CN103143380A - Solvent evaporation method for preparing graphite phase carbon nitride/{001} surface exposed anatase phase titanium dioxide nano composite material - Google Patents
Solvent evaporation method for preparing graphite phase carbon nitride/{001} surface exposed anatase phase titanium dioxide nano composite material Download PDFInfo
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Abstract
The invention discloses a solvent evaporation method for preparing graphite phase carbon nitride/{001} surface exposed anatase phase titanium dioxide nano composite material and relates to the preparation of organic polymer/inorganic semiconductor nano composite material. The invention aims to solve the problems that the conventional {001} surface exposed anatase phase titanium dioxide photocatalyst is wide in response range and low in quantum efficiency. The preparation method comprises the following steps: 1, preparing graphite phase carbon nitride; 2, preparing {001} surface exposed anatase phase titanium dioxide nanosheets; 3, preparing solid substances; and 4, preparing the graphite phase carbon nitride/{001} surface exposed anatase phase titanium dioxide nano composite material. The obtained graphite phase carbon nitride/{001} surface exposed anatase phase titanium dioxide nano composite material has high ultraviolet light catalytic activity and also has an excellent visible light catalytic capacity. The method is used for preparing the graphite phase carbon nitride/{001} surface exposed anatase phase titanium dioxide nano composite material.
Description
Technical field
The present invention relates to the preparation of organic polymer/inorganic semiconductor nano composite material.
Background technology
Along with the progress of expanding economy and society, problem of environmental pollution is on the rise.Photocatalysis technology is one of the most economical effective means of curbing environmental pollution, and has therefore obtained the attention of countries in the world governments.As typical semiconductor light-catalyst, that titanium dioxide has is nontoxic, cheap and easy to get, catalytic capability is strong, abrasion resistance good, chemical stability is high and the advantage such as reusable edible, thereby is subject to field of environment protection experts and scholars' extensive concern.Titanium dioxide mainly contains three kinds of crystal formations, is respectively anatase, rutile and brockite, and wherein anatase because the redox ability of photoproduction charge carrier has higher photocatalytic activity by force, is a kind of crystal formation that field of titanium dioxide photocatalysis is studied at most.Theoretical and experiment all shows, { the 001} face is its high energy crystal face to anatase, and the surface can reach 0.90Jm
-2, { photocatalytic activity of the anatase phase titanium dioxide that the 001} face exposes even is better than the titanium deoxide catalyst Degussa P25 of business.
Yet the anatase phase titanium dioxide photochemical catalyst also has the two large defectives that himself are difficult to overcome, i.e. photoresponse narrow range, and quantum efficiency is low.The energy gap of anatase phase titanium dioxide is 3.2eV, can only absorb the sunshine medium wavelength less than the ultraviolet light part of 387nm, and this part ultraviolet light only accounts for 3%～5% of whole solar spectrum.Under the irradiation of ultraviolet light, the electron excitation at titanium dioxide valence band place transits to conduction band, generates a hole in valence band simultaneously, thereby forms electron-hole pair.With the hydrone that is adsorbed on titanium dioxide surface and oxygen molecule, a series of chain reactions occuring after these photoproduction charge carriers process bulk diffusions and surface migration finally generates hydroxyl radical free radical, and hydroxyl radical free radical has very strong oxidability, thus the various organic pollutions of oxidation classification.Yet these light induced electron-holes are to very unstable, very easily occur compound again and cause the reduction of material quantum efficiency, thereby weaken its photo-catalysis capability.How to solve the photoresponse narrow range and just become the main research topic of anatase phase titanium dioxide photocatalysis field with the low problem of quantum efficiency.
Summary of the invention
The present invention is that existing in order to solve { the 001} face exposes anatase phase titanium dioxide photochemical catalyst photoresponse narrow range and the low problem of quantum efficiency, and provides solvent evaporation method to prepare that the graphite-phase carbonitride/{ the 001} face exposes the anatase phase titanium dioxide nano composite material.
Solvent evaporation method prepare the graphite-phase carbonitride/the 001} face exposes the anatase phase titanium dioxide nano composite material, and concrete steps are as follows:
One, urea is put into crucible, then crucible being placed in Muffle furnace is to calcine 1h～4h under 500 ℃～600 ℃ conditions in temperature, and controlling heating rate is 15 ℃/min, then naturally is down to room temperature, then grind into powder, obtains the graphite-phase carbonitride;
Two, 1mL～6mL titanium salt and 5mL～30mL alcohol are mixed, ultrasonic 0.5h～3h under air-proof condition again, then system is transferred in the water heating kettle liner, controlling the magnetic agitation rotating speed is 300 rev/mins～800 rev/mins, drips 0.1mL～2mL hydrofluoric acid solution, is then under 150 ℃～200 ℃ conditions in temperature, hydrothermal treatment consists 6h～24h, taking precipitate again, and use the absolute ethyl alcohol centrifuge washing makes that { the 001} face exposes the anatase phase titanium dioxide nanometer sheet;
Three, the graphite-phase carbonitride that 4mg～40mg step 1 is obtained and the alcohol of 40mL～80mL mix, { the 001} face exposure anatase phase titanium dioxide nanometer sheet that adds again step 2 to obtain, then ultrasonic dispersion 0.5h～2h, obtain suspension, then with suspension under ventilation condition, controlling magnetic agitation speed is 500 rev/mins～1000 rev/mins, stirs 4h～12h, obtains solid matter;
Four, the solid matter that step 3 is obtained is transferred in baking oven, is constant temperature 2h～8h under 80 ℃～120 ℃ conditions in temperature, then is ground into powder, and obtains graphite-phase carbonitride/{ 001} face exposure anatase phase titanium dioxide nano composite material.
Wherein, the titanium salt described in step 2 is titanium tetrachloride, titanium sulfate, titanyl sulfate, butyl titanate or isopropyl titanate;
Alcohol described in step 2 is ethanol or isopropyl alcohol;
Alcohol described in step 3 is methyl alcohol or ethanol.
The graphite-phase carbonitride is a kind of organic polymer, has and the similar layer structure of Graphene.Yet different from Graphene is, the graphite-phase carbonitride is a kind of semi-conducting material, and the extinction threshold value is in the 460nm left and right.With the graphite-phase carbonitride with { it is compound that the 001} face exposes anatase phase titanium dioxide, the latter's photophase scope can be widened visible region; In addition, because the band structure of graphite-phase carbonitride and the band structure of titanium dioxide match each other, have the graphite-phase carbonitride of pi-electron conjugated system and two-dimension plane structure and anatase phase titanium dioxide compound after, to be conducive to the transfer of photoproduction charge carrier between two components, thereby can suppress right compound again in light induced electron-hole, extend the life-span of photoproduction charge carrier and improve quantum efficiency and the photo-catalysis capability of titanium dioxide optical catalyst.
The invention has the beneficial effects as follows: the present invention is directed to that existing { the 001} face exposes anatase phase titanium dioxide photochemical catalyst photoresponse narrow range and the major defect such as quantum efficiency is low, the graphite-phase carbonitride that will have the conjugated pi electron structure by solvent evaporation method is compound with it, generates graphite-phase carbonitride/{ 001} face exposure anatase phase titanium dioxide nano composite material.In the gained nano composite material, titanium dioxide nanoplate is pure Anatase, and the about 38nm of the length of side, thickness are the 6nm left and right, and { 001} face exposure is about 76%, and the graphite-phase carbonitride of layer structure is coated on the surface of titanium dioxide nanoplate.{ the 001} face exposes anatase phase titanium dioxide nanometer particle to be compared, and the graphite-phase carbonitride/{ 001} face exposure anatase phase titanium dioxide nano composite material not only ultraviolet catalytic activity significantly improves, but also possesses good visible light catalytic ability with pure.And the raw material that use are cheap and easy to get, easy and simple to handle, and equipment and technology is simple, can be widely used as catalysis material and photoelectric material, can be used in and administer waste water, purify air, the aspect such as opto-electronic conversion.
The present invention is for the preparation of the graphite-phase carbonitride/{ the 001} face exposes the anatase phase titanium dioxide nano composite material.
Description of drawings
Fig. 1 is the transmission electron microscope photo of the graphite-phase carbonitride of embodiment one step 1 preparation;
Fig. 2 is the Fourier Tranform infrared spectrogram of the graphite-phase carbonitride of embodiment one step 1 preparation;
Fig. 3 is that { the 001} face exposes the transmission electron microscope photo of anatase phase titanium dioxide nanometer sheet in embodiment one step 2 preparation;
Fig. 4 is that { the 001} face exposes the high-resolution-ration transmission electric-lens photo of anatase phase titanium dioxide nanometer sheet in embodiment one step 2 preparation;
Fig. 5 is that { the 001} face exposes the XRD spectra of anatase phase titanium dioxide nanometer sheet in embodiment one step 2 preparation;
Fig. 6 be embodiment one preparation the graphite-phase carbonitride/{ the 001} face exposes the low power transmission electron microscope photo of anatase phase titanium dioxide nano composite material;
Fig. 7 be embodiment one preparation the graphite-phase carbonitride/{ the 001} face exposes the high power transmission electron microscope photo of anatase phase titanium dioxide nano composite material;
Fig. 8 be embodiment one preparation the graphite-phase carbonitride/{ the 001} face exposes the XRD spectra of anatase phase titanium dioxide nano composite material;
Fig. 9 is that { the graphite-phase carbonitride of 001} face exposure anatase phase titanium dioxide nanometer sheet and embodiment one preparation/{ the 001} face exposes anatase phase titanium dioxide nano composite material ultraviolet catalytic degradating organic dye methylene blue in embodiment one step 2 preparation, time dependent degradation rate curve map, when in figure, a represents without photochemical catalyst, methylene blue dye is from the degradation rate curve under UV-irradiation, in figure, b represents that { the 001} face exposes anatase phase titanium dioxide nanometer sheet ultraviolet catalytic degradating organic dye methylene blue in embodiment one step 2 preparation, time dependent degradation rate curve map, in figure c represent embodiment one preparation the graphite-phase carbonitride/{ the 001} face exposes anatase phase titanium dioxide nano composite material ultraviolet catalytic degradating organic dye methylene blue, time dependent degradation rate curve map,
Figure 10 is that { the graphite-phase carbonitride of 001} face exposure anatase phase titanium dioxide nanometer sheet and embodiment one preparation/{ the 001} face exposes anatase phase titanium dioxide nano composite material visible light photocatalytic degradation organic dyestuff methylene blue in embodiment one step 2 preparation, time dependent degradation rate curve map, when in figure, a represents without photochemical catalyst, methylene blue dye is from the degradation rate curve under radiation of visible light, in figure, b represents that { the 001} face exposes anatase phase titanium dioxide nanometer sheet visible light photocatalytic degradation organic dyestuff methylene blue in embodiment one step 2 preparation, time dependent degradation rate curve map, in figure c represent embodiment one preparation the graphite-phase carbonitride/{ the 001} face exposes anatase phase titanium dioxide nano composite material visible light photocatalytic degradation organic dyestuff methylene blue, time dependent degradation rate curve map.
The specific embodiment
Technical solution of the present invention is not limited to the following cited specific embodiment, also comprises any combination between each specific embodiment.
The specific embodiment one: present embodiment be the graphite-phase carbonitride/the 001} face exposes the preparation of anatase phase titanium dioxide nano composite material, and concrete steps are as follows:
One, urea is put into crucible, then crucible being placed in Muffle furnace is to calcine 1h～4h under 500 ℃～600 ℃ conditions in temperature, and controlling heating rate is 15 ℃/min, then naturally is down to room temperature, then grind into powder, obtains the graphite-phase carbonitride;
Two, 1mL～6mL titanium salt and 5mL～30mL alcohol are mixed, ultrasonic 0.5h～3h under air-proof condition again, then system is transferred in the water heating kettle liner, controlling the magnetic agitation rotating speed is 300 rev/mins～800 rev/mins, drips 0.1mL～2mL hydrofluoric acid solution, is then under 150 ℃～200 ℃ conditions in temperature, hydrothermal treatment consists 6h～24h, taking precipitate again, and use the absolute ethyl alcohol centrifuge washing makes that { the 001} face exposes the anatase phase titanium dioxide nanometer sheet;
Three, the graphite-phase carbonitride that 4mg～40mg step 1 is obtained and the alcohol of 40mL～80mL mix, { the 001} face exposure anatase phase titanium dioxide nanometer sheet that adds again step 2 to obtain, then ultrasonic dispersion 0.5h～2h, obtain suspension, then with suspension under ventilation condition, controlling magnetic agitation speed is 500 rev/mins～1000 rev/mins, stirs 4h～12h, obtains solid matter;
Four, the solid matter that step 3 is obtained is transferred in baking oven, is constant temperature 2h～8h under 80 ℃～120 ℃ conditions in temperature, then is ground into powder, and obtains graphite-phase carbonitride/{ 001} face exposure anatase phase titanium dioxide nano composite material.
The product that adopts the present embodiment method to obtain is that the graphite-phase carbonitride/{ the 001} face exposes the anatase phase titanium dioxide nano composite material, wherein the titanium dioxide component is the laminated structure of pure Anatase, the about 38nm of the length of side, thickness is the 6nm left and right, { 001} face exposure is about 76%, the graphite-phase carbonitride is layer structure, is coated on the surface of titanium dioxide nanoplate.
The specific embodiment two: what present embodiment was different from the specific embodiment one is that in step 2, titanium salt is titanium tetrachloride, titanium sulfate, titanyl sulfate, butyl titanate or isopropyl titanate.Other is identical with the specific embodiment one.
The specific embodiment three: what present embodiment was different from the specific embodiment one is: in step 2, alcohol is ethanol or isopropyl alcohol.Other is identical with the specific embodiment one.
The specific embodiment four: what present embodiment was different from the specific embodiment one is: in step 2, the concentration of hydrofluoric acid solution is 40wt%.Other is identical with the specific embodiment one.
The specific embodiment five: what present embodiment was different from the specific embodiment one is: in step 3, alcohol is methyl alcohol or ethanol.Other is identical with the specific embodiment one.
The specific embodiment six: what present embodiment was different from the specific embodiment one is: in step 3, the addition of graphite-phase carbonitride is 8mg.Other is identical with the specific embodiment one.
The specific embodiment seven: what present embodiment was different from the specific embodiment one is: in step 3, mixing time is 5h～8h.Other is identical with the specific embodiment one.
The specific embodiment eight: what present embodiment was different from one of specific embodiment one to seven is: in step 3, mixing time is 6h.Other is identical with one of specific embodiment one to seven.
The specific embodiment nine: what present embodiment was different from the specific embodiment one is: be constant temperature 3h～6h under 90 ℃～110 ℃ conditions in temperature in step 4.Other is identical with one of specific embodiment one to four.
The specific embodiment ten: what present embodiment was different from one of specific embodiment one to nine is: be constant temperature 4h under 100 ℃ of conditions in temperature in step 4.Other is identical with one of specific embodiment one to nine.
Adopt following examples checking beneficial effect of the present invention:
Embodiment one:
The present embodiment graphite-phase carbonitride/the 001} face exposes the preparation of anatase phase titanium dioxide nano composite material, and concrete steps are as follows:
One, urea is put into crucible, then crucible being placed in Muffle furnace is to calcine 2h under 550 ℃ of conditions in temperature, and controlling heating rate is 15 ℃/min, then naturally is down to room temperature, then grind into powder, obtains the graphite-phase carbonitride;
Two, 4mL butyl titanate and 15mL isopropyl alcohol are mixed, ultrasonic 1h under air-proof condition again, then system is transferred in the water heating kettle liner, controlling the magnetic agitation rotating speed is 800 rev/mins, drips the 0.5mL hydrofluoric acid solution, is then under 180 ℃ of conditions in temperature, hydrothermal treatment consists 12h, taking precipitate again, and use the absolute ethyl alcohol centrifuge washing makes that { the 001} face exposes the anatase phase titanium dioxide nanometer sheet;
Three, the graphite-phase carbonitride that the 8mg step 1 is obtained and the methyl alcohol of 50mL mix, { the 001} face exposure anatase phase titanium dioxide nanometer sheet that adds again step 2 to obtain, then ultrasonic dispersion 1h, obtain suspension, then with suspension under ventilation condition, controlling magnetic agitation speed is 800 rev/mins, stirs 6h, obtains solid matter;
Four, the solid matter that step 3 is obtained is transferred in baking oven, is constant temperature 4h under 100 ℃ of conditions in temperature, then is ground into powder, and obtains graphite-phase carbonitride/{ 001} face exposure anatase phase titanium dioxide nano composite material.
The transmission electron microscope photo of the graphite-phase carbonitride that the present embodiment step 1 makes as shown in Figure 1, in figure, scale is 100 nanometers, product is the micrometre grade thin layer structure as seen from the figure;
The Fourier Tranform infrared spectrogram of the graphite-phase carbonitride of the present embodiment step 1 preparation as shown in Figure 2, by the peak position of functional group's vibration absorption peak in figure as can be known product be the graphite-phase carbonitride;
The present embodiment step 2 make { transmission electron microscope photo that the 001} face exposes the anatase phase titanium dioxide nanometer sheet as shown in Figure 3, in figure, scale is 100 nanometers, and product is the nano-sheet structure as seen from the figure, the about 38nm of the length of side, thickness is the 6nm left and right, and { 001} face exposure is about 76%;
The present embodiment step 2 make { the high-resolution-ration transmission electric-lens photo that the 001} face exposes the anatase phase titanium dioxide nanometer sheet as shown in Figure 4, the interplanar distance that as can be seen from the figure is parallel to nanometer sheet upper and lower surfaces is 0.235nm, is high energy { 001} crystal face;
The present embodiment step 2 make { XRD spectra that the 001} face exposes the anatase phase titanium dioxide nanometer sheet as shown in Figure 5, titanium dioxide is pure Anatase as seen from the figure, and crystal property is good;
The graphite-phase carbonitride of the present embodiment preparation/{ the low power transmission electron microscope photo of 001} face exposure anatase phase titanium dioxide nano composite material as shown in Figure 6, in figure, scale is 100 nanometers, and product is the compound of titanium dioxide nanoplate and graphite-phase carbonitride as seen from the figure;
The graphite-phase carbonitride of the present embodiment preparation/{ the high power transmission electron microscope picture that the 001} face exposes the anatase phase titanium dioxide nano composite material as shown in Figure 7, graphite-phase carbonitride lamella covers that { the 001} face exposes the surface of anatase phase titanium dioxide nanometer sheet as seen from the figure;
The graphite-phase carbonitride of the present embodiment preparation/{ compound crystal formation that does not change the pure Anatase of titanium dioxide nanoplate of the graphite-phase carbonitride as seen from the figure XRD spectra that the 001} face exposes the anatase phase titanium dioxide nano composite material as shown in Figure 8.
Checking embodiment one step 2 obtain the 001} face expose the graphite-phase carbonitride that anatase phase titanium dioxide nanometer sheet and embodiment one obtain/photocatalytic activity of 001} face exposure anatase phase titanium dioxide nano composite material, concrete steps are as follows:
A. get respectively that embodiment one step 2 obtains the 001} face expose that titanium dioxide nanoplate and embodiment one obtain the graphite-phase carbonitride/{ 001} face exposure anatase phase titanium dioxide nano composite material 10mg is positioned in two 50mL beakers, and then add respectively the 10mL deionized water, and to add respectively 40 μ L mass concentrations be that 0.2% aqueous solution of methylene blue is in above-mentioned two kinds of reaction systems, dark place magnetic agitation 40 minutes;
B. shine under the high-pressure sodium lamp that is placed in 100W under the magnetic agitation condition, by uv-visible absorption spectra measuring and calculation methylene blue concentration over time; And shine being placed under the 300W xenon lamp under the magnetic agitation condition, and cover the optical filter elimination ultraviolet light of a 420nm on beaker, by uv-visible absorption spectra measuring and calculation methylene blue concentration over time.
{ the graphite-phase carbonitride that 001} face exposure anatase phase titanium dioxide nanometer sheet and embodiment one obtain/{ 001} face exposure anatase phase titanium dioxide nano composite material ultraviolet catalytic degradating organic dye methylene blue that embodiment one step 2 obtains, time dependent degradation rate curve map as shown in Figure 9, as can be seen from the figure, the graphite-phase carbonitride that obtains of embodiment one/{ the 001} face exposes the anatase phase titanium dioxide nano composite material, and to have a higher ultraviolet catalytic active;
{ the graphite-phase carbonitride that 001} face exposure anatase phase titanium dioxide nanometer sheet and embodiment one obtain/{ 001} face exposure anatase phase titanium dioxide nano composite material visible light photocatalytic degradation organic dyestuff methylene blue that embodiment one step 2 obtains, time dependent degradation rate curve map as shown in figure 10, as can be seen from the figure, the graphite-phase carbonitride that obtains of embodiment one/{ the 001} face exposes the anatase phase titanium dioxide nano composite material and also possesses good visible light catalytic ability.
Claims (10)
1. solvent evaporation method prepares graphite-phase carbonitride/{ 001} face exposure anatase phase titanium dioxide nano composite material, it is characterized in that solvent evaporation method prepare the graphite-phase carbonitride/the 001} face exposes the anatase phase titanium dioxide nano composite material, and concrete steps are as follows:
One, urea is put into crucible, then crucible being placed in Muffle furnace is to calcine 1h～4h under 500 ℃～600 ℃ conditions in temperature, and controlling heating rate is 15 ℃/min, then naturally is down to room temperature, then grind into powder, obtains the graphite-phase carbonitride;
Two, 1mL～6mL titanium salt and 5mL～30mL alcohol are mixed, ultrasonic 0.5h～3h under air-proof condition again, then system is transferred in the water heating kettle liner, controlling the magnetic agitation rotating speed is 300 rev/mins～800 rev/mins, dripping 0.1mL～2mL hydrofluoric acid solution, is then under 150 ℃～200 ℃ conditions in temperature, hydrothermal treatment consists 6h～24h, taking precipitate again, and use the absolute ethyl alcohol centrifuge washing;
Three, the graphite-phase carbonitride that 4mg～40mg step 1 is obtained and the alcohol of 40mL～80mL mix, the sediment that adds again step 2 to obtain, then ultrasonic dispersion 0.5h～2h, obtain suspension, then with suspension under ventilation condition, controlling magnetic agitation speed is 500 rev/mins～1000 rev/mins, stirs 4h～12h, obtains solid matter;
Four, the solid matter that step 3 is obtained is transferred in baking oven, is constant temperature 2h～8h under 80 ℃～120 ℃ conditions in temperature, then is ground into powder, and obtains graphite-phase carbonitride/{ 001} face exposure anatase phase titanium dioxide nano composite material.
2. solvent evaporation method according to claim 1 prepares that the graphite-phase carbonitride/{ the 001} face exposes the anatase phase titanium dioxide nano composite material, it is characterized in that the titanium salt described in step 2 is titanium tetrachloride, titanium sulfate, titanyl sulfate, butyl titanate or isopropyl titanate.
3. solvent evaporation method according to claim 1 prepares that the graphite-phase carbonitride/{ the 001} face exposes the anatase phase titanium dioxide nano composite material, it is characterized in that in step 2, alcohol is ethanol or isopropyl alcohol.
4. solvent evaporation method according to claim 1 prepares that the graphite-phase carbonitride/{ the 001} face exposes the anatase phase titanium dioxide nano composite material, and the concentration that it is characterized in that hydrofluoric acid solution in step 2 is 40wt%.
5. solvent evaporation method according to claim 1 prepares that the graphite-phase carbonitride/{ the 001} face exposes the anatase phase titanium dioxide nano composite material, it is characterized in that in step 3, alcohol is methyl alcohol or ethanol.
6. solvent evaporation method according to claim 1 prepares that the graphite-phase carbonitride/{ the 001} face exposes the anatase phase titanium dioxide nano composite material, and the addition that it is characterized in that graphite-phase carbonitride in step 3 is 8mg.
7. solvent evaporation method according to claim 1 prepares that the graphite-phase carbonitride/{ the 001} face exposes the anatase phase titanium dioxide nano composite material, it is characterized in that in step 3, mixing time is 5h～8h.
8. solvent evaporation method according to claim 7 prepares that the graphite-phase carbonitride/{ the 001} face exposes the anatase phase titanium dioxide nano composite material, it is characterized in that in step 3, mixing time is 6h.
9. solvent evaporation method according to claim 1 prepares that the graphite-phase carbonitride/{ the 001} face exposes the anatase phase titanium dioxide nano composite material, it is characterized in that in step 4 being constant temperature 3h～6h under 90 ℃～110 ℃ conditions in temperature.
10. solvent evaporation method according to claim 9 prepares that the graphite-phase carbonitride/{ the 001} face exposes the anatase phase titanium dioxide nano composite material, it is characterized in that in step 4 being constant temperature 4h under 100 ℃ of conditions in temperature.
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