CN102266787A - Preparation method of novel noble-metal-free catalyst for photolysis of water to produce hydrogen - Google Patents
Preparation method of novel noble-metal-free catalyst for photolysis of water to produce hydrogen Download PDFInfo
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- CN102266787A CN102266787A CN2010101924437A CN201010192443A CN102266787A CN 102266787 A CN102266787 A CN 102266787A CN 2010101924437 A CN2010101924437 A CN 2010101924437A CN 201010192443 A CN201010192443 A CN 201010192443A CN 102266787 A CN102266787 A CN 102266787A
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Abstract
The invention relates to a preparation method of a catalyst for solar decomposition of water to produce hydrogen without using noble metal as a catalyst promoter, particularly to a preparation method of a semiconductor nano particle-graphene composite material photocatalyst with graphene as a catalyst promoter, wherein the catalyst comprises CdS-graphene composite material and TiO2-graphene composite material. The hydrogen production efficiency of the photocatalyst by utilizing the graphene as the catalyst promoter can be matched with and even higher than that of the photocatalyst including the same mass of noble metal Pt under the same hydrogen production conditions. The graphene material has an excellent electron collection and transmission function, thereby promoting the effective segregation of electron holes, reducing the probability of compositing proton and increasing the photocatalysis efficiency of the photocatalyst and the hydrogen production efficiency of photodecomposition water; in addition, the graphene material has a simple preparation method, lower cost compared with the noble metal and no pollution to the environment and is beneficial to large scale preparation and production. According to the preparation of the photocatalyst by utilizing the graphene as the catalyst promoter, the cost of utilizing solar for the hydrogen production is reduced, and a new method for increasing the hydrogen production efficiency of the photodecomposition water is developed.
Description
Technical field
The present invention relates to a kind of decomposing water with solar energy catalyst for preparing hydrogen preparation method who does not utilize noble metal as co-catalyst, belong to photocatalysis technology and environmental science.
Background technology
Hydrogen Energy is considered to one of following optimal secondary energy sources because of its pollution-free grade.Along with utilization and exploitation, study focus for one that can utilize decomposing water with solar energy hydrogen manufacturing to become in the hydrogen preparation field to solar energy resources.Yet hydrogen production efficiency is generally lower in most of photocatalysis hydrogen production systems, and still needs precious metal material as co-catalyst.Therefore, one of photolysis water hydrogen very importance be exactly preparation with better stability, visible light-responded, high hydrogen production efficiency and cheap photochemical catalyst.The photochemical catalyst of based semiconductor and semiconductor composite are widely used in the photolysis water hydrogen system owing to have good physics and chemical property.For example, CdS, bandwidth is the n type semiconductor of 2.4eV, has the performance of visible absorption and photocatalytic hydrogen production by water decomposition.But, need transmit with other semiconductor or inorganic, the compound acceleration electronics of organic material, to improve its stability because the CdS photochemical stability is relatively poor, perishable.TiO
2Have high catalytic activity, chemical stability is strong, pollution-free, cheap, is most widely used material in the photocatalysis system at present.But titanium dioxide nano-particle need be by doping, dye sensitization, improve its response to visible light with modes such as other narrow bandwidth semiconductor are compound, to improve light hydrogen production by water decomposition efficient.Usually, precious metals pt, Pd, Ru and Rh are as co-catalyst and CdS, TiO
2Compound Deng semi-conducting material, to improve its photocatalytic activity and light hydrogen production by water decomposition efficient, but noble metal costs an arm and a leg, the difficult recovery, unfriendly to environment, thereby restricted its use, so the researcher wishes to set up new hydrogen manufacturing system or find not only cheap but also green material environmental protection replaces noble metal, reach high efficiency, low cost hydrogen manufacturing.
Have good electronics as carbon nano-structured materials such as CNTs and accept and hereditary property, the compound of these carbon structure materials and semi-conducting material has been applied in the light hydrogen production by water decomposition.Wherein Graphene has unique electric transmission character, and because Graphene has the individual layer atomic structure, can make the clear films material, and its unique bi-dimensional cellular shape planar structure all will improve absorption and electric transmission character to light greatly in addition.Therefore with grapheme material and TiO
2, the compound of semi-conducting material such as CdS will have good photocatalytic activity, conductibility and controllability simultaneously, thereby improve the efficient of light hydrogen production by water decomposition.This composite has higher hydrogen production efficiency, and the more important thing is this catalyst low price, and preparation is simple, and the new approaches or the new method that can replace noble metal catalyst is provided for us.
Summary of the invention
The purpose of this invention is to provide a kind of solar energy photocatalytic hydrogen production by water decomposition catalysis material that does not utilize precious metal material as co-catalyst, and this catalysis material utilizes Graphene as co-catalyst, have higher photocatalysis hydrogen production efficient, can replace precious metals pt.
The preparation that does not contain the photochemical catalyst of precious metal material of the present invention comprises following two aspects:
(1) preparation of CdS-graphene composite material photochemical catalyst;
(2) TiO
2The preparation of-graphene composite material photochemical catalyst.
The preparation process of CdS-graphene oxide photochemical catalyst is as follows:
The Sulfonated Graphene of 2mg is scattered in the deionized water for ultrasonic 30min of 20mL, dropwise splashes into the CdCl of 6mL 0.1mol/L
2Solution stirs the Na that splashes into 10mL 0.05mol/L behind the 2h again
2S solution, and after stirring 3h, after filtration is repeatedly washed, dry in 70 ℃ vacuum environment.
The preparation process of P25-graphene composite material photochemical catalyst is as follows:
The 2mg graphene oxide is scattered in 20mL water and the 10mL alcohol mixed solvent, and sonic oscillation 1h is uniformly dispersed it.Add 200mg titanium dioxide then, fully stir 2h, put into the stainless steel cauldron of 50mL, at 120 ℃ of heating 3h, after repeatedly washing after filtration, dry in 70 ℃ vacuum environment.
Method of the present invention is the Na with 0.25mol/L
2The Na of S solution and 0.35mol/L
2SO
3Solution is as sacrifice agent, with CdS-Graphene, the TiO of Graphene modification
2-Graphene composite nano materials is as photochemical catalyst, and light source carries out photocatalytic hydrogen production by water decomposition for the metal halid lamp of approximate solar spectrum under with nitrogen deoxygenation 40min condition.Wherein, CdS-Graphene photocatalysis hydrogen production be visible light (under the illuminate condition of λ＞400nm), TiO
2-Graphene composite nano materials photochemical catalyst is to carry out under all band illuminate condition.
Method of the present invention is CdS-Graphene, the TiO that Graphene is modified
2-Graphene composite nano materials is as the hydrogen generation efficiency of photochemical catalyst and CdS-Pt compound, the TiO of light deposition 2%Pt
2The photochemical catalyst of-Pt compound hydrogen production efficiency is under the same conditions compared.
Method of the present invention is that CdS-Graphene, TiO2-Graphene composite nano materials that Graphene is modified are compared with simple CdS, the hydrogen generation efficiency hydrogen production efficiency under the same conditions of P25 nano particle as the hydrogen generation efficiency of photochemical catalyst.
Advantage of the present invention and effect are:
(1) utilizes CdS-Graphene, the TiO of Graphene as co-catalyst
2-Graphene composite nano materials photochemical catalyst has very high hydrogen generation efficiency, can compare favourably with the catalyst hydrogen production efficiency under the same conditions of the Pt with same amount even better.
(2) Graphene has improved electric transmission speed as co-catalyst, has promoted effective separation of electron hole, has reduced the compound probability of exciton, and then has increased the efficient that light decomposes aquatic products hydrogen;
(3) Graphene for we provide a kind of more with low cost than noble metal, preparation technology is simple, and the new selection that environment is not polluted, this material will have the huge applications potentiality at aspects such as solar cell, photolysis water hydrogen, photocatalytic degradations.
Description of drawings
Fig. 1 is that CdS compound photochemical catalyst hydrogen production efficiency under radiation of visible light of CdS-graphene composite material, simple CdS nano particle, Pt load compares.
Fig. 2 is that P25 nano particle photochemical catalyst hydrogen production efficiency under all band irradiation of P25-graphene composite material, P25 nano particle, Pt load compares.
The specific embodiment
Below in conjunction with embodiment the present invention is illustrated:
The Sulfonated Graphene of embodiment 1:2mg is scattered in the deionized water for ultrasonic 30min of 20mL, dropwise splashes into the CdCl of 6mL 0.1mol/L
2Solution stirs the Na that splashes into 10mL 0.05mol/L behind the 2h again
2S solution, and after stirring 3h, after filtration is repeatedly washed, dry in 70 ℃ vacuum environment.
Embodiment 2: the 2mg graphene oxide is scattered in 20mL water and the 10mL alcohol mixed solvent, and sonic oscillation 1h is uniformly dispersed it.Add 200mg titanium dioxide nano-particle (P25, German Degussa degussa company) then, fully stir 2h, put into the stainless steel cauldron of 50mL, at 120 ℃ of heating 3h, repeatedly after the washing, dry in 70 ℃ vacuum environment after filtration.
Embodiment 3: simple CdS nanometer particle process method such as embodiment 1, the CdCl of 6mL 0.1mol/L
2Solution stirs the Na that splashes into 10mL 0.05mol/L behind the 2h again
2S solution, and after stirring 3h, after filtration is repeatedly washed, dry in 70 ℃ vacuum environment.
Embodiment 4: the composite catalyst that contains 2%Pt utilizes the method for light deposition, and the CdS of 100mg or P25 nano particle are scattered in the deionized water of 20ml, splash into the H of the 0.39mol/L of 27uL respectively
2PtCl
4The aqueous solution, under stirring condition, utilize then visible light (behind the illumination 3h of λ＞400nm), filter repeatedly washing after, dry in 70 ℃ vacuum environment.
Embodiment 5: reaction vessel is the 50mL quartz test tube, the Na of 0.25mol/L
2The Na of S solution and 0.35mol/L
2SO
3Liquor capacity is 20mL, CdS-graphene composite material photochemical catalyst 30mg, and logical nitrogen 40min removes the oxygen in the solution, with anti-chewing-gum plug sealing.Sample is in the recirculated cooling water in the visible light illumination process, carries out at ambient temperature to guarantee reaction.The hydrogen that produces in the system detects with GC-14C (Shimadzu) gas chromatograph,
Molecular sieve column (3m * 2mm), thermal conductivity cell detector (TCD), carrier gas is a nitrogen, adopts external standard method to measure.
Embodiment 6: present embodiment catalyst as different from Example 5 is simple CdS nano particle, and other step and experiment condition are identical with embodiment one.
Embodiment 7: present embodiment catalyst as different from Example 5 is the CdS nano particle that load has 2%Pt, and other step and experiment condition are identical with embodiment one.
Embodiment 8: present embodiment catalyst as different from Example 5 is TiO
2-graphene composite material photochemical catalyst, illumination condition are all band, and other step and experiment condition are identical with embodiment one.
Embodiment 9: present embodiment catalyst as different from Example 5 is simple P25 nano particle photochemical catalyst, and illumination condition is an all band, and other step and experiment condition are identical with embodiment one.
Embodiment 10: present embodiment catalyst as different from Example 5 is the P25 nano particle that load has 2%Pt, and illumination condition is an all band, and other step and experiment condition are identical with embodiment one.
Photochemical catalyst hydrogen manufacturing experimental result in the embodiment of the invention shows: this catalysis material utilizes Graphene as co-catalyst, has higher photocatalysis hydrogen production efficient, can effectively replace the precious metals pt of identical percentage composition.
Claims (12)
1. a novel photocatalysis photolysis water hydrogen Preparation of catalysts method of utilizing Graphene as co-catalyst comprises CdS-Graphene, TiO
2-graphene composite material photochemical catalyst the preparation method.It is characterized in that: utilize Graphene as co-catalyst, improved electric transmission speed, promoted effective separation of electron hole, reduced the compound probability of exciton, and then increased the efficient that light decomposes aquatic products hydrogen;
2. require the preparation method of described CdS-graphene composite material as right 1, it is characterized in that: the Sulfonated Graphene of 2mg is scattered in the deionized water for ultrasonic 30min of 20mL, dropwise splashes into the CdCl of 6mL 0.1mol/L
2Solution stirs the Na that splashes into 10mL 0.05mol/L behind the 2h again
2S solution, and after stirring 3h, after filtration is repeatedly washed, dry in 70 ℃ vacuum environment.
3. require the preparation method of described CdS-graphene composite material as right 2, it is characterized in that: used cadmium salt can comprise CdCl
2, Cd (NO
3)
2, CdSO
4Deng the salt that contains cadmium ion, and various inorganic, organic S of containing that can generate CdS with cadmium salt
2-Salt.
4. require the preparation method of described CdS-graphene composite material as right 2, it is characterized in that: can carry out the CdS nanostructured of compound different-shape and structure with Graphene, comprise nanotube, nano wire, nanometer band, nano particle and laminated structure etc.
5. require the preparation method of described CdS-graphene composite material as right 2, it is characterized in that: make Graphene modify the electronegative the whole bag of tricks in back, but electronegative Electrostatic Absorption chromium ion generates the CdS-graphene composite material thereby be easy to the sulphion reaction.
6. require described TiO as right 1
2The preparation method of-graphene composite material photochemical catalyst is characterized in that: the 2mg graphene oxide is scattered in 20mL water and the 10mL alcohol mixed solvent, and sonic oscillation 1h is uniformly dispersed it.Add 200mg titanium dioxide then, fully stir 2h, put into the stainless steel cauldron of 50ml, at 120 ℃ of heating 3h, after repeatedly washing after filtration, dry in 70 ℃ vacuum environment.
7. as the right 6 described TiO that requires
2The preparation method of-graphene composite material photochemical catalyst is characterized in that: prepare the used TiO of composite with Graphene
2Comprise P25 and utilize the different-shape such as nano particle, nano wire, nanotube, nanometer band of the titanium dioxide of other method preparation or the TiO of structure
2
8. as the right 6 described TiO that requires
2The preparation method of-graphene composite material photochemical catalyst is characterized in that: TiO
2The content of Graphene can be 0.5%-4% in the-graphene composite material, and the heating-up temperature of reactor can be 100-180 ℃.
9. require the described CdS-of utilization Graphene, TiO as right 1
2-graphene composite material photochemical catalyst photolysis water hydrogen is characterized in that: at the Na of 0.25mol/L
2The Na of S solution and 0.35mol/L
2SO
3Solution is as sacrifice agent solution 20mL, CdS-graphene composite material photochemical catalyst 30mg, and logical nitrogen 40min removes the oxygen in the solution, seals with anti-chewing-gum plug.Sample is in the recirculated cooling water in the visible light illumination process, carries out at ambient temperature to guarantee reaction.
10. require the described CdS-of utilization Graphene, TiO as right 9
2-graphene composite material photochemical catalyst photolysis water hydrogen is characterized in that: used solution is the Na at variable concentrations
2S solution and Na
2SO
3Solution, methanol solution etc. are also included within and directly carry out photocatalysis hydrogen production and oxygen in the simple aqueous solution or the organic solution as the solution of sacrifice agent.
11. require the described co-catalyst that utilizes as right 1, it is characterized in that: Graphene or graphene oxide and other material are as WO
3, ZnO, Fe
2O
3, TaO, NbO, semi-conducting materials such as CdSe, CdTe carry out the compound photochemical catalyst hydrogen production by water decomposition that carries out.
12. require the described co-catalyst that utilizes as right 1, it is characterized in that: the Graphene after various modifications or the doping, graphene oxide material are as co-catalyst.
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