CN115739128B - RuSe 2 Piezoelectricity H-production by CdS composite catalyst 2 Application in (a) - Google Patents
RuSe 2 Piezoelectricity H-production by CdS composite catalyst 2 Application in (a) Download PDFInfo
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Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The invention belongs to the field of piezoelectric photocatalysts, and in particular relates to RuSe 2 H produced by CdS composite catalyst 2 Is used in the application of (a). RuSe synthesis by simple impregnation method 2 the/CdS composite catalyst is used for producing H by piezoelectric photocatalysis under the synergistic effect of solar light irradiation and ultrasonic vibration 2 . The invention has the advantages of simple synthesis, green pollution-free and strong operability. The prepared catalyst has the characteristics of rich active sites, excellent stability, no secondary pollution and the like.
Description
Technical Field
The invention belongs to the technical field of piezoelectricity photocatalysis, and in particular relates to RuSe 2 Piezoelectricity H-production by CdS composite catalyst 2 Is used in the field of applications.
Background
The energy crisis hampers the world's socioeconomic development, and efforts are underway to develop clean energy. Hydrogen (H) 2 ) Are considered as potential clean energy carriers due to their high energy density and low environmental pollution. Piezoelectric-photocatalytic technology, i.e. coupling piezoelectric effect into photocatalytic reaction, light excitationThe action of the generator increases the carrier concentration of the material bulk phase, and the existing polarized electric field eliminates the shielding action of internal and external charges, so that bulk-phase electron-hole separation can be continuously driven. Further, the material is formed of two or more piezoelectric semiconductors (e.g. BaTiO 3 、KNbO 3 、BiFeO 3 ZnS and ZnSnO 3 Etc.) integrated piezoelectric-photocatalytic heterojunction, the generation of a bipolar or multipolarized electric field can drive the separation of electrons and holes of the material interface and bulk phase at the same time, facilitating the overall charge transfer, thus realizing excellent catalytic performance.
The catalytic performance can be effectively improved by constructing the promoted composite material with rich electron capture as an active site of oxidation-reduction reaction. At present, how to construct a high-efficiency piezoelectric photocatalyst is still an important point and a difficult point of research. CdS semiconductors are recognized as visible light driven photocatalysts with narrow forbidden bands, and are widely used in the field of photocatalysis. Although the CdS has serious photo-corrosion and high charge recombination speed, the structure-dependent photochemical performance of the CdS can be easily regulated by constructing different nano structures, so that the application potential of the CdS is further expanded. RuSe 2 As a very promising promoter, it can replace rare noble metals, it can improve charge separation efficiency as a promoter, se as an active site can promote hydrogen production rate. RuSe has not been reported at present 2 Preparation of/CdS composite catalyst and application thereof in piezoelectricity-photocatalysis.
Here we synthesized a RuSe 2 The CdS piezoelectric photocatalyst can effectively utilize the polarized electric field to improve H production 2 Efficiency is improved. Under the combined action of sunlight and ultrasonic waves, the optimized RuSe 2 Production of H by CdS 2 The amount was 13.6 times that of pure CdS. This work demonstrates RuSe 2 the/CdS composite material can introduce a polarized electric field under the synergistic effect of piezoelectricity-photocatalysis, so that the piezoelectricity catalytic performance is greatly improved.
Disclosure of Invention
The invention aims to provide a mixed-phase RuSe 2 Preparation method of/CdS composite catalyst and application of catalyst in piezoelectricity light H production 2 Has high catalytic activity and better stability.
The technical scheme of the invention is as follows: ruSe 2 Piezoelectricity H-production by CdS composite catalyst 2 Including: ruSe is to 2 Adding the/CdS composite catalyst into water, fully dispersing, adding lactic acid, and then introducing N 2 Finally, performing airtight reaction under the irradiation of ultrasound and sunlight;
the RuSe 2 The preparation method of the/CdS composite catalyst comprises the steps of mixing RuSe 2 Dispersing with CdS in distilled water, fully dispersing, reacting, filtering at room temperature after reaction, washing, drying to obtain dark green powder RuSe 2 a/CdS composite catalyst;
RuSe in composite catalyst 2 The mass is 1% -3% of the mass of CdS;
RuSe 2 is prepared through mixing selenium powder with C 2 H 6 O 2 Suspension and RuCl 3 Mixing the water solution fully, regulating to neutrality, reacting in microwave chemical reactor fully, separating out solid after reaction, washing and drying, and adding N 2 Annealing for 2+/-0.1 h at 400-500 ℃ under the atmosphere.
Preferably, the solar lamp power is 55W and the ultrasonic power is 240W.
The RuSe provided by the invention 2 In the preparation of the/CdS composite catalyst, the reaction time in the preparation of the composite catalyst is preferably 16-20 h; and/or RuSe in composite catalyst 2 The mass is 1.25% -1.75% of the mass of CdS.
Further, cdS preparation includes reacting CdCl 2 ·2.5H 2 Adding O and thiourea into ethylenediamine, fully mixing, performing hydrothermal reaction at 160 ℃ for 48 hours, collecting the obtained precipitate after the reaction is finished, washing with distilled water and ethanol for multiple times, and finally drying in vacuum.
More specifically, cdS was prepared by adding 2.312g of CdCl 2 ·2.5H 2 O and 2.312g thiourea were added to 50mL ethylenediamine. Transferring the mixed solution into a reaction kettle lined with polytetrafluoroethylene, performing hydrothermal reaction in an oven at 160 ℃ for 48 hours, centrifugally collecting the obtained precipitate, and washing with distilled water and ethanol for multiple times. Finally, vacuum drying at 60 DEG CDrying for 12h, and grinding to obtain yellow powder.
Further, ruSe 2 The power of the microwave chemical reactor in the preparation is set to 800+/-20W, and the time is set to 3+/-1 min.
More specifically, ruSe 2 Is prepared by dispersing 0.0234g selenium powder in 50mL C 2 H 6 O 2 Stirring, ultrasonic treating for 1 hr, and adding 583.16 μl RuCl 3 Aqueous solution (53.33 mg. ML) -1 RuCl 3 ·χH 2 O), stirring for 1h, to form a well-dispersed suspension. An appropriate amount of 0.1M KOH solution was added to adjust the pH of the suspension to neutral.
The irradiation power of the microwave chemical reactor is 800W, and the irradiation time is 3min. The resulting suspension after the reaction was washed several times by centrifugation with deionized water and then dried overnight in a vacuum oven at 60 ℃. RuSe to be obtained 2 Transferring the sample into a quartz tube, at N 2 Annealing at 400 ℃ for 2h under the atmosphere.
Compared with the prior art, the invention has the following beneficial effects
(1) The catalyst provided by the invention is RuSe 2 The CdS composite catalyst has the characteristics of simple synthesis condition, easy operation, high speed, high efficiency, good stability and the like.
(2)RuSe 2 The introduction of the catalyst did not change the crystal structure of CdS, and no other diffraction peaks appeared, indicating RuSe 2 the/CdS composite material has excellent crystallinity and purity. RuSe in composite catalyst 2 When the mass is 1% -3% of the mass of CdS, the hydrogen production capacity under the action of piezoelectricity-light can be obviously improved by cooperating with ultrasound and sunlight illumination, and the hydrogen production rate is obviously improved.
Drawings
FIG. 1 is a RuSe synthesized in example 1 2 Transmission electron microscopy of CdS catalyst.
FIG. 2 is a diagram showing the different ratios of RuSe synthesized in examples 1, 4, 7, 10 and comparative examples 1, 4 2 CdS composite material and CdS, ruSe 2 Is a XRD pattern of (C).
FIG. 3 shows the different ratios of RuS synthesized in examples 1, 4, 7, 10 and comparative examples 1, 4 under the simultaneous irradiation of sunlight and ultrasonic vibratione 2 CdS composite, cdS and 2H RuSe 2 Production of H by CdS 2 Is a performance graph of (a). FIG. 4 is a chart showing the ratio of RuSe under the action of ultrasonic vibration 2 CdS composite, cdS and 2H RuSe 2 Production of H by CdS 2 Is a performance graph of (a).
FIG. 5 is a chart of RuSe at different ratios under irradiation of sunlight 2 CdS composite, cdS and 2H RuSe 2 Production of H by CdS 2 Is a performance graph of (a).
Detailed Description
The present invention is not limited to the following embodiments, and those skilled in the art can implement the present invention in various other embodiments according to the present invention, or simply change or modify the design structure and thought of the present invention, which fall within the protection scope of the present invention. It should be noted that, without conflict, the embodiments of the present invention and features of the embodiments may be combined with each other.
The H production 2 The efficiency is calculated according to the following formula:
r: h production 2 Rate, unit: mu mol/(g.h)
V: hydrogen volume, unit: mu L (mu L)
m: catalyst mass, unit: g
t: reaction time, unit: h is a
Example 1
0.0234g of selenium powder is firstly dispersed in 50mL of C 2 H 6 O 2 Stirring, ultrasonic treating for 1 hr, and adding 583.16 μl RuCl 3 Aqueous solution (53.33 mg. ML) -1 RuCl 3 ·χH 2 O), stirring for 1h, to form a well-dispersed suspension. An appropriate amount of 0.1M KOH solution was added to adjust the pH of the suspension to neutral.
The irradiation power of the solid-liquid microwave synthesizer is 800W, and the irradiation time is 3min. The suspension obtained after the reaction was centrifugally washed with deionized water several times. Finally, at 60 DEG CDrying in a vacuum oven overnight. RuSe to be obtained 2 Transferring the sample into a quartz tube, at N 2 Annealing at 400 ℃ for 2h under the atmosphere.
The RuSe is prepared 2 The catalyst and the CdS catalyst in comparative example 1 were dissolved in distilled water, sonicated for 1h, stirred for 4h, and mixed well. Centrifuging, washing and drying at room temperature to obtain dark green powder, namely RuSe 2 A CdS composite catalyst. Adding RuSe 2 The mass is 1% of the mass of CdS.
2mg of the composite catalyst was weighed, 18mL of deionized water was added, and the mixture was sonicated for 30min. Adding 2mL of lactic acid, and introducing 30min N 2 Finally, sealing for 1h under the irradiation of ultrasonic and sunlight. After the experiment was completed, the gas in the 0.5mL tube was extracted, the peak area was detected by a gas chromatograph, and H production was calculated 2 The rate is analyzed and calculated to obtain the H production 2 The rate was 30858.76. Mu. Mol/(g.h).
Example 2
Compared with example 1, the difference is that: the conditions in the application method were changed to ultrasound, otherwise the same as in example 1.RuSe 2 Production of H by CdS catalyst 2 The rate was 723.24. Mu. Mol/(g.h).
Example 3
Compared with example 1, the difference is that: the conditions in the application method were changed to solar light, and the same as in example 1 was repeated. RuSe 2 Production of H by CdS catalyst 2 The rate was 21012.35. Mu. Mol/(g.h).
Example 4
Compared with example 1, the difference is that: ruSe is added in the preparation process 2 The mass was 1.5% of the mass of CdS, and the other preparation methods were the same as in example 1.
Application method As in example 1, ruSe prepared in example 4 2 H produced by CdS composite catalyst 2 The rate was 63857.24. Mu. Mol/(g.h), 7.54 times that of the pure CdS catalyst.
Under the same condition, adjust RuSe 2 The mass is 1.25% of the mass of CdS, and the hydrogen production rate is 50358 mu mol/(g.h); adjusting RuSe 2 The mass is 1.75% of the mass of CdS, and the hydrogen production rate is 48709 mu mol/(g.h).
Example 5
Compared with example 4, the difference is that: the conditions in the application method were changed to ultrasound, otherwise the same as in example 4.RuSe 2 H produced by CdS composite catalyst 2 The rate was 919.40. Mu. Mol/(g.h).
Example 6
Compared with example 4, the difference is that: the conditions in the application method were changed to solar light, and the same as in example 4 was repeated. RuSe 2 Production of H by CdS catalyst 2 The rate was 33269.43. Mu. Mol/(g.h).
Example 7
Compared with example 1, the difference is that: ruSe is added in the preparation process 2 The mass was 2% of the mass of CdS, and the other preparation methods were the same as in example 1.
Application method As in example 1, ruSe prepared in example 7 2 H produced by CdS composite catalyst 2 The rate was 27561.49. Mu. Mol/(g.h).
Example 8
Compared with example 7, the difference is that: the conditions in the application method were changed to ultrasound, otherwise the same as in example 7.RuSe 2 H produced by CdS composite catalyst 2 The rate was 630.67. Mu. Mol/(g.h).
Example 9
Compared with example 7, the difference is that: the conditions in the application method were changed to solar light, and the same as in example 7 was repeated. RuSe 2 Production of H by CdS catalyst 2 The rate was 18520.50. Mu. Mol/(g.h).
Example 10
Compared with example 1, the difference is that: ruSe is added in the preparation process 2 The mass was 3% of the mass of CdS, and the other preparation methods were the same as in example 1.
Application method As in example 1, ruSe prepared in example 7 2 H produced by CdS composite catalyst 2 The rate was 26428.49. Mu. Mol/(g.h).
Example 11
Compared with example 10, the difference is that: the conditions in the application method were changed to ultrasound, otherwise the same as in example 10.RuSe 2 H produced by CdS composite catalyst 2 The rate was 607.12. Mu. Mol/(g.h).
Example 12
Compared with example 10, the difference is that: the conditions in the application method were changed to solar light, and the same as in example 10 was repeated. RuSe 2 Production of H by CdS catalyst 2 The rate was 13547.11. Mu. Mol/(g.h).
Comparative example 1
Will be 2.312g CdCl 2 ·2.5H 2 O and 2.312g thiourea were added to 50mL ethylenediamine. Transferring the mixed solution into a reaction kettle lined with polytetrafluoroethylene, performing hydrothermal reaction in an oven at 160 ℃ for 48 hours, centrifugally collecting the obtained precipitate, and washing with distilled water and ethanol for multiple times. Finally, vacuum drying is carried out for 12 hours at 60 ℃, and CdS yellow powder is obtained by grinding.
2mgCdS catalyst was weighed, 18mL of water was added, and ultrasound was performed for 30min. Then adding 2mL of lactic acid, and then introducing 30min N 2 Finally, sealing for 1h under the irradiation of ultrasonic and sunlight. After the experiment was completed, the gas in the 0.5mL tube was extracted, the peak area was detected by a gas chromatograph, and H production was calculated 2 The rate is analyzed and calculated to obtain the H production 2 The rate was 8467.74. Mu. Mol/(g.h).
Comparative example 2
Compared with comparative example 1, the difference is that: the conditions in the application method were changed to ultrasound, and the other was the same as in comparative example 1.CdS catalyst H production 2 The rate was 11.69. Mu. Mol/(g.h).
Example 3
Compared with comparative example 1, the difference is that: the conditions in the application method are changed to sun light, and the other conditions are the same as those in comparative example 1.CdS catalyst H production 2 The rate was 269.17. Mu. Mol/(g.h).
Comparative example 4
The composite catalyst preparation method is different from example 4 in that: ruSe is to 2 Calcining the sample in a tube furnace for 2 hours at 600 ℃ under nitrogen atmosphere to obtain black powder pure 2H RuSe 2 And (3) a sample.
Application method the same as in example 4, 2H RuSe prepared in comparative example 4 2 Production of H by CdS catalyst 2 The rate was 17187.65. Mu. Mol/(g.h).
Comparative example 5
Compared with comparative example 4, the difference is that: the conditions in the application method were changed to ultrasound, and the other was the same as in comparative example 4.2H RuSe 2 Production of H by CdS catalyst 2 The rate was 143.71. Mu. Mol/(g.h).
Comparative example 6
Compared with comparative example 4, the difference is that: the conditions in the application method are changed to sun light, and the other conditions are the same as those in comparative example 4.2H RuSe 2 Production of H by CdS catalyst 2 The rate was 10235.03. Mu. Mol/(g.h).
Claims (6)
1.RuSe 2 Piezoelectricity H-production by CdS composite catalyst 2 Is characterized by comprising: ruSe is to 2 Adding the/CdS composite catalyst into water, fully dispersing, adding lactic acid, and then introducing N 2 Finally, performing airtight reaction under the irradiation of ultrasound and sunlight;
the RuSe 2 Preparation of the/CdS composite catalyst comprising reacting RuSe 2 Dispersing with CdS in distilled water, fully dispersing, reacting, filtering at room temperature after reaction, washing, drying to obtain dark green powder RuSe 2 a/CdS composite catalyst;
RuSe in composite catalyst 2 The mass is 1% -3% of the mass of CdS;
RuSe 2 is prepared through mixing selenium powder with C 2 H 6 O 2 Suspension and RuCl 3 Mixing the water solution fully, regulating to neutrality, reacting in microwave chemical reactor fully, separating out solid after reaction, washing and drying, and adding N 2 Annealing for 2+/-0.1 h at 400-500 ℃ under the atmosphere.
2. Ruse according to claim 1 2 Piezoelectricity H-production by CdS composite catalyst 2 Is characterized in that the solar lamp power is 55W and the ultrasonic power is 240W.
3. Ruse according to claim 1 2 Piezoelectricity H-production by CdS composite catalyst 2 The application of the catalyst is characterized in that the reaction time in the preparation of the composite catalyst is 16-20 h.
4.Ruse according to claim 1 2 Piezoelectricity H-production by CdS composite catalyst 2 Wherein the CdS preparation comprises the steps of 2 ·2.5H 2 Adding O and thiourea into ethylenediamine, fully mixing, performing hydrothermal reaction at 160 ℃ for 48 hours, collecting the obtained precipitate after the reaction is finished, washing with distilled water and ethanol for multiple times, and finally drying in vacuum.
5. Ruse according to claim 1 2 Piezoelectricity H-production by CdS composite catalyst 2 Is characterized in that RuSe in the composite catalyst 2 The mass is 1.25% -1.75% of the mass of CdS.
6. Ruse according to claim 1 2 Piezoelectricity H-production by CdS composite catalyst 2 Is characterized by RuSe 2 The power of the microwave chemical reactor in the preparation is set to 800+/-20W, and the time is set to 3+/-1 min.
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| "Photocatalytic and photo electrochemical properties of cadmium zincsulfide solid solution in the presence of Pt and RuS2 dual co-catalysts";A.P. Gaikwad et al.;《Applied Catalysis A: General》;第517卷;第91-99页 * |
| "孪晶Zn0.5Cd0.5S/Ru2S3-PSII 体系的组装及其 光催化全分解水应用研究";邓海朗等;《广东化工》;第48卷(第11期);第29-30页 * |
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