CN115739128A - RuSe 2 Photoelectric production H of CdS composite catalyst 2 In (1) - Google Patents
RuSe 2 Photoelectric production H of CdS composite catalyst 2 In (1) Download PDFInfo
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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Abstract
The invention belongs to the field of piezoelectric photocatalysts, and particularly relates to RuSe 2 Production of H by CdS composite catalyst 2 The use of (1). RuSe synthesis by simple impregnation method 2 the/CdS composite catalyst is used for producing H through piezoelectric photocatalysis under the synergistic effect of sunlight irradiation and ultrasonic vibration 2 . The invention has simple synthesis, no pollution 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 piezoelectric photocatalysis, and particularly relates to RuSe 2 catalyst/CdS complexChemical-pressure electrophoto production H 2 The use of (1).
Background
The energy crisis hinders the socioeconomic development of the world, and people are striving to develop clean energy. Hydrogen (H) 2 ) Is considered as a potential clean energy carrier due to high energy density and low environmental pollution. The piezoelectric-photocatalytic technology is characterized in that a piezoelectric effect is coupled into a photocatalytic reaction, the carrier concentration of a material bulk phase is increased under the action of light excitation, the shielding effect of internal and external charges is eliminated by a polarization electric field, and the bulk phase electron hole separation can be continuously driven. Further, from two or more piezoelectric semiconductors (e.g. BaTiO) 3 、KNbO 3 、BiFeO 3 ZnS and ZnSnO 3 Etc.) integrated piezoelectric-photocatalytic heterojunction, generates dual or multi-polarized electric field to drive the separation of electrons and holes of material interface and bulk phase, and facilitates the integral charge transfer, thereby realizing excellent catalytic performance.
By constructing the cocatalyst composite material with abundant electron capture as an active site of the oxidation-reduction reaction, the catalytic performance can be effectively improved. At present, how to construct a high-efficiency piezoelectric photocatalyst is still the focus and difficulty of research. The CdS semiconductor is recognized as a visible light drive photocatalyst with a narrow forbidden band, and is widely applied to the field of photocatalysis. Although the photo-etching of CdS is serious and the charge recombination speed is high, the structure-dependent photochemical performance of CdS can be easily adjusted by constructing different nano structures, so that the application potential of CdS is further expanded. RuSe 2 As a promising cocatalyst, the catalyst can replace rare noble metals, the catalyst can be used as an auxiliary catalyst to improve the charge separation efficiency, and Se as an active site can promote the hydrogen production rate. RuSe has not been reported yet 2 The preparation of the/CdS composite catalyst and the application thereof in piezoelectric-photocatalysis.
Here, we have synthesized a RuSe 2 the/CdS piezoelectric photocatalyst can effectively utilize a polarization electric field to improve the yield H 2 Efficiency. Under the combined action of sunlight and ultrasonic waves, optimized RuSe 2 CdS production H 2 The amount was 13.6 times that of pure CdS. This employee's cardImplements RuSe 2 the/CdS composite material can introduce a polarization electric field under the synergistic action of piezoelectric-photocatalysis, so that the piezoelectric catalysis performance is greatly improved.
Disclosure of Invention
The invention aims to provide mixed-phase RuSe 2 Preparation method of/CdS composite catalyst and application of catalyst to piezoelectric light production of H 2 Has high catalytic activity and better stability.
The technical scheme of the invention is as follows: ruSe 2 Photoelectric H production by CdS composite catalyst 2 The use of (a), comprising: mixing RuSe 2 Adding the CdS composite catalyst into water, fully dispersing, adding lactic acid, and introducing N 2 Finally, carrying out closed reaction under the irradiation of ultrasound and sunlight;
the RuSe being 2 The preparation method of the/CdS composite catalyst comprises the step of mixing RuSe 2 And CdS are dispersed in distilled water, and are subjected to full dispersion reaction, and after the reaction is finished, the mixture is filtered, washed and dried at room temperature to obtain blackish 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 the preparation method comprises mixing selenium powder C 2 H 6 O 2 Suspension with RuCl 3 Mixing the water solution, regulating to neutrality, reacting in microwave chemical reactor, separating solid, washing, drying, and adding N 2 Annealing at 400-500 deg.c in atmosphere for 2 +/-0.1 hr.
Preferably, the power of the sun lamp is 55W, and the power of the ultrasonic wave is 240W.
The RuSe provided by the invention 2 In the preparation of the/CdS composite catalyst, the reaction time is preferably 16-20 h in the preparation of the composite catalyst; and or, ruSe in composite catalyst 2 The mass is 1.25% -1.75% of the mass of CdS.
Further, cdS preparation includes adding CdCl 2 ·2.5H 2 Adding O and thiourea into ethylenediamine, mixing, performing hydrothermal reaction at 160 deg.C for 48 hr, collecting precipitate, adding distilled water and ethanolWashing, and vacuum drying.
More specifically, cdS preparation 2.312g of CdCl 2 ·2.5H 2 O and 2.312g of thiourea were added to 50mL of ethylenediamine. Transferring the mixed solution into a reaction kettle with a polytetrafluoroethylene lining, carrying out hydrothermal reaction in an oven at the reaction temperature of 160 ℃ for 48 hours, centrifugally collecting the obtained precipitate, and washing the precipitate with distilled water and ethanol for multiple times. Finally, vacuum drying is carried out for 12h at the temperature of 60 ℃, and yellow powder is obtained by grinding.
Further, ruSe 2 In the preparation, the power of the microwave chemical reactor is set to 800 +/-20W, and the time is set to 3 +/-1 min.
More specifically, ruSe 2 The preparation method comprises dispersing 0.0234g of selenium powder in 50mL of C 2 H 6 O 2 Stirring, ultrasonic treating for 1h, adding 583.16 μ L RuCl 3 Aqueous solution (53.33 mg. ML) -1 RuCl 3 ·χH 2 O), stirring for 1h to form a well-dispersed suspension. Adding a proper amount of 0.1M KOH solution, and adjusting the pH of the suspension to be neutral.
The irradiation power of the microwave chemical reactor is 800W, and the irradiation time is 3min. The suspension obtained after the reaction was washed several times with deionized water by centrifugation and then dried overnight in a vacuum oven at 60 ℃. RuSe to be obtained 2 The sample was transferred to 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 synthesis condition of the/CdS composite catalyst is simple, the operation is easy, and the catalyst has the characteristics of high speed, high efficiency, good stability and the like.
(2)RuSe 2 The introduction of the catalyst does not change the crystal structure of CdS, and other diffraction peaks do not appear, indicating that RuSe 2 the/CdS composite material has excellent crystallinity and purity. RuSe in composite catalyst 2 When the mass of the CdS is 1-3%, the hydrogen production capability under the piezoelectric-optical action can be obviously improved by cooperating with the ultrasonic and sunlight illumination, and the hydrogen production rate is obviously improved.
Drawings
FIG. 1 is a schematic view ofExample 1 synthetic RuSe 2 Transmission electron micrograph of/CdS catalyst.
FIG. 2 shows RuSe synthesized in examples 1, 4, 7 and 10 and comparative examples 1 and 4 in different ratios 2 Composite material of/CdS and CdS, ruSe 2 XRD pattern of (a).
FIG. 3 shows RuSe synthesized in different proportions in examples 1, 4, 7, 10 and comparative examples 1, 4 under the action of both sunlight and ultrasonic vibration 2 Composite of/CdS, cdS and 2H RuSe 2 CdS production H 2 Performance map of (2). FIG. 4 shows RuSe in different proportions under the action of ultrasonic vibrations 2 Composite of/CdS, cdS and 2H RuSe 2 Production of H from CdS 2 Performance map of (2).
FIG. 5 shows RuSe in different proportions under sunlight 2 Composite of/CdS, cdS and 2H RuSe 2 Production of H from CdS 2 Performance graph of (2).
Detailed Description
The present invention is not limited to the following embodiments, and those skilled in the art can implement the present invention in other embodiments according to the disclosure of the present invention, or make simple changes or modifications on the design structure and idea of the present invention, and fall into the protection scope of the present invention. It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict.
Said product H 2 The efficiency is calculated as follows:
r: produce H 2 Rate, unit: mu mol/(g.h)
V: hydrogen volume, unit: mu.L
m: catalyst mass, unit: g is a radical of formula
t: reaction time, unit: h is
Example 1
First, 0.0234g of selenium powder is dispersed in 50mL of C 2 H 6 O 2 In the middle, stirring evenly and ultrasonicallyFor 1h, 583.16. Mu.L of RuCl was added 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 and the pH of the suspension was adjusted 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 washed several times by centrifugation with deionized water. Finally, it was dried overnight in a vacuum oven at 60 ℃. RuSe to be obtained 2 The sample was transferred to a quartz tube at N 2 Annealing at 400 ℃ for 2h under the atmosphere.
Mixing the above RuSe 2 The catalyst and the CdS catalyst in the comparative example 1 were dissolved in distilled water, and subjected to ultrasonic treatment for 1 hour and stirring for 4 hours to mix uniformly. Centrifuging, washing and drying at room temperature to finally obtain dark green powder, namely RuSe 2 A CdS composite catalyst. Addition of RuSe 2 The mass is 1% of the mass of CdS.
Weighing 2mg of the composite catalyst, adding 18mL of deionized water, and carrying out ultrasonic treatment for 30min. Then 2mL of lactic acid is added, and then 30min N is introduced 2 And finally, sealing for 1h under the irradiation of ultrasound and sunlight. After the experiment was completed, the gas in the 0.5mL tube was extracted, the peak area was detected by gas chromatograph, and the H product was calculated 2 Rate, calculated by analysis to yield H 2 The rate was 30858.76. Mu. Mol/(g.h).
Example 2
Compared with example 1, the differences are: the conditions in the application method were changed to ultrasound, and the rest was the same as in example 1.RuSe 2 Production of H from 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 irradiation, and the rest was the same as in example 1.RuSe 2 Production of H from CdS catalyst 2 The rate was 21012.35. Mu. Mol/(g.h).
Example 4
Compared with example 1, the differences are: adding RuSe during the preparation process 2 The mass is 1.5% of the mass of CdS, and the other preparation methods are the same as example 1.
The application method is the same as that of example 1, example4 RuSe prepared 2 Production of H by CdS composite catalyst 2 The rate was 63857.24. Mu. Mol/(g.h), which is 7.54 times that of pure CdS catalyst.
Under the same conditions, ruSe was adjusted 2 The mass is 1.25 percent of the mass of CdS, and the hydrogen production rate is 50358 mu mol/(g.h); regulation of RuSe 2 The mass of the CdS is 1.75 percent of the mass of the 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, and the others were the same as in example 4.RuSe 2 Production of H by CdS composite catalyst 2 The rate was 919.40. Mu. Mol/(g.h).
Example 6
Compared with example 4, the differences are that: the conditions in the application method were changed to the sun illumination, and the rest was the same as in example 4.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: adding RuSe during the preparation process 2 The mass was 2% of the mass of CdS, and the other preparation methods were the same as example 1.
The application method is the same as that of RuSe prepared in example 1 and example 7 2 Production of H 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, and the others were the same as in example 7.RuSe 2 Production of H by CdS composite catalyst 2 The rate was 630.67. Mu. Mol/(g.h).
Example 9
The difference compared to example 7 is that: the conditions in the application method were changed to solar light, and the rest was the same as in example 7.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 differences are: adding RuSe during the preparation process 2 The mass is 3% of the mass of CdS, and the other preparation methods are the same as example 1.
The application method is the same as that of RuSe prepared in example 1 and example 7 2 Production of H 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, and the others were the same as in example 10.RuSe 2 Production of H by CdS composite catalyst 2 The rate was 607.12. Mu. Mol/(g.h).
Example 12
Compared with example 10, the differences are: the conditions in the application method were changed to the sun illumination, and the rest was the same as in example 10.RuSe 2 Production of H by CdS catalyst 2 The rate was 13547.11. Mu. Mol/(g.h).
Comparative example 1
2.312g of CdCl 2 ·2.5H 2 O and 2.312g of thiourea were added to 50mL of ethylenediamine. Transferring the mixed solution into a reaction kettle with a polytetrafluoroethylene lining, carrying out hydrothermal reaction in an oven at the reaction temperature of 160 ℃ for 48 hours, centrifugally collecting the obtained precipitate, and washing the precipitate with distilled water and ethanol for multiple times. And finally, vacuum drying for 12h at 60 ℃ and grinding to obtain CdS yellow powder.
Weighing 2mgCdS catalyst, adding 18mL water, and performing ultrasonic treatment for 30min. Then 2mL of lactic acid was added followed by 30min N 2 And finally, sealing for 1h under the irradiation of ultrasound and sunlight. After the experiment is finished, extracting the gas in a 0.5mL tube, detecting the peak area by using a gas chromatograph, and calculating the H product 2 Rate, calculated by analysis to yield H 2 The rate was 8467.74. Mu. Mol/(g.h).
Comparative example 2
Compared with the comparative example 1, the difference is that: the conditions in the application method were changed to ultrasound, and the others were the same as in comparative example 1. Production of H from CdS catalyst 2 The rate was 11.69. Mu. Mol/(g.h).
Example 3
Compared with the comparative example 1, the difference is that: the conditions in the application method were changed to solar light, and the rest was the same as in comparative example 1. Production of H from CdS catalyst 2 The rate was 269.17. Mu. Mol/(g.h).
Comparative example 4
Preparation method and preparation of composite catalystExample 4 differs from the following: ruse is mixed 2 Calcining the sample for 2 hours in a tube furnace at 600 ℃ in nitrogen atmosphere to obtain black powder pure 2H RuSe 2 And (4) sampling.
The procedure was as in example 4, control 4 and 2H RuSe prepared 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 rest was the same as in comparative example 4.2H RuSe 2 Production of H from 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 were changed to solar light, and the rest was the same as in comparative example 4.2H RuSe 2 Production of H from CdS catalyst 2 The rate was 10235.03. Mu. Mol/(g.h).
Claims (6)
1.RuSe 2 Photoelectric production H of CdS composite catalyst 2 The use of (a), comprising: ruse is mixed 2 Adding the CdS composite catalyst into water, adding lactic acid after full dispersion, and introducing N 2 Finally, carrying out closed reaction under the irradiation of ultrasound and sunlight;
the RuSe being 2 Preparation of a/CdS composite catalyst, including the reaction of RuSe 2 And CdS are dispersed in distilled water, and are subjected to full dispersion reaction, and after the reaction is finished, the mixture is filtered, washed and dried at room temperature to obtain blackish 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 the preparation method comprises mixing selenium powder C 2 H 6 O 2 Suspension with RuCl 3 Mixing the water solution, regulating to neutrality, reacting in microwave chemical reactor, separating out solid, washing, drying, and adding N 2 Annealing at 400-500 deg.c in atmosphere for 2 +/-0.1 hr.
2. The Ruse according to claim 1 2 catalyst/CdS complexChemical-pressure electric production H 2 The application is characterized in that the power of the sun lamp is 55W, and the ultrasonic power is 240W.
3. The Ruse according to claim 1 2 Photoelectric production H of CdS composite catalyst 2 The application is characterized in that the reaction time in the preparation of the composite catalyst is 16-20 h.
4. The Ruse according to claim 1 2 Photoelectric H production by CdS composite catalyst 2 Wherein the CdS preparation comprises adding CdCl 2 ·2.5H 2 Adding O and thiourea into ethylenediamine, fully mixing, carrying out hydrothermal reaction at 160 ℃ for 48 hours, collecting the obtained precipitate after the reaction is finished, washing the precipitate for multiple times by using distilled water and ethanol, and finally drying the precipitate in vacuum.
5. The RuSe of claim 1 2 Photoelectric production H of CdS composite catalyst 2 The use of (A) in a composite catalyst, wherein the composite catalyst comprises RuSe 2 The mass is 1.25% -1.75% of the mass of CdS.
6. The Ruse according to claim 1 2 Photoelectric production H of CdS composite catalyst 2 The use of (A) in (B), wherein RuSe is present 2 The power of the microwave chemical reactor is set to 800 +/-20W and the time is set to 3 +/-1 min in the preparation process.
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| CN116371425A (en) * | 2023-03-30 | 2023-07-04 | 常州大学 | CdS-Vs/Co rich in sulfur vacancies 2 RuS 6 Preparation and application of composite catalyst |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116371425A (en) * | 2023-03-30 | 2023-07-04 | 常州大学 | CdS-Vs/Co rich in sulfur vacancies 2 RuS 6 Preparation and application of composite catalyst |
| CN116371425B (en) * | 2023-03-30 | 2024-01-23 | 常州大学 | CdS-Vs/Co rich in sulfur vacancies 2 RuS 6 Preparation and application of composite catalyst |
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