3N4/α-Fe2O3/ RGO tri compound catalysis material.
6. g-C according to claim 53N4The preparation method of base composite photocatalyst material, which is characterized in that including following
Step:
(1)g-C3N4Preparation
Urea and deionized water are weighed, urea is dissolved in deionized water, is stirred to homogeneous aqueous solution of urea is formed, later
Aqueous solution of urea is transferred in crucible and is put into Muffle furnace high-temperature calcination, after muffle furnace cooled to room temperature, is taken out
Block in crucible, grinding obtain g-C3N4Powder；
(2)α-Fe2O3Preparation
It weighs ferric nitrate and sodium hydroxide is dissolved in deionized water, gained suspension is transferred in reaction vessel after stirring
10~12h is kept the temperature at 148~152 DEG C, after reaction vessel cooled to room temperature, it is heavy to be washed repeatedly with deionized water and ethyl alcohol
It forms sediment and dries, the powder after drying is calcined in Muffle furnace, after muffle furnace cooled to room temperature, i.e. acquisition α-
Fe2O3；
(3)g-C3N4/α-Fe2O3Preparation
By the above-mentioned g-C prepared3N4With α-Fe2O3Mixing ultrasonic disperse filters out in deionized water, after stirring to be precipitated and does
Dry, the blocks of solid after mill-drying is later up to g-C3N4/α-Fe2O3；
(4) preparation of GO
GO is prepared by raw material of natural graphite；Ultrasonic disperse in deionized water is added in GO obtained and obtains GO suspension；
(5)g-C3N4/α-Fe2O3The preparation of/RGO
By the g-C of above-mentioned preparation3N4/α-Fe2O3It is dispersed in GO suspension, hydrazine hydrate is added after stirring, continue to stir, later will
Solution after stirring filters out precipitating, and washing, alcohol are dry after washing, and the blocks of solid after mill-drying is to get arriving final product g-
C3N4/α-Fe2O3/RGO。
7. g-C according to claim 63N4The preparation method of base composite photocatalyst material, it is characterised in that: step (1)
In, the mass ratio of urea and deionized water is 3:4；The temperature schedule of Muffle furnace calcining is to be heated up with the heating rate of 15 DEG C/min
1h is kept the temperature after to 400 DEG C, then rises to 500 DEG C with same heating rate, keeps the temperature natural cooling after 2h.
8. g-C according to claim 63N4The preparation method of base composite photocatalyst material, it is characterised in that: step (2)
In, the temperature schedule of Muffle furnace calcining is that 280 DEG C are warming up to the heating rate of 5 DEG C/min, keeps the temperature natural cooling after 0.5h；It stirs
Mixing the time is 30~40min, and drying condition is dry 24~36h at 60 DEG C.
9. g-C according to claim 63N4The preparation method of base visible-light photocatalysis material, it is characterised in that: step (3)
Middle mixing time is 10~12h, and drying condition is dry 24~36h at 60 DEG C.
10. g-C according to claim 63N4The preparation method of base visible-light photocatalysis material, it is characterised in that: step
(5) stirring condition is that 10~12h is stirred at 95 DEG C in, and drying condition is dry 24~36h at 60 DEG C.
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