CN115779951A - Composite photocatalyst C-MoO 2 /C 3 N 4 And preparation method and application thereof - Google Patents
Composite photocatalyst C-MoO 2 /C 3 N 4 And preparation method and application thereof Download PDFInfo
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Abstract
The invention provides a composite photocatalyst C-MoO 2 /C 3 N 4 A preparation method and application thereof, belonging to the technical field of nano material synthesis and photocatalysis; in the invention, a C source is firstly utilized to reduce a molybdenum source and a carbon-doped C-MoO is prepared by hydrothermal reaction 2 Then, C is added 3 N 4 And C-MoO 2 Self-assembling in the self-assembly liquid to obtain the composite photocatalyst C-MoO 2 /C 3 N 4 (ii) a The composite photocatalyst C-MoO 2 /C 3 N 4 Is an S-shaped heterojunction, can enlarge the absorption range of light, enhance the separation of photon-generated carriers, prolong the service life of the carriers, maintain stronger electron reduction capability and hole oxidation capability, and prepare hydrogen in photocatalytic waterThe method has good application in the field.
Description
Technical Field
The present invention belongs to the field of nano material synthesis and lightThe technical field of catalysis, in particular to a composite photocatalyst C-MoO 2 /C 3 N 4 And a preparation method and application thereof.
Background
In recent years, hydrogen has been considered as an ideal, clean, sustainable candidate fuel to replace the exhausted fossil fuels, and the production of hydrogen is mainly: the technology of preparing hydrogen by utilizing semiconductors to convert solar energy into photocatalytic water splitting of hydrogen energy attracts wide attention of people.
A large number of semiconductors are currently found and used for photocatalytic water splitting to produce hydrogen, mainly sulfides, nitrides, oxides, hydroxides, and borides. Metal oxides and nitrides are widely used in these photocatalysts. C 3 N 4 Has good forbidden bandwidth, is a promising semiconductor photocatalyst, however, due to the rapid recombination of photo-generated electrons and holes and the lack of photocatalytic active sites, naked C 3 N 4 Photocatalytic H 2 The activity of the precipitation reaction is extremely low. These problems lead to C 3 N 4 The yield of hydrogen prepared by photocatalytic water splitting alone is not high, and the application of the hydrogen in practice is limited.
Molybdenum dioxide (MoO) 2 ) Has high conductivity and chemical stability similar to noble metal, making it a promising substitute for electron transfer, but due to MoO 2 The carrier recombination of the carrier per se is faster, so that the pure MoO 2 The performance as a photocatalyst is not high. Thus MoO 2 The MoO can be improved by compounding with another semiconductor to improve the carrier separation efficiency 2 The photocatalytic performance of (a). Existing MoO 2 Although recombination with other semiconductors can improve carrier separation efficiency, it still has the problem of reduced redox potential, which limits MoO 2 Application of the composite catalyst. Therefore, it is desirable to provide a method capable of improving the separation efficiency of carriers while increasing the oxidation-reduction potential.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a composite photocatalyst C-MoO 2 /C 3 N 4 And a preparation method and application thereof. In the invention, a C source is firstly utilized to reduce a molybdenum source and a carbon-doped C-MoO is prepared by hydrothermal reaction 2 Then, C is added 3 N 4 And C-MoO 2 Self-assembling in self-assembly liquid to obtain the composite photocatalyst C-MoO 2 /C 3 N 4 (ii) a The composite photocatalyst C-MoO 2 /C 3 N 4 The photo-induced heterojunction is an S-shaped heterojunction, can expand the light absorption range, enhance the separation of photo-generated carriers, prolong the service life of the carriers, keep stronger electron reduction capability and hole oxidation capability, and has good application in the field of photocatalytic water hydrogen production.
The invention firstly provides a composite photocatalyst C-MoO 2 /C 3 N 4 The composite photocatalyst C-MoO 2 /C 3 N 4 In which C is doped into MoO 2 To obtain C-MoO 2 Granulating, then mixing C-MoO 2 Self-assembly loading of particles in C 3 N 4 On the chip.
The invention also provides the composite photocatalyst C-MoO 2 /C 3 N 4 The method of preparing, comprising:
dissolving a carbon source and a molybdenum source in water, uniformly mixing, then carrying out hydrothermal reaction, cooling, centrifuging, washing and drying after the reaction is finished to obtain C-MoO 2 ；
Subjecting the C-MoO 2 Dispersing in n-hexane, and adding C 3 N 4 Performing ultrasonic treatment until the mixture is completely dispersed to obtain a mixed solution, and stirring the mixed solution to C-MoO 2 Fully self-assembled to C 3 N 4 And centrifuging and drying after stirring to obtain the composite photocatalyst C-MoO 2 /C 3 N 4 。
Further, the carbon source comprises starch, glucose or dicyandiamide, the molybdenum source comprises ammonium molybdate or sodium molybdate, and the dosage ratio of the carbon source to the molybdenum source is 1.4:10
Further, the hydrothermal reaction is carried out for 6h at 180 ℃.
Further, the C-MoO 2 And C 3 N 4 The mass ratio of (1-11): 100, said C-MoO 2 And the dosage ratio of the n-hexane is 1-11 g:20-50mL.
Further, said C 3 N 4 The preparation method comprises the following steps: calcining urea at 500-600 deg.C, cooling to obtain C 3 N 4 。
Further, the calcination is carried out by heating to 500-600 ℃ at a heating rate of 2-5 ℃/min and then calcining for 2-4h.
Further, the stirring time is 5-12h.
The invention also provides the composite photocatalyst C-MoO 2 /C 3 N 4 The application in photocatalytic hydrogen production from water.
Compared with the prior art, the invention has the beneficial effects that:
C-MoO prepared in the invention 2 /C 3 N 4 The light absorption range is expanded, the separation of photon-generated carriers is enhanced, the service life of the carriers is prolonged, and the strong electron reduction capability and the hole oxidation capability are maintained. The experimental result shows that the composite photocatalyst C-MoO 2 /C 3 N 4 The hydrogen evolution rate of (C) is pure C 3 N 4 About 1.8 times of the total weight of the product.
In the invention, C is used for doping MoO 2 To improve MoO 2 The carrier separation, and then the photocatalytic performance of the composite catalyst is improved. In the invention C 3 N 4 Is in the form of a sheet having a large surface area, C-MoO 2 Can better load at C 3 N 4 The above. Monolithic C-MoO 2 /C 3 N 4 The resistance of electron transmission is reduced, and therefore better photocatalytic performance is achieved. In addition, compared with the existing heterojunction, the S-type heterojunction has better carrier separation effect due to the existence of a built-in electric field, and has higher oxidation-reduction potential so that the reaction is easier to carry out.
The invention adopts a simple self-assembly methodTo C-MoO 2 /C 3 N 4 The S-type heterojunction composite photocatalyst is low in cost, economical and environment-friendly.
Drawings
FIG. 1 shows a composite photocatalyst C-MoO of the present invention 2 /C 3 N 4 The synthesis process diagram of (1).
FIG. 2 shows a composite photocatalyst C-MoO according to the present invention 2 /C 3 N 4 TEM image of (a).
FIG. 3 shows a composite photocatalyst C-MoO according to the present invention 2 /C 3 N 4 And a performance diagram of the photocatalytic hydrogen production of the comparative material; FIG. a is at C 3 N 4 Loaded with C-MoO of different masses 2 A performance map of (a); panel b is a graph of the cycling performance of the best performing samples in panel a.
FIG. 4 shows a composite photocatalyst C-MoO according to the present invention 2 /C 3 N 4 And XPS plot of comparative material with CMC of C-MoO 2 /C 3 N 4 For short.
FIG. 5 shows a composite photocatalyst C-MoO according to the present invention 2 /C 3 N 4 Schematic of the charge separation and transfer mechanism of (1).
Detailed Description
The present invention is further described with reference to the drawings and the specific embodiments, but the scope of the present invention is not limited to the following specific embodiments, and those skilled in the art can implement the present invention in other specific embodiments or make simple changes or modifications within the scope of the present invention based on the disclosure of the present invention. It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict.
Example 1:
FIG. 1 shows a composite photocatalyst C-MoO 2 /C 3 N 4 A synthetic scheme of (a); the composite photocatalyst C-MoO is intuitively reflected in the figure 2 /C 3 N 4 The synthesis process of (1) firstly synthesizing C-MoO respectively 2 And C 3 N 4 Monomer, then byThe assembly method obtains the composite sample C-MoO 2 /C 3 N 4 . The specific preparation process is as follows:
(1)C-MoO 2 the preparation of (1):
140mg of glucose was dissolved in water with stirring, and then 1g of ammonium molybdate was added thereto with stirring until completely dissolved. Putting the mixed solution into a polytetrafluoroethylene reaction kettle at 180 ℃ for 6 hours, cooling, centrifuging, washing, drying in vacuum after the reaction is finished, and finally collecting to obtain C-MoO 2 And (4) sampling.
(2)C 3 N 4 The preparation of (1):
placing 5g of urea in a magnetic boat under N 2 Furnace at 550 deg.C, 2.5 deg.C/min, 4h, and cooling to obtain C 3 N 4 And (3) sampling.
(3)C-MoO 2 /C 3 N 4 The preparation of (1):
3mg of C-MoO 2 Completely dispersed in 20ml of n-hexane, and then 100mg of C was added 3 N 4 Ultrasonic treatment is carried out until the mixture is completely dispersed, and then stirring is carried out for 12 hours until the mixture is C-MoO 2 Fully self-assembled reverse C 3 N 4 The above. Centrifuging and vacuum drying to obtain the composite sample C-MoO 2 /C 3 N 4 。
FIG. 4 shows a composite photocatalyst C-MoO 2 /C 3 N 4 Pure sample C 3 N 4 And C-MoO 2 The XPS diagram shows that the material is successfully prepared. Furthermore, as can be seen from the figure, the shift of the peak in the figure can be used to derive C in the absence of illumination 3 N 4 Will be transferred to C-MoO 2 A built-in electric field is formed thereon in the direction of C 3 N 4 Point of C-MoO 2 . When the light is on, C-MoO 2 And C 3 N 4 Photo-generated carriers are generated, and electrons are generated from C-MoO due to the existence of a built-in electric field 2 Flow direction of conduction band C 3 N 4 Valence band of (1), and C 3 N 4 Holes in the valence band recombine to form this S-shaped transfer path.
Example 2:
(1)C-MoO 2 the preparation of (1):
140mg of glucose was dissolved in water with stirring, and then 1g of ammonium molybdate was added thereto with stirring until completely dissolved. Putting the mixed solution into a polytetrafluoroethylene reaction kettle at 180 ℃ for 6h, cooling, centrifuging, washing, drying in vacuum after the reaction is finished, and finally collecting to obtain C-MoO 2 And (3) sampling.
(2)C 3 N 4 The preparation of (1):
putting 5g urea into a magnetic boat, heating in an N2 furnace at 550 deg.C for 4h at 2.5 deg.C/min, and cooling to obtain C 3 N 4 And (3) sampling.
(3)C-MoO 2 /C 3 N 4 The preparation of (1):
5mg of C-MoO 2 Completely dispersed in 20ml of n-hexane, then 100mg of C were added 3 N 4 Performing ultrasonic treatment until the mixture is completely dispersed, and then stirring for 12 hours until the mixture is C-MoO 2 Fully self-assembled reverse C 3 N 4 The above. Centrifuging and vacuum drying to obtain the composite sample C-MoO 2 /C 3 N 4 。
Example 3:
(1)C-MoO 2 the preparation of (1):
140mg of glucose was dissolved in water with stirring, and then 1g of ammonium molybdate was added thereto with stirring until completely dissolved. Putting the mixed solution into a polytetrafluoroethylene reaction kettle at 180 ℃ for 6h, cooling, centrifuging, washing, drying in vacuum after the reaction is finished, and finally collecting to obtain C-MoO 2 And (4) sampling.
(2)C 3 N 4 The preparation of (1):
putting 5g urea into a magnetic boat, heating in an N2 furnace at 550 deg.C for 4h at 2.5 deg.C/min, and cooling to obtain C 3 N 4 And (4) sampling.
(3)C-MoO 2 /C 3 N 4 The preparation of (1):
7mg of C-MoO 2 Completely dispersed in 20ml of n-hexane, then 100mg of C were added 3 N 4 Performing ultrasonic treatment until the mixture is completely dispersed, and then stirring for 12 hours until the mixture is C-MoO 2 Fully self-assembled reverse C 3 N 4 The above. Centrifuging and vacuum drying to obtain a composite sample C-MoO 2 /C 3 N 4 。
Example 4:
(1)C-MoO 2 the preparation of (1):
140mg of glucose was dissolved in water with stirring, and then 1g of ammonium molybdate was added and stirred until completely dissolved. Putting the mixed solution into a polytetrafluoroethylene reaction kettle at 180 ℃ for 6h, cooling, centrifuging, washing, drying in vacuum after the reaction is finished, and finally collecting to obtain C-MoO 2 And (3) sampling.
(2)C 3 N 4 The preparation of (1):
putting 5g urea into a magnetic boat, heating in an N2 furnace at 550 deg.C for 4h at 2.5 deg.C/min, and cooling to obtain C 3 N 4 And (4) sampling.
(3)C-MoO 2 /C 3 N 4 The preparation of (1):
9mg of C-MoO 2 Completely dispersed in 20ml of n-hexane, then 100mg of C were added 3 N 4 Ultrasonic treatment is carried out until the mixture is completely dispersed, and then stirring is carried out for 12 hours until the mixture is C-MoO 2 Fully self-assembled reverse C 3 N 4 The above. Centrifuging and vacuum drying to obtain the composite sample C-MoO 2 /C 3 N 4 。
Example 5:
(1)C-MoO 2 the preparation of (1):
140mg of glucose was dissolved in water with stirring, and then 1g of ammonium molybdate was added thereto with stirring until completely dissolved. Putting the mixed solution into a polytetrafluoroethylene reaction kettle at 180 ℃ for 6h, cooling, centrifuging, washing, drying in vacuum after the reaction is finished, and finally collecting to obtain C-MoO 2 And (3) sampling.
(2)C 3 N 4 The preparation of (1):
putting 5g urea into a magnetic boat, heating in an N2 furnace at 550 ℃, 2.5 ℃/min and 4h, and finally cooling to obtain C 3 N 4 And (4) sampling.
(3)C-MoO 2 /C 3 N 4 The preparation of (1):
11mg of C-MoO 2 Completely dispersed in 20ml of n-hexane, and then 100mg of C was added 3 N 4 Ultrasonic treatment is carried out until the mixture is completely dispersed, and then stirring is carried out for 12 hours until the mixture is C-MoO 2 Fully self-assembled reverse C 3 N 4 The above. Centrifuging and vacuum drying to obtain a composite sample C-MoO 2 /C 3 N 4 。
Example 6:
(1)MoO 2 the preparation of (1):
144mg of MoO 3 48mg of molybdenum powder. Adding into 40ml water, stirring for 2h to disperse. Putting the mixed solution into a polytetrafluoroethylene reaction kettle at 200 ℃ for 15h, cooling, centrifuging, washing, drying in vacuum after the reaction is finished, and finally collecting to obtain MoO 2 And (3) sampling.
(2)C 3 N 4 The preparation of (1):
5g of urea is put into a magnetic boat and placed in N 2 Furnace at 550 deg.C, 2.5 deg.C/min, 4h, and cooling to obtain C 3 N 4 And (4) sampling.
(3)C-MoO 2 /C 3 N 4 The preparation of (1):
7mg of MoO 2 Completely dispersed in 20ml of n-hexane, and then 100mg of C was added 3 N 4 Ultrasonically treating until the mixture is completely dispersed, and then stirring for 12 hours until MoO 2 Fully self-assembled reverse C 3 N 4 The above. Centrifuging and vacuum drying to obtain a composite sample MoO 2 /C 3 N 4 。
The conditions for preparing hydrogen by photocatalytic water cracking are as follows: the light source equipment used is a 300W xenon lamp, the reaction vessel is a 100mL flat-bottom three-neck flask, and the sacrificial agent is triethanolamine aqueous solution with the volume ratio of 10%. 10mg of sample to be detected, 80mL of corresponding type sacrificial agent and 3% of Pt as a catalyst group are ultrasonically stirred for 20min until the sample is uniformly dispersed in the aqueous solution. And then, communicating the reactor with nitrogen for 10-20 min, removing redundant air in the reactor, and introducing the nitrogen for 30-40 min when a circulation stability test is carried out. The yield of hydrogen per unit time at which the reaction of the sample occurred was measured by means of a gas chromatograph model Japan Shimadzu gas chromatograph model GC-8A with a TCD detector, and the measurement results are shown in FIG. 2.
C-MoO can be seen in FIG. 2 2 Is a particle of about 50nm, C 3 N 4 Is of a sheet structure, a composite sample C-MoO 2 /C 3 N 4 Has a structure of C-MoO 2 Loaded at C 3 N 4 On the surface, such a structure improvesThe transfer of carriers inside the material increases the active sites for the reaction.
FIG. 3 is a C-MoO of the present invention 2 /C 3 N 4 Performance diagrams of photocatalytic hydrogen production of composite and comparative materials; FIG. a is at C 3 N 4 Loaded with C-MoO of different masses 2 A performance map of (a); panel b is a graph of the cycling performance of the best performing samples in panel a. As can be seen, panel c is pure MoO 2 And C doped MoO 2 Load to C 3 N 4 The hydrogen production performance is shown in the figure, and the doping C can effectively improve MoO 2 The separation of the photon-generated carriers, and further the photocatalytic hydrogen production performance is improved.
FIG. 5 shows the catalytic mechanism of the composite photocatalyst in the preparation of hydrogen by photocatalytic water splitting, C-MoO 2 And C 3 N 4 Photo-generated electrons can be generated after the absorption of photons, and C-MoO is generated due to the existence of a built-in electric field 2 Electron in conduction band would and C 3 N 4 Hole recombination in the valence band enhances separation of photogenerated carriers, C 3 N 4 Electrons on the conduction band will be captured by Pt and H will be + Reduction to H 2 (ii) a And C-MoO 2 The holes in the valence band are consumed by triethanolamine, forming an electron transfer path like S.
The present invention is not limited to the above-described embodiments, and any obvious improvements, substitutions or modifications can be made by those skilled in the art without departing from the spirit of the present invention.
Claims (9)
1. Composite photocatalyst C-MoO 2 /C 3 N 4 The method for producing (a), characterized by comprising:
dissolving a carbon source and a molybdenum source in water, uniformly mixing, then carrying out hydrothermal reaction, cooling, centrifuging, washing and drying after the reaction is finished to obtain C-MoO 2 ；
Subjecting the C-MoO to 2 Dispersing in n-hexane, and adding C 3 N 4 Ultrasonic wave is carried out toDispersing completely to obtain mixed solution, stirring the mixed solution to C-MoO 2 Fully self-assembled to C 3 N 4 And centrifuging and drying after stirring to obtain the composite photocatalyst C-MoO 2 /C 3 N 4 。
2. The composite photocatalyst, C-MoO, of claim 1 2 /C 3 N 4 The method for preparing (1), wherein the carbon source comprises starch, glucose or dicyandiamide, and the molybdenum source comprises ammonium molybdate or sodium molybdate; the molar ratio of the carbon element to the molybdenum element is 1.4:10.
3. the composite photocatalyst, C-MoO, of claim 1 2 /C 3 N 4 The preparation method is characterized in that the hydrothermal reaction is carried out for 6 hours at 180 ℃.
4. The composite photocatalyst C-MoO as claimed in claim 1 2 /C 3 N 4 Characterized in that the C-MoO 2 And C 3 N 4 The mass ratio of (1-11): 100, said C-MoO 2 And the dosage ratio of the n-hexane is 1-11 g:20-50mL.
5. The composite photocatalyst C-MoO as claimed in claim 1 2 /C 3 N 4 Characterized in that, C is 3 N 4 The preparation method comprises the following steps: calcining urea at 500-600 deg.C, cooling to obtain C 3 N 4 。
6. The composite photocatalyst, C-MoO, of claim 5 2 /C 3 N 4 The preparation method is characterized in that the calcination is carried out for 2-4h after the temperature is raised to 500-600 ℃ at the temperature raising speed of 2-5 ℃/min.
7. The composite photocatalyst, C-MoO, of claim 1 2 /C 3 N 4 The preparation method is characterized in that the stirring time is 5-12h.
8. Composite photocatalyst C-MoO prepared by the method of any one of claims 1 to 7 2 /C 3 N 4 The composite photocatalyst C-MoO 2 /C 3 N 4 In which C is doped into MoO 2 To obtain C-MoO 2 Granules, then mixing C-MoO 2 Self-assembly loading of particles in C 3 N 4 On the chip.
9. The composite photocatalyst, C-MoO, of claim 8 2 /C 3 N 4 The application in photocatalytic hydrogen production from water.
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