CN103908977A - Preparation method and application of magnetic composite photocatalysis material based on graphite-phase carbon nitride - Google Patents
Preparation method and application of magnetic composite photocatalysis material based on graphite-phase carbon nitride Download PDFInfo
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Abstract
The invention aims at providing a preparation method and application of a magnetic composite photocatalysis material based on graphite-phase carbon nitride. The graphite-phase carbon nitride composite photocatalysis material with magnetic separation performance is prepared by employing a metal salt and melamine as precursors and employing a simple sintering process. The magnetism of the composite material can be adjusted and controlled through the addition amount of the metal salt. The obtained graphite-phase carbon nitride magnetic composite photocatalysis material has good magnetic reclaim performance and stability, also has obviously-improved photocatalytic activity under the condition of visible light compared with a simple graphite-phase carbon nitride composite photocatalysis material, also has good separation and cyclic reutilization performances, and is applicable to remove organic pollutants such as dyes or organic micromolecules in water through photocatalysis degradation.
Description
Technical field
The invention belongs to a kind of preparation method based on graphite-phase carbonitride magnetic coupling catalysis material and in the application of removing the organic pollutions such as Wastewater Dyes molecule.
Background technology
Graphite-phase carbon nitride material is a class novel photocatalysis material that obtains in recent years developing rapidly, and this class material is a kind of carboritride of polymerization.With traditional titanium dioxide, the inorganic semiconductor materials such as zinc oxide are compared, and this material has the features such as Stability Analysis of Structures, unique, synthetic method is simple, synthesis condition is gentle.Meanwhile, such material all has broad application prospects at numerous areas such as dyestuff degraded, photolysis water hydrogen and novel sensors.Importantly this type of material can carry out the reaction of degradation of dye under sunshine, can only issue compared with third contact of a total solar or lunar eclipse degradation reaction in ultraviolet light conditions with the obvious advantagely with most of oxides, adds the stability of strong alkali-acid resistance, has greatly improved its industrial application value.About the synthetic existing more bibliographical information of this class material, if the people such as Wang X.C. are at Natural Materials2009 the 8th volume 76-80 page; And the paper delivered at Journal of the American Chemical Society2012 the 134th volume 4393-4397 page of the people such as Du A.J..
Application study for graphite-phase carbon nitride material mainly concentrates on the aspects such as dyestuff degraded, photolysis water hydrogen and novel sensor.Although graphite-phase carbon nitride material has good degradation capability for some organic pollution (as organic dye molecule, phenol etc.) in waste water, but its lower quantum efficiency has limited its practical application, this is due to due to the quick restructuring of photogenerated charge carrying object.Therefore, in order to address this problem, people have made a lot of effort to improve the photocatalytic activity of graphite-phase carbon nitride material, for example by metal or nonmetallic doping, design porous graphite phase carbon nitride material with compound etc. with other photochemical catalysts.But in the time of practical application in industry, want from a large amount of reaction dissolvents, catalysis material to be reclaimed, conventionally adopt method centrifugal and that filter to carry out, equipment investment is large, and operating cost is high.
Summary of the invention
The object of the invention is a kind of preparation method based on graphite-phase carbonitride magnetic coupling catalysis material and the application in light degradation removal Organic Pollutants in Wastewater.By simple heating and calcining method, make graphite-phase carbon nitride material and magnetic-particle compound, not only can improve the photocatalytic activity under absorbability and the visible ray condition of catalysis material to visible ray, and make graphite-phase carbonitride catalysis material there is excellent magnetic recyclability, thereby significantly promote its value in industrial application.Graphite-phase carbonitride magnetic coupling catalysis material of the present invention can be applied to the photocatalytic degradation of the organic pollutions such as organic dyestuff in wastewater molecule and remove.
Technical scheme of the present invention is as follows:
A kind of synthetic method based on graphite-phase carbonitride magnetic coupling catalysis material, it is characterized in that: using slaine and melamine as presoma, through a kind of graphite-phase carbonitride magnetic coupling catalysis material with magnetic separating property of calcining preparation, thereby and magnetic particle embedded and in graphite-phase carbon nitride material, formed a kind of magnetic coupling catalysis material based on graphite-phase carbonitride.
Synthetic method based on graphite-phase carbonitride magnetic coupling catalysis material of the present invention, is characterized in that: described slaine presoma comprises ferric trichloride, ferric nitrate, ferrous sulfate, iron ammonium sulfate etc.The described magnetic intensity based on graphite-phase carbonitride magnetic coupling catalysis material can regulate by the addition of slaine precursor.
Synthetic method based on graphite-phase carbonitride magnetic coupling catalysis material of the present invention, is characterized in that: by simple heat treatment method, make graphite-phase carbon nitride material and magnetic material compound, the callable magnetic coupling catalysis material of preparation magnetic.
Application based on graphite-phase carbonitride magnetic coupling catalysis material of the present invention, it is characterized in that: the organic pollution such as organic dyestuff and organic molecule in degrading waste water, and can photochemical catalyst be reclaimed and be recycled by externally-applied magnetic field.
Application based on graphite-phase carbonitride magnetic coupling catalysis material of the present invention, it is characterized in that: adding of magnetic-particle not only makes graphite-phase carbonitride catalysis material possess magnetic recovery performance, increased the catalytic activity of graphite-phase carbonitride catalysis material under visible ray condition simultaneously.
According to a preferred embodiment of the invention, the precursor reagent slaine using in magnetic modifying process and the mass ratio of melamine are preferably 1: 40 to 1: 200, more preferably 1: 160.
According to a preferred embodiment of the invention, the slaine precursor of certain proportioning and melamine are scattered in a small amount of ethanol under ultrasonic assisting, and dry in 80 degree, then pack in monkey in Muffle furnace 500 ℃ of calcinings after 2 hours again in 520 ℃ of calcinings 2 hours, product is placed in to ethanol washing at least 1 time.The mixture that contains product is by mode conventional in current industrial production, and product separation out, for example Separation of Solid and Liquid, centrifugal, filtration, magnetic separate.After washing, the product obtaining is carried out under convection drying or vacuum condition dry.
The present invention relates to method as above, wherein said dry can be natural drying, can be also bake drying, or not heat or heat drying under vacuum condition, baking temperature is not in principle higher than the decomposition temperature of prepared material.
The invention still further relates to the purposes based on graphite-phase carbonitride magnetic coupling catalysis material obtaining by the inventive method.Because prepared increased magnetic recyclability character based on graphite-phase carbonitride magnetic coupling catalysis material, thereby there is good magnetic recovery and the function of recycling, what obtain by the inventive method in addition, has than the photocatalysis performance under visible ray condition of the better visible absorption character of original graphite-phase carbon nitride material and Geng Gao based on graphite-phase carbonitride magnetic coupling catalysis material.The example of this type of purposes is organic dye molecule and other organic molecules in degrading waste water.Described organic dye molecule can be methyl red, methyl orange, crystal violet, methylene blue, rhodamine B etc.; Described organic molecule can be phenol, hydroquinones, parachlorophenol, Polychlorinated biphenyls etc.
Following examples and accompanying drawing are only implemented example of the present invention for describing in detail, are not used for limiting the scope of the invention.
Accompanying drawing explanation
Fig. 1 has provided the schematic diagram based on graphite-phase carbonitride magnetic coupling catalysis material preparation method of preparing in embodiment 1-5.
Fig. 2 has provided respectively the powder x-ray diffraction figure based on graphite-phase carbonitride magnetic coupling catalysis material 1,2,3,4 and 5 and simple graphite-phase carbon nitride material preparing in embodiment 1-5.
Fig. 3 has provided respectively the thermogravimetric curve figure based on graphite-phase carbonitride magnetic coupling catalysis material 1,2,3,4 and 5 and simple graphite-phase carbon nitride material preparing in embodiment 1-5.
Fig. 4 has provided respectively the hysteresis curve based on graphite-phase carbonitride magnetic coupling catalysis material 1,2,3,4 and 5 of preparing in embodiment 1-5, also comprises the photo that can show visually the magnetic property of composite photocatalyst material 1.
Fig. 5 has provided respectively (high-resolution) transmission electron microscope figure based on graphite-phase carbonitride magnetic coupling catalysis material 1 preparing in representative embodiment 1.
Fig. 6 has provided respectively light absorption figure and the energy band diagram based on graphite-phase carbonitride magnetic coupling catalysis material 1,2,3,4 and 5 and simple graphite-phase carbon nitride material in embodiment 1-5, prepared.
Fig. 7 provided respectively in embodiment 1-5, prepare based on graphite-phase carbonitride magnetic coupling catalysis material 1,2,3,4 and 5 and simple graphite-phase carbon nitride material light degradation property figure to rhdamine B under visible ray.
Fig. 8 has provided respectively the light degradation circulation based on graphite-phase carbonitride magnetic coupling catalysis material 1,2,3,4 and 5 and simple graphite-phase carbon nitride material of preparing in embodiment 1-5, efficiency and reacted x-ray diffraction pattern.
Fig. 9 has provided respectively (high-resolution) transmission electron microscope figure after degradation reaction based on graphite-phase carbonitride magnetic coupling catalysis material preparing in representative embodiment 1.
Figure 10 has provided respectively and can show intuitively the photo of the magnetic separating property under additional magnetic field condition based on graphite-phase carbonitride magnetic coupling catalysis material 1,2,3,4 and 5 of preparing in embodiment 1-5.
The specific embodiment
Embodiment 1
Do not add the graphite-phase carbon nitride material of magnetic, the method providing at Langmuir2009 the 25th volume the 17th phase 10397-10401 page with reference to Zou Z.G etc. is synthetic.Take 2g melamine powder, be put in monkey, then add upper cover and be placed in Muffle furnace, and in 500 ℃ of calcining 2h, then in 520 ℃ of calcining 2h.Prepared product characterizes through powder x-ray diffraction method, and the graphite-phase carbon nitride material of its structure and above-mentioned bibliographical information is identical (sees g-C in Fig. 2
3n
4).
Above-mentioned made graphite-phase carbon nitride material, 150 ℃ of heating in vacuum 12 hours, is obtained sloughing the graphite-phase carbon nitride material of water and other magazine gas, and its structure characterizes and does not change through powder x-ray diffraction method, and its BET specific area is through low temperature N
2adsorption and desorption isotherms is determined as 10m
2/ g, duct is continuous multi-stage artery structure, pore-size distribution mainly concentrates between 25-100nm.
By the synthetic method based on No. 1 sample of graphite-phase carbonitride magnetic coupling catalysis material of simple heating and calcining method be: take 0.0125g FeCl
36H
2o is dissolved in a small amount of ethanol, then takes 2g melamine powder and adds in above-mentioned ferric chloride solution, after ultrasonic auxiliary lower dispersion, puts into 80 ℃, baking oven dry.Afterwards dried mix powder is put in monkey, then adds upper cover and be placed in Muffle furnace and carry out, in 500 ℃ of calcining 2h, then in 520 ℃ of calcining 2h.Prepared product characterizes through powder x-ray diffraction method, shows that product is that the mixing phase of graphite-phase carbon nitride material and iron oxide (is shown in Fe in Fig. 2
2o
3/ g-C
3n
4-1).Product proves through thermogravimetric analysis, the Fe that this product contains 2.8% (mass percent)
2o
3; Saturation magnetization under its room temperature condition is 0.37emug
-1.The energy gap of utilizing UV-Vis DRS spectroscopic data to calculate this photochemical catalyst is 2.5eV; Its BET specific area is through low temperature N
2adsorption and desorption isotherms is determined as 20m
2/ g, duct is continuous multi-stage artery structure, pore-size distribution mainly concentrates between 25-200nm.The lattice fringe spacing of calculating by transmission electron microscope figure has proved the existence of iron oxide particles and graphite-phase carbon nitride material, and iron oxide particles has been evenly dispersed in graphite-phase carbon nitride material (seeing Fig. 5).
Embodiment 2
Take 0.025g FeCl
36H
2o is dissolved in a small amount of ethanol, then takes 2g melamine powder and adds in above-mentioned ferric chloride solution, after ultrasonic auxiliary lower dispersion, puts into 80 ℃, baking oven dry.Afterwards gained powder is placed in to crucible, adds upper cover and be put in Muffle furnace in 500 ℃ of calcining 2h, then in 520 ℃ of calcining 2h.Prepared product characterizes through powder x-ray diffraction method, shows that product is that the mixing phase of graphite-phase carbonitride and iron oxide (is shown in Fe in Fig. 2
2o
3/ g-C
3n
4-2).Product proves through thermogravimetric analysis, the Fe that this product contains 4.9% (mass percent)
2o
3; Saturation magnetization under its room temperature condition is 0.48emu g
-1.The energy gap of utilizing UV-Vis DRS spectroscopic data to calculate this photochemical catalyst is 2.41eV; Its BET specific area is through low temperature N
2adsorption and desorption isotherms is determined as 23m
2/ g, duct is continuous multi-stage artery structure, pore-size distribution mainly concentrates between 50-250nm.
Embodiment 3
Take 0.05g FeCl
36H
2o is dissolved in a small amount of ethanol, then takes 2g melamine powder and adds in above-mentioned ferric chloride solution, after ultrasonic auxiliary lower dispersion, puts into 80 ℃, baking oven dry.Afterwards gained powder is placed in to crucible, with reference to embodiment 2 methods, in 500 ℃ of calcining 2h, then in 520 ℃ of calcining 2h.Prepared product characterizes through powder x-ray diffraction method, shows that product is that the mixing phase of graphite-phase carbonitride and iron oxide (is shown in Fe in Fig. 2
2o
3/ g-C
3n
4-3).Product proves through thermogravimetric analysis, the Fe that this product contains 6.5% (mass percent)
2o
3; Saturation magnetization under its room temperature condition is 0.72emu g
-1.The energy gap of utilizing UV-Vis DRS spectroscopic data to calculate this photochemical catalyst is 2.27eV; Its BET specific area is through low temperature N
2adsorption and desorption isotherms is determined as 24m
2/ g, duct is continuous multi-stage artery structure, pore-size distribution mainly concentrates between 50-200nm.
Embodiment 4
Take 0.1g FeCl
36H
2o is dissolved in a small amount of ethanol, then takes 2g melamine powder and adds in above-mentioned ferric chloride solution, after ultrasonic auxiliary lower dispersion, puts into 80 ℃, baking oven dry.Gained powder is placed in to crucible, with reference to embodiment 2 methods, in 500 ℃ of calcining 2h, then in 520 ℃ of calcining 2h.Prepared product characterizes through powder x-ray diffraction method, shows that product is that the mixing phase of graphite-phase carbonitride and iron oxide (is shown in Fe in Fig. 2
2o
3/ g-C
3n
4-4).Product proves through thermogravimetric analysis, the Fe that this product contains 8.0% (mass percent)
2o
3; Saturation magnetization under its room temperature condition is 1.26emu g
-1.The energy gap of utilizing UV-Vis DRS spectroscopic data to calculate this photochemical catalyst is 2.09eV; Its BET specific area is through low temperature N
2adsorption and desorption isotherms is determined as 23m
2/ g, duct is continuous multi-stage artery structure, pore-size distribution mainly concentrates between 25-200nm.
Embodiment 5
Take 0.2g FeCl
36H
2o is dissolved in a small amount of ethanol, then takes 2g melamine powder and adds in above-mentioned ferric chloride solution, after ultrasonic auxiliary lower self-dispersing, puts into 80 ℃, baking oven dry.With reference to embodiment 2 methods, in 500 ℃ of calcining 2h, then in 520 ℃ of calcining 2h.Prepared product characterizes through powder x-ray diffraction method, shows that product is that the mixing phase of graphite-phase carbonitride and iron oxide (is shown in Fe in Fig. 2
2o
3/ g-C
3n
4-5).Product proves through thermogravimetric analysis, the Fe that this product contains 11.6% (mass percent)
2o
3; Saturation magnetization under its room temperature condition is 1.56emug
-1.The energy gap of utilizing UV-Vis DRS spectroscopic data to calculate this photochemical catalyst is 1.66eV; Its BET specific area is through low temperature N
2adsorption and desorption isotherms is determined as 10m
2/ g, duct is continuous multi-stage artery structure, pore-size distribution mainly concentrates between 25-200nm.
Embodiment 6
Take respectively in 50mg embodiment 1-5 prepared based on graphite-phase carbonitride magnetic coupling catalysis material, be placed in 60mL, in the rhodamine B aqueous solution of 5mg/L, under the condition of magnetic agitation, stir in the dark and within 60 minutes, make its absorption saturated, then be to irradiate and carry out light-catalyzed reaction under the visible ray of 500W xenon lamp at power, before measuring its absorbance and react with ultraviolet specrophotometer, the ratio of original absorbance is with the variation relation in reaction time, thereby the concentration of inferring rhodamine B in reaction solution with react before the ratio of original concentration with the variation relation (seeing Fig. 7) in reaction time, the light-catalyzed reaction time that can find out graphite-phase carbonitride magnetic coupling catalysis material 1 and 2 is less than simple graphite-phase carbon nitride material, and the light-catalyzed reaction time of composite photocatalyst material 3-5 is greater than simple graphite-phase carbon nitride material, show that composite 1 and 2 is having more excellent photocatalytic activity.Experimental result meets First-order kinetics equation (ln (C/C
0)=kt, t is the light-catalyzed reaction time, C and C
0dyes concentration when being respectively reaction time t and reacting initial, k is reaction rate constant), be respectively 0.036 by calculating graphite-phase carbonitride magnetic coupling catalysis material 1-5 with the reaction rate constant (k value) of simple graphite-phase carbon nitride material, 0.028,0.017,0.009,0.004 and 0.020min
-1, the photocatalytic activity of composite photocatalyst material 1 is the highest, and its reaction rate constant value is 1.8 times of simple graphite-phase carbon nitride materials.
Embodiment 7
In order to check the stability of graphite-phase carbonitride magnetic coupling catalysis material, use prepared composite 1 in embodiment 1 to carry out three circular responses (seeing Fig. 8 and 9), Fig. 8 shows that the photocatalysis efficiency of magnetic coupling catalysis material after three circular responses has only reduced by 1.5%, and reacted x-ray diffraction pattern has shown that obvious broadening phenomenon does not occur this material.After Fig. 9 has shown three circular responses, magnetic particle is still embedded in graphite-phase carbon nitride material equably.Therefore, graphite-phase carbonitride magnetic coupling catalysis material is having excellent photocatalysis stability.
Embodiment 8
Take respectively in a certain amount of embodiment 1-5 prepared based on graphite-phase carbonitride magnetic coupling catalysis material and simple graphite-phase carbon nitride material, and pack in vial, then vial is inverted, place a small magnet in bottle bottom, can see that graphite-phase carbonitride magnetic coupling catalysis material 1-5 is adsorbed on vial bottom (as Figure 10), has shown that fabulous magnetic separates callable performance.
Claims (6)
1. the synthetic method based on graphite-phase carbonitride magnetic coupling catalysis material, is characterized in that: using slaine and melamine as presoma, through a kind of graphite-phase carbonitride magnetic coupling catalysis material with magnetic separating property of calcining preparation.
2. according to claim 1 based on graphite-phase carbonitride magnetic coupling catalysis material, it is characterized in that: described slaine presoma comprises ferric trichloride, ferric nitrate, ferrous sulfate, iron ammonium sulfate etc.The described magnetic intensity based on graphite-phase carbonitride magnetic coupling catalysis material can regulate by the addition of slaine precursor.
3. according to claim 1 and the synthetic method based on graphite-phase carbonitride magnetic coupling catalysis material claimed in claim 2, it is characterized in that: by add slaine presoma in melamine reactant, by simple calcining processing method, prepare the recyclable composite photocatalyst material of magnetic based on graphite-phase carbonitride.
4. claim 1 and the application based on graphite-phase carbonitride magnetic coupling catalysis material claimed in claim 2, is characterized in that: the organic pollution such as dyestuff and organic molecule being used in degraded removal waste water.
5. claim 1 and the application based on graphite-phase carbonitride magnetic coupling catalysis material claimed in claim 2, is characterized in that: can be reclaimed and be recycled by the method for externally-applied magnetic field.
6. the application based on graphite-phase carbonitride magnetic coupling catalysis material claimed in claim 4, it is characterized in that: adding of magnetic-particle not only makes graphite-phase carbonitride catalysis material possess magnetic recovery performance, increased the catalytic activity of graphite-phase carbonitride catalysis material under visible ray condition simultaneously.
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