CN103769213A - Preparation method for phosphor-doped graphite-phase carbon nitride visible-light catalyst - Google Patents
Preparation method for phosphor-doped graphite-phase carbon nitride visible-light catalyst Download PDFInfo
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Abstract
The invention belongs to the technical field of environment purification photocatalytic material and discloses a preparation method for a phosphor-doped graphite-phase carbon nitride visible-light catalyst. The method comprises the following steps: dispersing melamine into a dilute phosphoric acid solution to enable phosphoric acid molecules to be uniformly adsorbed and dispersed to the surface of melamine particles; then heating to remove solvent water, and after the melamine particles are fully dried, performing programmed heating on the dried melamine particles to 520 DEG C to enable the melamine to generate thermal polycondensation; and cooling and grinding a product to obtain the phosphor-doped graphite-phase carbon nitride visible-light catalyst. The raw materials of the phosphor-doped graphite-phase carbon nitride visible-light catalyst are readily available; the preparation method is simple; complicated equipment is not needed; the preparation method is suitable for large-scale production; the prepared phosphor-doped graphite-phase carbon nitride composite visible-light catalyst is high in visible-light catalysis performance and high in catalysis stability.
Description
Technical field
The present invention is specifically related to a kind of preparation method of phosphorus doping graphite-phase carbonitride visible light catalyst, belongs to depollution of environment photocatalyst material preparing technical field.
Background technology
Photocatalysis technology is a kind of green technology that has important application prospect at energy field, and photocatalysis oxidation technique, take semiconductor as catalyst, take luminous energy as the energy, is carbon dioxide and water by organic pollutant degradation.Find that from 1972 nano titanium oxide can be at decomposition water under illumination, Nano semiconductor photocatalysis technology has caused the extensive concern in the world, and is considered to the depollution of environment technology of tool development prospect and application prospect.In recent years, many Chinese scholars have been carried out research deeply and widely to polytype nano semiconductor material such as metal oxide, sulfide, nitride, but the problems such as the quantum efficiency of photochemical catalyst is low, sunshine utilization rate is low are not solved yet at all, restricting the extensive use of photocatalysis technology, therefore the high-efficiency photocatalysis material of the visible light-inducing of searching and synthesizing new is the important topic of photocatalysis field always.
Recently, (the Xinchen Wang et al. such as Wang Xinchen, A metal-free polymeric photocatalyst for hydrogen production from water under visible light.Nature Materials, 2009,8:76-80) find graphite-phase carbonitride energy hydrogen production by water decomposition under radiation of visible light, and there is good stability, cheap and easy to get, structure is easy to the advantages such as regulation and control, is the potential novel visible catalysis material of a class.But be subject to its structure and band gap limits, pure graphite-phase carbonitride has the limitation that self cannot break through in actual application, as large (2.7eV) of energy gap, light absorption mainly concentrates on visible region (λ < 450nm), lower to the utilization rate of sunshine; The light induced electron producing after optical excitation and hole are easy to compound, and the efficiency of photo-generated carrier is low, and photocatalysis performance is poor etc.
In order to improve visible light catalysis activity and the catalytic stability of graphite-phase carbonitride, researcher has carried out the study on the modification of a series of graphite-phase carbonitrides.Shubin Yang(Shubin Yang et al., Exfoliated graphitic carbon nitride nanosheets as efficient catalysts for hydrogen evolution under visible light.Advanced Materials, 2013,25:2452-2456) adopt the synthetic thick about 2nm of graphite-phase carbonitride thin layer of layer stripping, there is larger length-width ratio, higher specific area and carbon-nitrogen ratio, this is not only conducive to provide more hydrogen production activity center, and can increase electric charge transmission and reduce light the restructuring ability that swashs charge carrier.Guigang Zhang(Guigang Zhang, Polycondensation of thiourea into carbon nitride semiconductors as visible light photocatalysts.Journal of Materials Chemistry, 2012, 22:8083-8091) with the synthetic sulfur doping graphite-phase carbonitride semi-conducting material of hetero atom regulation and control thermal polymerization, increase specific area, it is cancellated synthetic that the introducing of sulphur can be controlled graphite-phase carbonitride, accelerate the process of graphite-phase carbonitride polymerization, control heating-up temperature and can generate nano-scale, can synthetic there is better structure, the carbonitride semi-conducting material of electronics and optical property.Wang Xinchen etc. (Chinese invention patent CN103272639A) have prepared polymeric modification graphite-phase azotized carbon nano sheet visible light catalyst, and this catalyst has high-specific surface area, narrow band gap width, photo-generated carrier separation fast, transfer ability.The visible light catalyst of above-mentioned modification has effectively improved graphite-phase carbonitride specific area, more activity site is provided, improve utilization rate to visible ray, but also limited absorption and the utilization of visible ray, improve limited to the photocatalytic activity of degradation of contaminant.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of preparation method of phosphorus doping graphite-phase carbonitride visible light catalyst.Phosphorus doping graphite-phase carbonitride prepared by the present invention has good photocatalytic activity and photocatalysis stability, and the visible light catalyst standby with this legal system will have broad application prospects in depollution of environment photocatalysis field.
For solving the problems of the technologies described above technical scheme of the present invention be, first by melamine microparticulate in the phosphoric acid,diluted aqueous solution, make phosphoric acid molecules evenly be adsorbed on melamine microparticle surfaces, then heating is except anhydrating, after dry, mixture is through temperature programming to 520 ℃, it is occurred after the serial reactions such as polycondensation, and product, through cooling, grinding, obtains phosphorus doping graphite-phase carbonitride visible light catalyst.
The preparation method of described a kind of phosphorus doping graphite-phase carbonitride visible light catalyst mainly comprises the steps:
A. measure 85% SPA 2mL～8mL and move in 100mL volumetric flask, add deionized water and be made into the dilute phosphoric acid solution that concentration is 0.292mol/L～1.17mol/L;
B. described in removing step a, dilute phosphoric acid solution 0.25mL～3.0mL joins in the beaker that contains 5mL deionized water, stir 5min～10min, under agitation 5.00g melamine pressed powder is slowly added in this dilute phosphoric acid solution afterwards, making the mol ratio of phosphoric acid and melamine in solution is 1:100～1:20, continue to stir 20min～60min, make phosphoric acid evenly adsorb and be dispersed in melamine microparticle surfaces.Then gained suspension is under agitation heated to 60 ℃～80 ℃ and removes aqueous solvent, then be dried 1h～3h in 60 ℃～80 ℃ baking ovens;
C. step b gained mixture is placed in to crucible, after building crucible cover, put into Muffle furnace, Muffle furnace temperature programming to 520 ℃ is calcined, average heating speed is 1.3 ℃/min～1.5 ℃/min, and 520 ℃ insulation 2h, after naturally cooling by gained solid abrasive;
D. step c gained pressed powder is put in crucible again, the uncovered Muffle furnace of putting into, average speed temperature programming to 520 ℃ with 5.0 ℃/min～6.0 ℃/min is calcined, and at 520 ℃ of insulation 2h, naturally cooling rear taking-up product, obtains phosphorus doping graphite-phase carbonitride visible light catalyst after grinding.
Preferably, the concentration of dilute phosphoric acid solution described in step a is 0.793mol/L, and the amount of melamine pressed powder is 5.00g, and the mol ratio of described phosphoric acid and melamine is 1:100,1:50,1:20.
Preferably, in step b, gained suspension is heated to 70 ℃～80 ℃ and removes aqueous solvent under mechanical agitation condition.
Preferably, in step c, Muffle furnace temperature programming step is, first in 15min, is warming up to 300 ℃, constant temperature 1h, is then warming up to 350 ℃, constant temperature 1h, be warming up to 400 ℃, constant temperature 1h, is warming up to 480 ℃ afterwards again, constant temperature 1h, then be warming up to 500 ℃, constant temperature 1h, is finally warming up to 520 ℃, controlling each heat temperature raising time is 5min～7min, is incubated 2h after being warming up to 520 ℃.
Preferably, in steps d, Muffle furnace temperature programming step is, first heat 20min～30min and be warming up to 450 ℃, and constant temperature 1h, then be warming up to 520 ℃ through 5min～10min, and then insulation 2h.
The invention has the advantages that, raw material sources are extensive, and preparation method is simple, do not need complex device, are suitable for large-scale production, and prepared phosphorus doping graphite-phase carbonitride composite visible light catalyst has excellent visible light catalytic performance and good catalytic stability.
Accompanying drawing explanation
Fig. 1 is the X ray diffracting spectrum of phosphorus doping graphite-phase carbonitride visible light catalyst;
Fig. 2 is the x-ray photoelectron spectroscopy of graphite-phase carbonitride;
The high pressure liquid chromatography figure of rhodamine B catabolite when Fig. 3 is phosphorus doping graphite-phase carbonitride photocatalytic degradation different time;
Fig. 4 is the circulation experiment result figure of phosphorus doping graphite-phase carbonitride visible light photocatalytic degradation rhodamine B.
The specific embodiment
The dilute phosphoric acid solution 1mL that pipettes concentration and be 0.793mol/L joins in the beaker that contains 5mL deionized water, stir 10min, under agitation 5.00g melamine pressed powder is slowly added in this dilute phosphoric acid solution afterwards, continue to stir 50min, make phosphoric acid evenly adsorb and be dispersed in melamine microparticle surfaces.Gained suspension is under agitation heated to 80 ℃ and removes aqueous solvent, then be dried 2h in 80 ℃ of baking ovens.Dried mixture is placed in to crucible, puts into Muffle furnace after building crucible cover, first in 15min, be warming up to 300 ℃, constant temperature 1h, is then warming up to 350 ℃, constant temperature 1h, be warming up to 400 ℃, constant temperature 1h, is warming up to 480 ℃ afterwards again, constant temperature 1h, is then warming up to 500 ℃, constant temperature 1h, finally be warming up to 520 ℃, controlling each heat temperature raising time is 5min, is incubated 2h after being warming up to 520 ℃, after naturally cooling by gained solid abrasive; Gained pressed powder is put in crucible again, and the uncovered Muffle furnace of putting into, first heats 20min and is warming up to 450 ℃, constant temperature 1h, then be warming up to 520 ℃ through 10min, and then insulation 2h, naturally cooling rear taking-up product, obtains phosphorus doping graphite-phase carbonitride visible light catalyst after grinding.
In the present embodiment, the X ray diffracting spectrum of prepared phosphorus doping graphite-phase carbonitride visible light catalyst as shown in Figure 1.As can be seen from Figure 1, prepared sample has two obvious characteristic diffraction peaks at 27.4 ° and 13.2 °, and (002) and (100) crystal face of corresponding graphite-phase carbonitride, proves that the sample making is graphite-phase carbonitride respectively.Fig. 2 is the x-ray photoelectron spectroscopy of prepared phosphorus doping graphite-phase carbonitride, as can be seen from Figure 2 phosphorus doping graphite-phase carbonitride visible light catalyst has P elements peak to occur at 133.5eV place, in the visible light catalyst that proves to prepare, has really been doped into P elements.
The performance test of prepared phosphorus doping graphite-phase carbonitride visible light catalyst is as follows: in open reactor, add the rhodamine B solution that 0.150g prepared catalyst and 150mL concentration are 4mg/L, under dark condition, stirring 2h reaches after adsorption equilibrium, open visible light source (300W iodine-tungsten lamp added a cover optical filter filtering the following light of 400nm) irradiation, from reaction system, sample in a certain time interval, after high speed centrifugation separated light catalyst, get supernatant liquor spectrophotometer and measure absorbance under 554nm wavelength, obtain the change in concentration situation of rhodamine B in solution.Experimental result shows, in the time of radiation of visible light 60min, phosphorus doping graphite-phase carbonitride visible light catalyst is 97.3% to the visible light photocatalytic degradation rate of rhodamine B, and the pure graphite-phase carbonitride of preparing under the same terms is only 49.7% to the visible light photocatalytic degradation rate of rhodamine B.
When prepared phosphorus doping graphite-phase carbonitride photocatalytic degradation different time, the high pressure liquid chromatography figure of rhodamine B catabolite as shown in Figure 3.In Fig. 3, abscissa is retention time/min, ordinate is relative intensity, as seen from Figure 3, under the prepared carbonitride catalysis of phosphorus doping graphite-phase and radiation of visible light, rhodamine B can be degraded rapidly and be formed little molecule intermediate product, and intermediate product also can be degraded rapidly, when 75min, rhodamine B and intermediate product thereof are just completely degraded substantially, illustrate that phosphorus doping graphite-phase carbonitride has efficient visible light catalysis activity.
The dilute phosphoric acid solution 0.5mL that pipettes concentration and be 0.793mol/L joins in the beaker that contains 5mL deionized water, stir 5min, under agitation 5.00g melamine pressed powder is slowly added in this dilute phosphoric acid solution afterwards, continue to stir 30min, make phosphoric acid evenly adsorb and be dispersed in melamine microparticle surfaces.Gained suspension is under agitation heated to 80 ℃ and removes after aqueous solvent, then be dried 2h in 80 ℃ of baking ovens.Dried mixture is placed in to crucible, puts into Muffle furnace after building crucible cover, first in 15min, be warming up to 300 ℃, constant temperature 1h, is then warming up to 350 ℃, constant temperature 1h, be warming up to 400 ℃, constant temperature 1h, is warming up to 480 ℃ afterwards again, constant temperature 1h, is then warming up to 500 ℃, constant temperature 1h, finally be warming up to 520 ℃, controlling each heat temperature raising time is 6min, is incubated 2h after being warming up to 520 ℃, after naturally cooling by gained solid abrasive; Gained pressed powder is put in crucible again, and the uncovered Muffle furnace of putting into, first heats 20min and is warming up to 450 ℃, constant temperature 1h, then be warming up to 520 ℃ through 10min, and then insulation 2h, naturally cooling rear taking-up product, obtains phosphorus doping graphite-phase carbonitride visible light catalyst after grinding.It is 96.0% to the photocatalytic activity of rhodamine B that experiment records above-mentioned phosphorus doping graphite-phase carbonitride visible light catalyst in the time of radiation of visible light 60min, the visible light photocatalytic degradation rate (49.7%) apparently higher than pure graphite-phase carbonitride to rhodamine B.
The dilute phosphoric acid solution 2.5mL that pipettes concentration and be 0.793mol/L joins in the beaker that contains 5mL deionized water, stir 10min, under agitation 5.00g melamine pressed powder is slowly added in this dilute phosphoric acid solution afterwards, continue to stir 60min, make phosphoric acid evenly adsorb and be dispersed in melamine microparticle surfaces.Gained suspension is heated to 80 ℃ under stirring condition and removes after aqueous solvent, then be dried 2h in 80 ℃ of baking ovens.Dried mixture is placed in to crucible, puts into Muffle furnace after building crucible cover, first in 15min, be warming up to 300 ℃, constant temperature 1h, is then warming up to 350 ℃, constant temperature 1h, be warming up to 400 ℃, constant temperature 1h, is warming up to 480 ℃ afterwards again, constant temperature 1h, is then warming up to 500 ℃, constant temperature 1h, finally be warming up to 520 ℃, controlling each heat temperature raising time is 5min, is incubated 2h after being warming up to 520 ℃, after naturally cooling by gained solid abrasive; Gained pressed powder is put in crucible again, and the uncovered Muffle furnace of putting into, first heats 20min and is warming up to 450 ℃, constant temperature 1h, then be warming up to 520 ℃ through 10min, and then insulation 2h, naturally cooling rear taking-up product, obtains phosphorus doping graphite-phase carbonitride visible light catalyst after grinding.It is 90.5% to the rate of falling of rhodamine B that experiment records above-mentioned phosphorus doping graphite-phase carbonitride visible light catalyst in the time of radiation of visible light 60min.
Choose the prepared phosphorus doping graphite-phase carbonitride visible light catalyst of embodiment 1 rhodamine B degradation that circulates and test to investigate its photocatalysis stability under visible ray.In circulation experiment, phosphorus doping graphite-phase carbonitride photochemical catalyst is used to repetition rhodamine B degradation solution, and after illumination 75min, catalyst is through centrifugation, and washing, carries out rhodamine B degradation solution testing next time after being dried.Circulation experiment result figure by the phosphorus doping graphite-phase carbonitride visible light photocatalytic degradation rhodamine B shown in accompanying drawing 4 can find out, after 9 times are cycled to repeat use, this photochemical catalyst still keeps efficient photocatalytic activity, show that this photochemical catalyst has good photocatalysis stability, abscissa in accompanying drawing 4 is time/min, and ordinate is percentage degradation rate.
Claims (5)
1. a preparation method for phosphorus doping graphite-phase carbonitride visible light catalyst, is characterized in that, it take melamine as presoma, prepares P elements doped graphite phase carbon nitride visible light catalyst take phosphoric acid as phosphorus source, specifically comprises the following steps:
A. measure concentration and be phosphoric acid 2mL～8mL of 85% and move in 100mL volumetric flask, add deionized water and be made into the dilute phosphoric acid solution that concentration is 0.292mol/L～1.17mol/L;
B. described in removing step a, dilute phosphoric acid solution 0.25mL～3.0mL joins in the beaker that contains 5mL deionized water, stir 5min～10min, under agitation 5.00g melamine pressed powder is slowly added in this dilute phosphoric acid solution afterwards, making the mol ratio of phosphoric acid and melamine in solution is 1:100～1:20, continue to stir 20min～60min, make phosphoric acid evenly adsorb and be dispersed in melamine microparticle surfaces, then gained suspension is under agitation heated to 60 ℃～80 ℃, remove aqueous solvent, then be dried 1h～3h in 60 ℃～80 ℃ baking ovens; Obtain mixture;
C. step b gained mixture is placed in to crucible, puts into Muffle furnace after building crucible cover, Muffle furnace temperature programming to 520 ℃ is calcined, average heating speed is 1.3 ℃/min～1.5 ℃/min, and at 520 ℃ of insulation 2h, after naturally cooling, by gained solid abrasive, obtain pressed powder;
D. step c gained pressed powder is put in crucible again, the uncovered Muffle furnace of putting into, average speed temperature programming to 520 ℃ with 5.0 ℃/min～6.0 ℃/min is calcined, and at 520 ℃ of insulation 2h, naturally cooling rear taking-up product, obtains phosphorus doping graphite-phase carbonitride visible light catalyst after grinding.
2. the preparation method of phosphorus doping graphite-phase carbonitride visible light catalyst as claimed in claim 1, is characterized in that,
The mol ratio of described phosphoric acid and melamine is 1:50.
3. the preparation method of phosphorus doping graphite-phase carbonitride visible light catalyst as claimed in claim 1, is characterized in that, in step b, gained suspension is heated to 70 ℃～80 ℃ and removes aqueous solvent under mechanical agitation condition.
4. the preparation method of phosphorus doping graphite-phase carbonitride visible light catalyst as claimed in claim 1, is characterized in that, Muffle furnace heating schedule step is described in step c, first in 15min, be warming up to 300 ℃, constant temperature 1h, is then warming up to 350 ℃, constant temperature 1h, then be warming up to 400 ℃, constant temperature 1h, be warming up to afterwards 480 ℃, constant temperature 1h, is then warming up to 500 ℃, constant temperature 1h, finally be warming up to 520 ℃, controlling each heat temperature raising time is 5min～10min, is incubated 2h after being warming up to 520 ℃.
5. the preparation method of phosphorus doping graphite-phase carbonitride visible light catalyst as claimed in claim 1, it is characterized in that, the temperature programming of Muffle furnace described in steps d step is, first heat 20min～30min and be warming up to 450 ℃, constant temperature 1h, be warming up to 520 ℃ through 5min～10min again, and then insulation 2h.
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