CN104801325A - Photocatalyst composite structure and preparation method thereof - Google Patents
Photocatalyst composite structure and preparation method thereof Download PDFInfo
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- CN104801325A CN104801325A CN201410035063.0A CN201410035063A CN104801325A CN 104801325 A CN104801325 A CN 104801325A CN 201410035063 A CN201410035063 A CN 201410035063A CN 104801325 A CN104801325 A CN 104801325A
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Abstract
The present invention provides a photocatalyst composite structure and a preparation method thereof. The photocatalyst composite structure has backbone-branch structural feature; the graphite type carbon nitride (g-C3N4) is the backbone, and carbon nanotubes(CNTs) grown in situ on the backbone chemical through vapor deposition (CVD) are the branches; and the nano photocatalyst coats on the entire backbone-branch complex structure surface. The invention has the advantages that the photocatalyst composite structure can degrade organic contaminants and realize photocatalytic water decomposition for hydrogen production under ultraviolet and visible light; in addition, the backbone-branch composite structure has large specific surface area, and can fully contact with organic pollutants and electrolyte solution to improve the photocatalytic efficiency.
Description
[technical field]
The present invention relates to a kind of trunk-branch's photocatalyst complex structure body material, be mainly used in the field of Environment Protection of degradable organic pollutant under ultraviolet and visible ray, and at the energy field of photocatalytic hydrogen production by water decomposition.
[background technology]
TiO
2, the oxide semiconductor material such as ZnO, NiO has very strong oxidability under certain condition, can realize the degraded to toxic organic compound; And nontoxic, stable, with low cost, in field of environmental pollution control, there is broad prospect of application.But these catalysis materials only can absorb the ultraviolet light in sunshine, and the easy compound of electronics and hole that optical excitation produces, cause the problems such as the efficiency of light energy utilization is low, quantum efficiency is low.A lot of research by metal or nonmetal doping, noble metal surface deposition, with CNTs or Graphene compound and with the method such as other semiconductors coupling to Photocatalyst, the object of modification is mainly: the compound widening optical absorption intensity and scope, suppression photo-generated carrier.
Graphite type carbon nitride (g-C
3n
4) become the focus of photocatalysis field research, on the one hand, g-C
3n
4be all show high stability in the solution of 0 to 14 under light illumination and at pH, be considered to the most stable in all carbon nitrogen allotropes; On the other hand, g-C
3n
4belong to a kind of organic polymer semiconductor, energy gap is 2.73, and light abstraction width extend to the visible region of 450nm, can carry out photocatalytic hydrogen production by water decomposition under visible light.But, g-C
3n
4the easy compound of the photo-generated carrier produced under light illumination, causes its photocatalysis efficiency lower.For solving the problem, manyly to research and propose g-C
3n
4the method of modification, and achieve remarkable result.As being template with SBA-15, taking cyanamide as presoma, preparing mesoporous g-C
3n
4nanometer rods, specific area is than the block g-C of general preparation
3n
4improve 10-20 doubly, then with mesoporous g-C
3n
4nanometer rods is carrier, successfully water is reduced to hydrogen after carried noble metal Pt, Au; By TiO
2be carried on g-C
3n
4on, make C
3n
4/ TiO
2light abstraction width expand to 300 to 450nm, improve utilization rate that is visible, ultraviolet light, meanwhile, C
3n
4with TiO
2the hetero-junctions that contact interface is formed, facilitate photo-generate electron-hole and be separated, photocatalytic degradation result shows, C
3n
4/ TiO
2the degradation rate of Pyrogentisinic Acid is C respectively
3n
4and TiO
22.41 and 3.12 times.
CNT (CNTs) has good mechanical performance and electron storage and conductive performance, is widely used as the carrier of photochemical catalyst, promotes the separation of photo-generated carrier in catalysis material, and achieve good result in photocatalysis field.By by C
3n
4the method of presoma cyanamide and multi-walled carbon nano-tubes (MWNTs) Hybrid Heating, prepares g-C
3n
4/ CNTs composite photo-catalyst, result shows, the independent g-C of Photocatalyzed Hydrogen Production speed ratio
3n
4improve 3.7 times.In addition, CNTs/TiO
2the photocatalysis performance of composite photocatalyst material have also been obtained extensive research, take butyl titanate as titanium source, adopts sol-gel process to make it be carried on homodisperse carbon nano tube surface, prepares TiO
2/ CNTs composite photo-catalyst, is shown by the degradation experiment result of methyl orange, TiO
2/ CNTs compound is at TiO
2when content is relatively less, photocatalysis performance is still higher than the pure TiO under the same terms
2, wherein, CNTs serves important light induced electron derivative ac-tion in composite photocatalyst system.
At present, the composition form of photocatalysis complex structure body mainly contains two kinds, two or more oxide catalysis material compound of the first, hetero-junctions is formed at contact interface place, promote the derivation of photo-generated carrier, this kind of general light abstraction width of structure is wider, but specific area is less, cause it little with the contact area of the solution that is degraded, and the hetero-junctions electrical conductivity performance formed is superior not as good as conductive material.There is research with ZnO nano fiber for core, TiO
2for shell is wrapped in ZnO nano fiber surface, prepare ZnO/TiO
2nuclear shell structured nano-fiber, uv-visible absorption spectra shows, ZnO nano fiber and TiO
2the maximum absorption wavelength of nanofiber is respectively 360nm and 280nm, and ZnO/TiO
2the absorbing wavelength of nuclear shell structured nano-fiber has obvious red shift, but this two-dimensional structure material is compared with three-dimensional structure material, and specific area is relatively little, causes it to amass little with the solution contact surface that is degraded, thus affects its photocatalysis performance.It two is that one or more catalysis materials are combined with conductive material, to promote that photo-generated carrier is separated, but its defect to be the scope of light absorption narrower, mainly concentrate on ultra-violet (UV) band, or it is stable not to have visible light-responded catalysis material, easy photodissociation.There is research by ZnO, Graphene (RGO) and the ultrasonic mixing of CNTs, prepare ZnO/RGO/CNTs composite photo-catalyst, under ultraviolet light the degradation experiment of methylene blue is shown, after 260min, the degradation rate of pure ZnO is 62%, and ZnO/RGO and ZnO/RGO/CNTs reaches 88% and 96% respectively.This explanation, conductive material Graphene and CNT improve the photocatalysis performance of composite photo-catalyst to a certain extent, but the ZnO/RGO/CNTs composite photo-catalyst prepared owing to adopting the method for ultrasonic mixing, owing to not forming a kind of combination closely and desirable composite construction between each component, so photocatalysis performance improves limited.
[summary of the invention]
The object of the invention is to overcome the deficiencies in the prior art, a kind of photocatalyst complex structure body and preparation method thereof is provided.
The object of the invention is to be achieved through the following technical solutions:
A kind of photocatalyst complex structure body, as the graphite type carbon nitride (g-C of trunk
3n
4), the metallic catalyst of growth CNTs, growth in situ is in g-C
3n
4on CNTs branch and be carried on the nano-oxide photochemical catalyst of whole trunk-branch's composite construction surface;
The metallic catalyst chosen from Fe of described growth CNTs, cobalt, one or several in nickel.
The particle of described nano-oxide photochemical catalyst is titanium dioxide, zinc oxide, the combination of one or more in nickel oxide.
Described nano-oxide photochemical catalyst is coated on the surface of trunk-branch's complex structure body by sol-gal process.
Described trunk structure g-C
3n
4for tubulose, bar-shaped, sheet and spherical mesoporous or non-meso-hole structure, size is between 0.1 μm ~ 50 μm.
Branched structure is single wall or many walls CNTs, and pipe diameter is between 2 ~ 50nm.
Described load is at trunk g-C
3n
4be tubulose, bar-shaped, sheet and particle with the nano-oxide photochemical catalyst form on branch CNTs, size is between 5nm ~ 100nm.
A method for the preparation of photocatalyst complex structure body, its concrete steps are:
The first step, preparation or purchase g-C
3n
4, trunk g-C
3n
4size is comparatively large, and scope is between 0.1 μm ~ 50 μm;
Second step, by impregnating method at g-C
3n
4at least one metal ion in upper load iron, cobalt, nickel, after oven dry, becomes the catalyst that CVD grows CNTs;
3rd step, impregnated of the g-C of metal ion
3n
4under inert gas shielding, pass into carbon source material as acetylene growth in situ CNTs, caliber controls between 2 ~ 50nm;
4th step, the trunk-branched structure surface uniform coated with nano photochemical catalyst formed, as titanium dioxide, zinc oxide, nickel oxide etc., the size of photocatalyst particles controls between 5 ~ 100nm.
Described g-C
3n
4widen the light abstraction width of complex structure body with the combination of nano-oxide photochemical catalyst, the utilization rate of sunshine has been improved.
Described g-C
3n
4and the hetero-junctions formed between nano-oxide photochemical catalyst becomes the another kind of effective way that light induced electron conducts, and makes light induced electron derive in time.
Described trunk-branching type photocatalyst complex structure body has large specific area, can ensure that the abundant spread loads of nano-oxide photochemical catalyst is at g-C
3n
4the surface of trunk and CNTs branch, forms the photocatalyst complex structure body of the larger particles easily reclaimed, and solves the problem that nano-photocatalyst difficulty reclaims; Large specific area is conducive to the absorption to the thing that is degraded, and improves photocatalytic degradation efficiency.
Growing the nano transition metal being reduced generation in the process of CNTs at CVD, is the catalyst active center of growth CNTs, again by metal-CNTs and metal-g-C
3n
4between hetero-junctions effect, promote light induced electron conduction and be separated.
Compared with prior art, good effect of the present invention is:
In the present invention, with g-C
3n
4for trunk, the CNT (CNTs) of chemical vapour deposition technique (CVD) growth in situ on it is branch, nano-oxide photocatalyst coating, in whole trunk-branch's composite construction surface, constructs a kind of novel photocatalyst complex structure body.From composition, g-C
3n
4stable in properties, and energy gap is narrower, and light abstraction width is widened to visible region, is combined with the nano-oxide photochemical catalyst of ultraviolet light response, makes complex structure body show the characteristic of the full spectral absorption of as seen-ultraviolet.From structure, trunk-branch's complex structure body specific area is large, can fully contact with the solution that is degraded, and improves photocatalytic degradation efficiency; CNTs connects g-C simultaneously
3n
4with nano-oxide photochemical catalyst, the light induced electron of both guarantees is derived in time; g-C
3n
4the hetero-junctions formed with nano-oxide photochemical catalyst becomes another passage that photo-generated carrier is derived, and photo-generate electron-hole separative efficiency is improved further.
Photocatalyst complex structure body of the present invention can under ultraviolet and visible ray degradable organic pollutant and photocatalytic hydrogen production by water decomposition; In addition, trunk-branch's complex structure body has large specific area, fully can contact with organic pollution and electrolyte solution, improves photocatalysis efficiency.
[detailed description of the invention]
The detailed description of the invention of a kind of photocatalyst complex structure body of the present invention and preparation method thereof is below provided.
The invention provides a kind of trunk-branching type photocatalyst complex structure body, comprise (a) g-C as the larger particles of trunk
3n
4, (b) grows the metallic catalyst of CNTs, and (c) growth in situ is in g-C
3n
4on CNTs branched structure, (d) is carried on the nano-oxide photochemical catalyst of whole trunk-branch's composite construction surface, to form the complex structure body photochemical catalyst of the high-quantum efficiency that can make full use of sunshine.
The method for optimizing of the preparation of described trunk-branching type photocatalyst complex structure body is: the first step, preparation or purchase g-C
3n
4, trunk g-C
3n
4size is comparatively large, and scope is between 0.1 μm to 50 μm.Second step, by impregnating method at g-C
3n
4at least one metal ion in upper load iron, cobalt, nickel, after oven dry, becomes the catalyst that CVD grows CNTs.3rd step, impregnated of the g-C of metal ion
3n
4under inert gas shielding, pass into carbon source material as acetylene growth in situ CNTs, caliber controls between 2 to 50nm.4th step, the trunk-branched structure surface uniform coated with nano photochemical catalyst formed, as titanium dioxide, zinc oxide, nickel oxide etc., the size of photocatalyst particles controls between 5nm to 100nm.
Embodiment 1
G-C
3n
4trunk
Get 5g melamine in 100ml deionized water, ultrasonic disperse, add a certain amount of rare H
2sO
4(volume ratio H
2sO
4: H
2o=1: 1), use deionized water filtration washing after stirring 2h, 80 DEG C are dried 12h.Then get the sample 3g after oven dry bottom porcelain Noah's ark, put into tube furnace, the lower 600 DEG C of roasting 4h of argon shield, obtain g-C
3n
4.
G-C
3n
4upper impregnating metal ion
By the nickel nitrate aqueous solution 100ml of variable concentrations and 2g g-C
3n
4ultrasonic mixing, wherein, the concentration of nickel nitrate aqueous solution, between 0.005M to 0.02M, after stir about 2h, centrifugally makes Separation of Solid and Liquid, and solid obtains the g-C of nickel-loaded ion after drying in 60 DEG C
3n
4.
G-C
3n
4upper growth in situ CNTs branched structure
By the g-C of load nickel nitrate
3n
4powder is laid in bottom porcelain Noah's ark, puts into tube furnace, under argon shield, rise to 550 DEG C with the speed of 3 DEG C/min, leads to acetylene gas 10min, at g-C after insulation 1h with the speed of 20ml/min
3n
4upper CVD growth in situ CNTs, obtains g-C after being cooled to room temperature
3n
4/ CNTs trunk-branched structure body.
Loaded with nano oxidation photocatalyst
Getting a certain amount of butyl titanate joins in 50ml glacial acetic acid, after stirring 1h, gets 1gg-C
3n
4/ CNTs complex structure body powder joins in solution; after stirring; 5ml deionized water is dropwise added in suspension; after continuing to stir 12h, solid-liquid centrifugation is separated, after solid is dried at 60 DEG C; put into tube furnace; under argon shield, rise to 550 DEG C with the speed of 3 DEG C/min, roasting 1h, obtain a kind of trunk-branch's photocatalyst complex structure body of the present invention.
Under simulated solar irradiation irradiates, the photocatalytic activity of trunk of the present invention-branch's photocatalysis complex structure body is tested.Be degraded to model reaction with methyl orange, analyze the situation of the change of methyl orange solution absorbance before and after degraded, test trunk of the present invention-branch's photocatalyst complex structure body photocatalytic activity.Test condition is as follows: methyl orange aqueous solution concentration is 30mg/ml, methyl orange solution volume 100ml, the quality of the photocatalysis complex structure body added is 0.05g, simulated solar light source adopts the xenon lamp of 250W, after lucifuge stirs 1h, degradation reaction 2h, adopts ultraviolet-uisible spectrophotometer test methyl orange concentration, and calculates the degradation rate of methyl orange.With the test result of comparative sample in table 1.
Table 1 photocatalytic activity compares
As can be known from the results of Table 1, by method of the present invention by g-C
3n
4, CNTs and TiO
2after being configured to the photocatalyst structure body of trunk-branch of the present invention, photocatalysis performance obtains significant raising.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, without departing from the inventive concept of the premise; can also make some improvements and modifications, these improvements and modifications also should be considered within the scope of protection of the present invention.
Claims (10)
1. a photocatalyst complex structure body, is characterized in that, as the graphite type carbon nitride (g-C of trunk
3n
4), the metallic catalyst of growth CNTs, growth in situ is in g-C
3n
4on CNTs branch and be carried on the nano-oxide photochemical catalyst of whole trunk-branch's composite construction surface.
2. a kind of photocatalyst complex structure body as claimed in claim 1, is characterized in that, the metallic catalyst chosen from Fe of described growth CNTs, and cobalt, one or several in nickel, are preferably cobalt.
3. a kind of photocatalyst complex structure body as claimed in claim 1, is characterized in that, the particle of described nano-oxide photochemical catalyst is titanium dioxide, zinc oxide, the combination of one or more in nickel oxide, is preferably zinc oxide.
4. a kind of photocatalyst complex structure body as claimed in claim 1, is characterized in that, described nano-oxide photochemical catalyst is coated on the surface of trunk-branch's complex structure body by sol-gal process.
5. a kind of photocatalyst complex structure body as claimed in claim 1, is characterized in that, described trunk structure g-C
3n
4for tubulose, bar-shaped, sheet and spherical mesoporous or non-meso-hole structure, size is between 0.1 μm ~ 50 μm.
6. a kind of photocatalyst complex structure body as claimed in claim 1, is characterized in that, branched structure is single wall or many walls CNTs, and pipe diameter is between 2 ~ 50nm.
7. a kind of photocatalyst complex structure body as claimed in claim 1, is characterized in that, described load is at trunk g-C
3n
4be tubulose, bar-shaped, sheet and particle with the nano-oxide photochemical catalyst form on branch CNTs, size is between 5nm ~ 100nm.
8. a preparation method for photocatalyst complex structure body, is characterized in that, its concrete steps are:
The first step, preparation or purchase g-C
3n
4, trunk g-C
3n
4size is comparatively large, and scope is between 0.1 μm ~ 50 μm;
Second step, by dipping method at g-C
3n
4at least one metal ion in upper load iron, cobalt, nickel, after oven dry, becomes the catalyst that CVD grows CNTs;
3rd step, impregnated of the g-C of metal ion
3n
4under inert gas shielding, pass into carbon source material growth in situ CNTs, caliber controls between 2 ~ 50nm;
4th step, the trunk-branched structure surface uniform coated with nano oxidation photocatalyst formed, the size of the particle of nano-oxide photochemical catalyst controls between 5 ~ 100nm.
9. the preparation method of a kind of photocatalyst complex structure body as claimed in claim 8, is characterized in that, in the third step, carbon source material is acetylene.
10. the preparation method of a kind of photocatalyst complex structure body as claimed in claim 8, is characterized in that, in the 4th step, nano-oxide photochemical catalyst is the one in titanium dioxide, zinc oxide, nickel oxide.
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| CN106567102A (en) * | 2016-10-09 | 2017-04-19 | 华东理工大学 | Preparation method of TiO2/carbon nano-tube (CNT)/Ni photoelectric active combination electrode |
| CN106694015A (en) * | 2016-11-17 | 2017-05-24 | 陕西师范大学 | Simple preparation method of high-dispersion nickel oxide cluster modified carbon nitride photocatalyst for decomposing water to produce hydrogen |
| CN107115880A (en) * | 2017-04-24 | 2017-09-01 | 吉林师范大学 | A kind of MoS2/CNTs/g C3N4 composite photo-catalysts and preparation method thereof |
| CN107537544A (en) * | 2017-09-19 | 2018-01-05 | 江苏理工学院 | A kind of g C3N4- CNTs heterojunction photocatalysts and preparation method thereof |
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| CN107537544B (en) * | 2017-09-19 | 2020-02-14 | 江苏理工学院 | g-C3N4-CNTs heterojunction photocatalyst and preparation method thereof |
| CN107537544A (en) * | 2017-09-19 | 2018-01-05 | 江苏理工学院 | A kind of g C3N4- CNTs heterojunction photocatalysts and preparation method thereof |
| CN107952465A (en) * | 2017-12-16 | 2018-04-24 | 湖南科技大学 | A kind of composite catalyst of cyclohexane selectivity oxidation, preparation method and application |
| CN107952465B (en) * | 2017-12-16 | 2020-08-28 | 湖南科技大学 | Composite catalyst for selective oxidation of cyclohexane, preparation method and application |
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