CN113578296B - Lamellar gray TiO2 photocatalytic material and preparation method thereof - Google Patents
Lamellar gray TiO2 photocatalytic material and preparation method thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 64
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title description 4
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
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Abstract
The invention provides lamellar gray TiO 2 Photocatalytic material and preparation method thereof, relates to the technical field of photocatalytic material, and the lamellar gray TiO 2 The preparation method of the photocatalytic material comprises the following steps: to contain Ti 3 AlC 2 Dropwise adding HF solution into a powder container, sequentially magnetically stirring, centrifugally washing until the pH value of the mixed solution is more than 6, and drying to obtain Ti 3 C 2 A powder; to said Ti 3 C 2 ZnCl is added into the powder 2 Uniformly mixing the powder, calcining to obtain prefabricated powder, washing and drying the prefabricated powder to obtain lamellar gray TiO 2 Photocatalytic material. Compared with the prior art, the invention provides lamellar gray TiO 2 The photocatalytic material and the preparation method thereof improve the utilization rate of sunlight and the photocatalytic hydrogen production performance.
Description
Technical Field
The invention relates to the technical field of photocatalytic materials, in particular to lamellar gray TiO 2 Photocatalytic material and method of making the same.
Background
With the gradual decrease of fossil fuels, the development and utilization of new energy are eager. Photocatalytic hydrogen production is an important component for converting solar energy into chemical energy and is an effective strategy for efficiently utilizing solar energy. TiO (titanium dioxide) 2 The photocatalyst has the characteristics of low cost, high chemical stability, repeated use, no secondary pollution, no toxicity and the like, and becomes a research hot spot of photocatalytic materials in recent years. But TiO 2 The forbidden bandwidth of (2.3 eV) is larger, and only about 5% of ultraviolet light in the solar spectrum can be absorbed, so that the utilization rate of sunlight is greatly limited. In addition, the higher photo-generated electron-hole recombination rate also leads to TiO 2 Is low. Therefore, there are limitations in the application of photocatalytic hydrogen production.
Disclosure of Invention
The invention solves the problems of the prior TiO 2 The utilization rate of sunlight and the photocatalytic hydrogen production performance of the photocatalytic material are low.
To solve the problems, the invention provides a lamellar gray TiO 2 The preparation method of the photocatalytic material comprises the following steps:
step S1, filling Ti into the steel 3 AlC 2 Dropwise adding HF solution into a powder container, sequentially magnetically stirring, centrifugally washing until the pH value of the mixed solution is more than 6, and drying to obtain Ti 3 C 2 A powder;
step S2, to the Ti 3 C 2 ZnCl is added into the powder 2 Mixing the powder uniformly, calcining to obtain prefabricated powder, and pre-preparing the powderWashing and drying the prepared powder to obtain lamellar gray TiO 2 Photocatalytic material.
Preferably, in step S1, the magnetic stirring includes: magnetically stirring at 30-60 deg.c for 48-72 hr.
Preferably, in step S1, the centrifugal washing includes: centrifugal washing is carried out in a centrifugal machine by deionized water, the rotating speed of the centrifugal machine is 4000r/min-5000r/min, and the washing times are 10-20 times.
Preferably, in step S1 and/or step S2, the drying includes: drying at 60-80deg.C for 12-24 hr.
Preferably, the ZnCl 2 The mass of the powder is Ti 3 C 2 5-6 times of the powder mass.
Preferably, the calcination treatment includes: calcination is carried out in a muffle furnace at a temperature of 350-450 ℃.
Preferably, the calcination treatment further includes: heating from room temperature at 3-6deg.C/min for 3-5h.
Preferably, in step S2, the mixing manner includes: subjecting the Ti to 3 C 2 Powder and ZnCl 2 The powder was put into a mortar and ground for 1h.
Preferably, in step S2, the washing includes repeatedly performing centrifugal washing on the fully ground prefabricated powder with deionized water and absolute ethyl alcohol in a centrifuge, where the rotational speed of the centrifuge is 4000r/min-5000r/min, and the washing times are 5-10 times.
The lamellar gray TiO provided by the invention 2 Compared with the prior art, the preparation method of the photocatalytic material has the advantages that the method utilizes the HF etching method to prepare the Ti 3 C 2 Lamellar structure and using ZnCl 2 Calcination of Ti by molten salt method 3 C 2 Preparation of lamellar Gray TiO 2 Photocatalytic material, wherein ZnCl 2 Forming molten state at high temperature, inserting multiple layers of Ti 3 C 2 In the sheet layer, ti is added 3 C 2 Is such that Ti during calcination 3 C 2 The lamellar structure is preserved so as to obtainLamellar gray TiO of (C) 2 The photocatalytic material has high specific surface area, provides a large number of active sites for photocatalytic reaction, and is favorable for TiO 2 The separation of photo-generated electrons and holes, the photocatalysis performance is improved, and the gray TiO 2 The photocatalytic material is favorable for widening the light absorption range and improving the utilization rate of sunlight, and the lamellar gray TiO prepared by the invention 2 The photocatalytic material has higher photocatalytic hydrogen production performance.
The invention also provides lamellar gray TiO 2 Photocatalytic material according to lamellar gray TiO as described above 2 The preparation method of the photocatalytic material is used for preparation.
The lamellar gray TiO provided by the invention 2 Photocatalytic material and the lamellar gray TiO 2 The preparation method of the photocatalytic material has the same advantages as compared with the prior art, and is not described in detail herein.
Drawings
FIG. 1 shows lamellar gray TiO in an embodiment of the invention 2 A flow chart of a preparation method of the photocatalytic material;
FIG. 2 shows Ti as an example of the invention 3 AlC 2 、Ti 3 C 2 And calcining at 350deg.C and 400deg.C to obtain lamellar gray TiO 2 XRD pattern of the photocatalytic material;
FIG. 3 shows lamellar gray TiO in an embodiment of the invention 2 Photoluminescence spectrum of the photocatalytic material;
FIG. 4 shows lamellar gray TiO in an embodiment of the invention 2 SEM images of photocatalytic material;
FIG. 5 shows lamellar gray TiO in an embodiment of the invention 2 EDS diagram of photocatalytic material;
FIG. 6 shows lamellar gray TiO in an embodiment of the invention 2 Photo-catalytic hydrogen production pattern of photo-catalytic material.
Detailed Description
In order that the above objects, features and advantages of the invention will be readily understood, a more particular description of the invention will be rendered by reference to specific embodiments thereof which are illustrated in the appended drawings.
It should be noted that in the description of embodiments of the present application, the term "some embodiments" of the description means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same implementations or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
As shown in FIG. 1, an embodiment of the present invention provides a lamellar gray TiO 2 The preparation method of the photocatalytic material comprises the following steps:
step S1, filling Ti into the steel 3 AlC 2 Dropwise adding HF solution into a powder container, sequentially magnetically stirring, centrifugally washing until the pH value of the mixed solution is more than 6, and drying to obtain Ti 3 C 2 A powder;
step S2, to the Ti 3 C 2 ZnCl is added into the powder 2 Uniformly mixing the powder, calcining to obtain prefabricated powder, washing and drying the prefabricated powder to obtain lamellar gray TiO 2 Photocatalytic material.
In the present embodiment Ti 3 C 2 Is a member of MXene two-dimensional materials, has unique lamellar structure, excellent conductivity, chemical stability and rich active catalytic sites, and ensures that Ti 3 C 2 The application in the field of photocatalysis is more extensive. For example, ti 3 C 2 Has high specific surface area, can provide enough active sites for photocatalysis reaction, ti 3 C 2 Has hydrophilicity, is favorable for adsorbing a large amount of water molecules on the surface, provides convenience for producing hydrogen by photocatalysis, and Ti 3 C 2 The excellent conductivity facilitates electron transfer. But Ti is 3 C 2 The energy band structure of the catalyst does not meet the hydrogen production requirement, so that the catalyst does not have hydrogen production performance, but under the calcination condition, ti 3 C 2 The surface can oxidize to generate TiO 2 Particles, however, the original lamellar structure is difficult to maintain, and the actual light is limitedApplication in the catalytic field. Thus, ti was calcined by molten salt method in this example 3 C 2 ZnCl is introduced in the process of (2) 2 Lamellar gray TiO was prepared 2 Photocatalytic material, wherein ZnCl 2 Forming molten state at high temperature, inserting multiple layers of Ti 3 C 2 In the sheet layer, ti is added 3 C 2 Is such that Ti during calcination 3 C 2 The lamellar structure is preserved so that the prepared lamellar gray TiO 2 The photocatalytic material has high specific surface area, provides a large number of active sites for photocatalytic reaction, and is favorable for TiO 2 The separation of photo-generated electrons and holes, the photocatalysis performance is improved, and the gray TiO 2 The photocatalytic material is favorable for widening the light absorption range and improving the utilization rate of sunlight, and the lamellar gray TiO prepared by the invention 2 The photocatalytic material has higher photocatalytic hydrogen production performance.
On the other hand, the calcination method is a commonly used method, has simple process, low cost, large yield and high safety coefficient, and is carried out in air and can be Ti 3 C 2 Providing continuous oxygen, ti 3 C 2 The surface can grow TiO in situ in a short time 2 Can be fully oxidized within a certain time to obtain a catalyst containing a large amount of TiO 2 Wrapping a small amount of Ti 3 C 2 And the calcining temperature and the heating speed are conveniently controlled. On the other hand, ti prepared by HF etching in this example 3 C 2 The surface of the lamellar structure can be provided with a large number of F functional groups (-F), the surface functional groups influencing the performance can be removed by calcining, the defect concentration of the crystal surface is effectively reduced, the recombination center of photo-generated electron holes is reduced, and the photocatalytic hydrogen production performance is improved.
In some embodiments, in step S1, the magnetic stirring comprises: magnetically stirring at 30-60 deg.c for 48-72 hr. Thereby making Ti 3 AlC 2 The powder is fully dissolved in HF solution, and the dissolution effect is good.
In some embodiments, in step S1, the centrifugal washing comprises: centrifugal washing is carried out in a centrifugal machine by deionized water, the rotating speed of the centrifugal machine is 4000r/min-5000r/min, and the washing times are 10-20 times. Thus, the washing effect is good.
In some embodiments, in step S1 and/or step S2, the drying comprises: drying at 60-80deg.C for 12-24 hr. Thereby making the prepared Ti 3 C 2 The powder has high purity.
In this example, znCl 2 The powder forms a molten state at high temperature and is inserted between the lamellar layers, thereby avoiding lamellar Ti 3 C 2 But ZnCl is deposited on 2 Excessive amounts are detrimental to Ti 3 C 2 With oxygen, thus, in some embodiments, the ZnCl 2 The mass of the powder is Ti 3 C 2 5-6 times of the powder mass. Not only avoid lamellar Ti 3 C 2 Is beneficial to the accumulation of Ti 3 C 2 Contact with oxygen.
In the present embodiment, due to Ti 3 C 2 Has stability below 200deg.C, no oxidation reaction, ti 3 C 2 Only partial oxidation occurs at 300 ℃, calcination is carried out at a temperature higher than 300 ℃ and is favorable for oxidation reaction, but the temperature is too high and can be oxidized into CO 2 Resulting in Ti 3 C 2 Is not present. Thus, in some embodiments, the calcination treatment comprises: calcination is carried out in a muffle furnace at a temperature of 350-450 ℃. Not only is favorable for the generation of oxidation reaction, but also can ensure Ti 3 C 2 Is a two-dimensional structure of (a).
In some embodiments, the calcination process further comprises: heating from room temperature at 3-6deg.C/min for 3-5h. Thereby making Ti 3 C 2 Can be fully oxidized to obtain a two-dimensional layered structure with a carbon layer as a framework support, and a large amount of TiO with higher crystallinity is generated on the surface of the carbon layer 2 And (3) particles.
In some embodiments, the manner of mixing in step S2 includes: subjecting the Ti to 3 C 2 Powder and ZnCl 2 Placing the powder into a mortar, grinding 1And h, uniformly mixing and facilitating subsequent calcination.
In some embodiments, in step S2, the washing includes repeatedly performing centrifugal washing on the fully ground pre-manufactured powder with deionized water and absolute ethanol in a centrifuge at a rotational speed of 4000r/min to 5000r/min for 5-10 times. Thus, the washing effect is good.
Therefore, the embodiment of the invention provides lamellar gray TiO 2 Compared with the prior art, the preparation method of the photocatalytic material has the advantages that the method utilizes the HF etching method to prepare the Ti 3 C 2 Lamellar structure and using ZnCl 2 Calcination of Ti by molten salt method 3 C 2 Preparation of lamellar Gray TiO 2 Photocatalytic material, wherein ZnCl 2 Forming molten state at high temperature, inserting multiple layers of Ti 3 C 2 In the sheet layer, ti is added 3 C 2 Is such that Ti during calcination 3 C 2 The lamellar structure is preserved so that the prepared lamellar gray TiO 2 The photocatalytic material has high specific surface area, provides a large number of active sites for photocatalytic reaction, and is favorable for TiO 2 The separation of photo-generated electrons and holes, the photocatalysis performance is improved, and the gray TiO 2 The photocatalytic material is favorable for widening the light absorption range and improving the utilization rate of sunlight, and the lamellar gray TiO prepared by the invention 2 The photocatalytic material has higher photocatalytic hydrogen production performance.
The embodiment of the invention also provides lamellar gray TiO 2 Photocatalytic material according to lamellar gray TiO as described above 2 The preparation method of the photocatalytic material is used for preparation.
The lamellar gray TiO provided by the invention 2 Photocatalytic material and the lamellar gray TiO 2 The preparation method of the photocatalytic material has the same advantages as compared with the prior art, and is not described in detail herein.
Example 1
As shown in fig. 2-6, the present embodiment provides a lamellar gray TiO 2 The preparation method of the photocatalytic material comprises the following steps ofThe steps are as follows:
In this example, the laminar gray TiO prepared in this example was used in a photocatalytic hydrogen production system 2 The photocatalytic material is used for carrying out a hydrogen production experiment, and specifically comprises the following steps: 10mg of lamellar gray TiO prepared in this example 2 The photocatalytic material was suspended in an aqueous solution of triethanolamine (50 mL,20 vol%) with the addition of 3% H 2 PtCl 6 And (3) irradiating the aqueous solution for 30min under a xenon lamp with the power of 300W to enable platinum to be deposited on the surface of the catalyst, collecting data every 1h, and enabling the hydrogen production rate to be up to 9.2mmoL/h/g at 4h and 2.3 mmoL/h/g at most. It can be seen that the lamellar gray TiO prepared by the invention 2 The photocatalytic material has higher hydrogen production performance.
Example 2
As shown in fig. 2, 3, 4 and 6, the present embodiment provides a lamellar gray TiO 2 The preparation method of the photocatalytic material comprises the following steps:
Example 3
The present example provides a lamellar gray TiO 2 The preparation method of the photocatalytic material comprises the following steps:
Although the present disclosure is described above, the scope of protection of the present disclosure is not limited thereto. Various changes and modifications may be made by one skilled in the art without departing from the spirit and scope of the disclosure, and these changes and modifications will fall within the scope of the invention.
Claims (7)
1. Lamellar gray TiO 2 The preparation method of the photocatalytic material is characterized by comprising the following steps:
step S1, filling Ti into the steel 3 AlC 2 Dropwise adding HF solution into a powder container, sequentially magnetically stirring, centrifugally washing until the pH value of the mixed solution is more than 6, and drying to obtain Ti 3 C 2 A powder;
step S2, to the Ti 3 C 2 ZnCl is added into the powder 2 Uniformly mixing the powder, calcining to obtain prefabricated powder, washing and drying the prefabricated powder to obtain lamellar gray TiO 2 A photocatalytic material;
the ZnCl 2 The mass of the powder is Ti 3 C 2 5-6 times of the powder;
the calcination treatment includes: calcining in a muffle furnace at 350-450 ℃;
the calcination treatment further includes: heating from room temperature at 3-6deg.C/min for 3-5h.
2. Lamellar gray TiO according to claim 1 2 The preparation method of the photocatalytic material is characterized in that in step S1, the magnetic stirring includes: magnetically stirring 48-72h at 30-60 deg.C.
3. Lamellar gray TiO according to claim 1 2 A method for preparing a photocatalytic material, wherein in step S1, the centrifugal washing includes: centrifugal washing is carried out in a centrifugal machine by deionized water, the rotating speed of the centrifugal machine is 4000r/min-5000r/min, and the washing times are 10-20 times.
4. Lamellar gray TiO according to claim 1 2 A method for preparing a photocatalytic material, wherein in step S1 and/or step S2, the drying includes: drying 12-24. 24h at 60-80deg.C.
5. Lamellar gray TiO according to claim 1 2 The preparation method of the photocatalytic material is characterized in that in step S2, the mixing mode includes: subjecting the Ti to 3 C 2 Powder and ZnCl 2 The powder was put into a mortar and ground for 1h.
6. Lamellar gray TiO according to claim 1 2 The preparation method of the photocatalytic material is characterized in that in the step S2, the prefabricated powder is washed after being ground, the washing comprises the steps of repeatedly performing centrifugal washing on the prefabricated powder after being fully ground in a centrifugal machine by deionized water and absolute ethyl alcohol, wherein the rotating speed of the centrifugal machine is 4000r/min-5000r/min, and the washing times are 5-10 times.
7. Lamellar gray TiO 2 Photocatalytic material, characterized in that it is a lamellar gray TiO according to any one of claims 1-6 2 The preparation method of the photocatalytic material is used for preparation.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110930016.2A CN113578296B (en) | 2021-08-13 | 2021-08-13 | Lamellar gray TiO2 photocatalytic material and preparation method thereof |
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