CN112191263B - TiO 2 2 Photo catalysisChemical composite material and preparation method and application thereof - Google Patents

TiO 2 2 Photo catalysisChemical composite material and preparation method and application thereof Download PDF

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CN112191263B
CN112191263B CN202011157436.3A CN202011157436A CN112191263B CN 112191263 B CN112191263 B CN 112191263B CN 202011157436 A CN202011157436 A CN 202011157436A CN 112191263 B CN112191263 B CN 112191263B
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tio
composite material
photocatalytic composite
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CN112191263A (en
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许成群
刘晓露
杨嘉乐
陈泽源
顾凤龙
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Wuyi University
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    • B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/24—Nitrogen compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • 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
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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
    • B01J37/0027—Powdering
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    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/08—Heat treatment
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    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
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    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
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    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/30—Treatment of water, waste water, or sewage by irradiation
    • C02F1/32—Treatment of water, waste water, or sewage by irradiation with ultraviolet light
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    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
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    • C09K11/0883—Arsenides; Nitrides; Phosphides
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    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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    • C02F2101/308—Dyes; Colorants; Fluorescent agents
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    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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    • C02F2101/38—Organic compounds containing nitrogen
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2305/00—Use of specific compounds during water treatment
    • C02F2305/10—Photocatalysts
    • 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
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    • Y02W10/30—Wastewater or sewage treatment systems using renewable energies
    • Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy

Abstract

The invention relates to a TiO 2 Photocatalytic composite material, the surface of which comprises TiO 2 Nanosheet and supported on TiO 2 g-C on nanosheets 3 N 4 And (4) quantum dots. The TiO is 2 The preparation method of the photocatalytic composite material comprises the following steps: s1, adding TiO 2 Dissolving the nanosheets and urea in water, and stirring to form a suspension; s2, heating and evaporating the turbid liquid to obtain a white solid; s3, calcining the white solid. The invention also relates to application of the photocatalytic composite material in degrading rhodamine b. The TiO being 2 The photocatalytic composite material has the advantages of high electron hole separation rate, high photocatalytic efficiency and the like, is applied to degrading rhodamine b under ultraviolet light, and has the efficiency of degrading rhodamine b being conventional TiO 2 4-10 times of the material.

Description

TiO 2 2 Photocatalytic composite material, preparation method and application thereof
Technical Field
The invention relates to the field of photocatalytic materials, in particular to TiO 2 A photocatalytic composite material, a preparation method and application thereof.
Background
The photocatalysis technology can degrade toxic non-biodegradable pollutants into non-toxic small molecular substances such as CO and H 2 O and various corresponding inorganic ions to achieve harmlessnessAnd (4) transforming. With the development of human society, the consumption of fossil energy and environmental pollution have come along, and the problems have to be considered. Water is a necessary condition for people to live, so that water pollution treatment becomes a major concern for human beings.
Rhodamine b is an important representative of artificially synthesized dyes with bright peach red color, xanthene dyes and is widely present in printing and dyeing wastewater. Because the dye is difficult to biodegrade and carcinogenic, and can cause great harm to water environment when being used in large quantity, the dye is very important to the degradation treatment of the dye-containing wastewater.
Titanium dioxide (TiO) 2 ) The photocatalyst is an important semiconductor photocatalytic material, and has the characteristics of good photochemical stability, no toxicity, strong oxidizing ability to pollutants under illumination and the like. However, the ultraviolet light has the defects that the band gap energy is large, and the ultraviolet light can only be excited by ultraviolet light with short wavelength, and the energy occupied by the ultraviolet light in sunlight is only 3-5%, so that the utilization rate of the ultraviolet light to the sunlight is very low. Furthermore, tiO 2 After being excited by light, the generated photo-generated electrons and holes are easy to recombine, the photo-generated carrier efficiency is reduced, and the photo-catalytic activity is severely restricted. Therefore, for TiO with high photocatalytic activity 2 The research of (2) has important theoretical significance and practical application value.
Disclosure of Invention
The present invention is directed to solving one of the technical problems of the prior art. To this end, the invention provides a new titanium dioxide (TiO) with simple structure 2 ) The photocatalytic composite material can improve the electron hole separation rate of the material and improve TiO 2 Photodegradability to organic contaminants.
An object of the present invention is to provide a TiO compound 2 The photocatalytic composite material is realized by the following technical means:
TiO 2 2 Photocatalytic composite material comprising TiO 2 Nanosheet and supported on TiO 2 g-C on nanosheets 3 N 4 And (4) quantum dots.
Further, the g-C 3 N 4 The size of the quantum dots is 15-50nm.
Further, the TiO 2 The thickness of the photocatalytic composite material is in the nanometer level, and the cross section size is in the micrometer level.
Another object of the present invention is to provide the above TiO 2 The preparation method of the photocatalytic composite material is realized by the following technical means:
TiO 2 2 The preparation method of the photocatalytic composite material comprises the following steps:
s1, adding TiO 2 Dissolving a nano sheet (TNS) and urea in water, and stirring to form a suspension;
s2, heating and evaporating the turbid liquid to obtain a white solid;
s3, calcining the white solid.
Further, the TiO 2 The mass ratio of the nanosheets to urea is 3: (500-1000).
Further, in S2, the temperature of the heating evaporation is 75-85 ℃.
Further, in S3, the calcination is carried out by gradually raising the temperature, wherein the temperature raising rate is 5-15 ℃/min.
Further, in S3, the calcination temperature is 550-580 ℃ in the calcination.
Further, the method also comprises a process of grinding the obtained product after the step S3.
Another object of the present invention is to provide a method for producing the above-mentioned TiO compound 2 Application of the photocatalytic composite material in degrading rhodamine b.
The invention has the beneficial effects that:
to TiO 2 2 The structure of the photocatalytic composite material introduces g-C 3 N 4 Quantum dots of so that g-C 3 N 4 Quantum dot supported on TiO 2 On the nano-chip, the TiO of the invention is obtained 2 Photocatalytic composite material due to g-C 3 N 4 Quantum dots and TiO 2 The strong interaction between the two nano sheets can form a heterojunction, is favorable for the rapid migration of photo-generated electrons, and improves TiO 2 Photocatalytic performance.
The TiO being 2 The photocatalytic composite material has the advantages of high electron hole separation rate, high photocatalytic efficiency and the like, is applied to degrading rhodamine b under ultraviolet light, and has the efficiency of degrading rhodamine b being conventional TiO 2 4-10 times of the material.
Drawings
FIG. 1 shows TiO described in example 1 of the present invention 2 A flow diagram of the preparation process of the photocatalytic composite material;
FIGS. 2 (a) and 2 (b) are Scanning Electron Microscope (SEM) diagrams of the resulting samples of example 2 and comparative example 1, respectively, in test example 1 of the present invention;
FIG. 3 is a schematic view of infrared spectroscopic analysis of the resulting samples of examples 1 to 3 and comparative examples 1 to 2 in test example 2 of the present invention;
FIG. 4 is a schematic diagram showing X-ray diffraction patterns of the resulting samples of examples 1 to 3 and comparative examples 1 to 2 in test example 3 of the present invention;
FIG. 5 is a schematic diagram showing photoluminescence spectra of the obtained samples of example 2, comparative example 1 and comparative example 2 in test example 4 of the present invention;
FIG. 6 shows the results of examples 1-3 and comparative examples 1-2 in test example 5 of the present invention, and no catalyst (no catalyst) and TiO 2 A test schematic diagram of the photocatalytic degradation efficiency of The Nanosheet (TNS) to rhodamine b is shown.
Wherein, the no catalyst (no catalyst) is that no substance with positive effect on degrading rhodamine b is added, namely a blank sample.
Detailed Description
In order that the invention may be better understood, reference will now be made to the following examples. The scope of the invention is not limited to the embodiments of the invention. Unless otherwise noted, the ingredients and test methods mentioned in the examples of this patent disclosure are conventional methods known to those skilled in the art.
TiO as described in this example 2 Reference to specific methods of synthesis of nanoplatelets (Yang, jinlin, et al, angewandte Chemie International Edition 58.26 (2019): 8740-8745.);
TiO described in examples 1 to 3 2 The flow of the preparation process of the photocatalytic composite material is shown in fig. 1. Visible, tiO 2 Intercalation of nano-sheet with K ion TiO 2 After a series of proton exchange, the layered structure is exfoliated by TMAH intercalation to form a single-layer nanosheet structure; and TiO 2 2 Dissolving the nanosheet and urea in water, uniformly stirring, heating for evaporation, and carrying out high-temperature thermal polymerization on the mixture of the nanosheet and urea to obtain g-C 3 N 4 Quantum dots can be uniformly loaded on TiO with sheet structure 2 To obtain the final TiO 2 A photocatalytic composite material.
Example 1
TiO 2 2 A photocatalytic composite material comprising TiO having a thickness of 1.1nm and a cross-sectional dimension of 10 to 15 μm 2 Nanosheets; and supported on TiO 2 g-C with an average size of 15nm on the nanoplatelets 3 N 4 And (4) quantum dots. The preparation method comprises the following steps:
s1, weighing 60mg of TiO 2 Adding the nanosheets and 10g of urea into a beaker, adding 50mL of water, and uniformly stirring to obtain a suspension;
s2, heating and evaporating the suspension liquid under the condition of an oil bath at the temperature of 80 ℃ to obtain a white solid;
s3, transferring the white solid mixture into a 100ml aluminum oxide crucible with a cover, placing the crucible into a muffle furnace, gradually heating to 550 ℃ at a heating rate of 10 ℃/min, and calcining for 4 hours at 550 ℃;
and S4, naturally cooling to room temperature, grinding the obtained sample again, and marking the obtained product as 15T10U.
Example 2
TiO 2 2 A photocatalytic composite material comprising TiO having a thickness of 1.1nm and a cross-sectional dimension of 10 to 15 μm 2 A nanosheet; and supported on TiO 2 g-C with an average size of 50nm on the nanoplatelets 3 N 4 And (4) quantum dots. The preparation method comprises the following steps:
s1, weighing 60mg of TiO 2 Adding the nanosheet and 15g of urea into a beaker, adding 50mL of water, and uniformly stirring to obtain the productObtaining suspension;
s2, heating and evaporating the suspension liquid under the condition of oil bath at the temperature of 85 ℃ to obtain a white solid;
s3, transferring the white solid mixture into a 100ml aluminum oxide crucible with a cover, placing the crucible in a muffle furnace, gradually heating to 580 ℃ at a heating rate of 15 ℃/min, and calcining for 4 hours at 580 ℃;
and S4, naturally cooling to room temperature, grinding the obtained sample again, and marking the obtained product as 15T15U.
Example 3
TiO 2 2 A photocatalytic composite material comprising TiO having a thickness of 1.1nm and a cross-sectional dimension of 10 to 15 μm 2 Nanosheets; and supported on TiO 2 g-C with an average size of 35nm on the nanoplatelets 3 N 4 And (4) quantum dots. The preparation method comprises the following steps:
s1, weighing 60mg of TiO 2 Adding the nanosheet and 20g of urea into a beaker, adding 50mL of water, and uniformly stirring to obtain a suspension;
s2, heating and evaporating the suspension liquid under the condition of oil bath at the temperature of 75 ℃ to obtain a white solid;
s3, transferring the white solid mixture into a 100ml aluminum oxide crucible with a cover, placing the crucible into a muffle furnace, gradually heating to 550 ℃ at a heating rate of 5 ℃/min, and calcining for 4 hours at 550 ℃;
s4, naturally cooling to room temperature, grinding the obtained sample again, and marking the obtained product as 15T20U.
Comparative example 1
The kind of raw material, the amount of raw material added, the preparation method and the parameters of comparative example 1 were the same as those of example 1 except that urea was not added to S1 of comparative example 1, and the obtained product was marked as CTNS.
Comparative example 2
The kind of raw material, the amount of raw material added, the preparation method and the parameters of comparative example 2 were the same as those of example 1 except that TiO was not added to S1 of comparative example 2 2 Nanosheet, the resulting product was labeled UCN.
Test example 1
Scanning Electron Microscope (SEM) topography:
the Scanning Electron Microscope (SEM) morphology of the samples obtained in example 2 and comparative example 1 is shown in FIG. 2, and from the SEM image, tiO in the sample of example 2 is shown 2 The photocatalytic composite material has a complete massive sheet structure, and fine particles, namely g-C, are uniformly dispersed on the surface of the nanosheet 3 N 4 And (4) quantum dots. The two are fully combined to promote the rapid migration of photo-generated electrons, so that the photocatalytic performance of the material is greatly improved. However, the sample of comparative example 1 did not have the above phenomenon.
Test example 2
Infrared spectroscopic analysis (FTIR):
infrared spectroscopic analysis (FTIR) of the samples obtained in examples 1 to 3 and comparative examples 1 to 2 is shown in FIG. 3. As can be seen from FIG. 3, the UCN of comparative example 2 exhibits typical pure phase g-C 3 N 4 A characteristic absorption peak; CTNS at 467cm for comparative example 1 -1 Presents typical TiO 2 The broad peak, 15T10U of example 1, compared to the peak shape of CTNS, was nearly identical. While the 15T15U of example 2 was obtained at 1242, 1319, 1406, 1463 and 1630cm with increasing urea content in the pretreatment -1 A series of weak peaks are appeared, the stretching mode of the CN heterocyclic ring is met, and the appearance of the new peaks indicates that the TiO is 2 In fact there is a low loading of g-C 3 N 4 And (4) quantum dots. Furthermore, it is apparent that g-C is observed in 15T20U of example 3 3 N 4 Typical characteristic peaks of (A), indicating that there is a sufficient amount of g-C 3 N 4 In TiO 2 Loading on the nanoplatelets. Meanwhile, the CTNS broad peak is from 467cm -l Reduced to 457cm of 15T15U -l Also illustrates the g-C 3 N 4 Quantum dots and TiO 2 There is a strong interfacial interaction between them. The result is beneficial to the electron transfer of the photocatalytic material, so that the rapid recombination of a photoproduction hole and a photoproduction electron is inhibited, and the photocatalytic degradation efficiency of the catalyst is improved.
Test example 3
X-ray diffraction (XRD) pattern:
x-ray diffraction of samples obtained in examples 1 to 3 and comparative examples 1 to 2The emission (XRD) pattern is shown in FIG. 4. As can be seen from FIG. 4, tiO 2 After the nanosheet is calcined at 550 ℃ for 4h, ti is generated 1.73 O 4 1.07 -phase transition of nanosheet to anatase (CTNS). Furthermore, urea is mixed with TiO 2 The nanosheets adopt a similar heat treatment process, and the obtained samples 15TxU all present anatase phases, which shows that the phase change of the material is not interfered by the addition and thermal polymerization of urea. The peak value gradually decreases from CTNS, 15T10U to 15T20U with increasing urea content during calcination, which is associated with g-C on the lattice plane 3 N 4 The coverage of the quantum dots is relevant. At the same time, no significant g-C was found 3 N 4 Diffraction peaks show that the catalyst has low load and high dispersity and can effectively promote the separation of photoproduction electrons and photoproduction holes of the catalyst.
Test example 4
Photoluminescence spectrum test:
photoluminescence spectra of samples 15T15U, CTNS and UCN obtained in example 2, comparative example 1 and comparative example 2 are shown in fig. 5. As can be seen from FIG. 5, the fluorescence quenching of sample 15T15U and sample CTNS is more pronounced than that of sample UCN, while that of sample 15T15U is the most pronounced, indicating that TiO 2 A proper amount of g-C is loaded on the nano-chip 3 N 4 The quantum dots can inhibit the recombination of photo-generated electrons and photo-generated holes, so that the performance of the photocatalytic material is greatly improved.
Test example 5
Testing photocatalytic degradation efficiency:
samples from examples 1-3, comparative examples 1-2, and no added catalyst (no catalyst) and TiO 2 The photocatalytic degradation efficiency of the single-layer nanosheet (TNS) to rhodamine b is shown in FIG. 6. As can be seen from FIG. 6, under 365nm UV light without catalyst, rhodamine b is hardly degraded over time. The TNS sample is degraded by about 10% only under dark adsorption, and has no obvious change under the later illumination condition. The degradation efficiency of anatase (CTNS) formed after calcining the sample TNS at 550 ℃ for 4h is further improved, and the degradation efficiency is only about 40% after 40 minutes of illumination. Sample 15TxU (15T 10U, 15T 15U) obtained after copolymerization of urea and TNS15T 20U) compared with CTNS, the degradation efficiency of the sample 15T15U reaches 100% in about 40 min.
Table 1 shows the ratio of the residual mass to the original mass of rhodamine b catalytically degraded by the light of different samples at different times. The smaller the ratio, the more desirable the results.
TABLE 1 ratio of residual mass to original mass of rhodamine b photocatalytically degraded by different samples at different times
Figure BDA0002743223360000061
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.

Claims (9)

1. TiO 2 2 Photocatalytic composite material, characterized in that the TiO is 2 The photocatalytic composite material comprises TiO 2 Nanosheet and supported on TiO 2 g-C on nanosheets 3 N 4 Quantum dots; the TiO is 2 The synthesis method of the nano sheet comprises the following steps: intercalation of TiO by K ions 2 Preparation K 0.8 [Ti 1.73 Li 0.27 ]O 4 After proton exchange, the layered structure H 1.07 Ti 1.73 O 4 ·H 2 TiO with O exfoliated by TMAOH intercalation to form single-layer nano-sheet structure 2 Nanosheets;
the TiO is 2 The preparation method of the photocatalytic composite material comprises the following steps:
s1, adding TiO 2 Dissolving the nanosheets and urea in water, and stirring to form a suspension;
s2, heating and evaporating the turbid liquid to obtain a white solid;
s3, calcining the white solid;
the TiO is 2 The thickness of the photocatalytic composite material is in the nanometer level, and the cross section size is in the micrometer level.
2. The TiO of claim 1 2 Photocatalytic composite material characterized by the g-C 3 N 4 The size of the quantum dots is 15-50nm.
3. TiO according to any one of claims 1 to 2 2 The preparation method of the photocatalytic composite material is characterized by comprising the following steps of:
s1, adding TiO 2 Dissolving the nanosheets and urea in water, and stirring to form a suspension;
s2, heating and evaporating the turbid liquid to obtain a white solid;
s3, calcining the white solid;
the TiO is 2 The synthesis method of the nano sheet comprises the following steps: intercalation of TiO by K ions 2 Preparation K 0.8 [Ti 1.73 Li 0.27 ]O 4 After proton exchange, the layered structure H 1.07 Ti 1.73 O 4 ·H 2 TiO with O exfoliated by TMAOH intercalation to form single-layer nano-sheet structure 2 Nanosheets.
4. The TiO of claim 3 2 The preparation method of the photocatalytic composite material is characterized in that the TiO is 2 The mass ratio of the nanosheets to urea is 3: (500-1000)。
5. The TiO of claim 3 2 The preparation method of the photocatalytic composite material is characterized in that in S2, the heating and evaporation temperature is 75-85 ℃.
6. The TiO of claim 3 2 The preparation method of the photocatalytic composite material is characterized in that in S3, calcination is carried out by gradually increasing the temperature, wherein the temperature increase rate is 5-15 ℃/min.
7. The TiO of claim 3 2 The preparation method of the photocatalytic composite material is characterized in that in S3, the calcination temperature is 550-580 ℃.
8. The TiO of claim 3 2 The preparation method of the photocatalytic composite material is characterized by further comprising a process of grinding the product obtained in the step S3.
9. The TiO of any one of claims 1 to 2 2 Application of a photocatalytic composite material in photocatalytic degradation of rhodamine B.
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