CN114849692B - TiO (titanium dioxide) 2 -C-MoO 2 Preparation method and application of nanocomposite - Google Patents

TiO (titanium dioxide) 2 -C-MoO 2 Preparation method and application of nanocomposite Download PDF

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CN114849692B
CN114849692B CN202210390958.0A CN202210390958A CN114849692B CN 114849692 B CN114849692 B CN 114849692B CN 202210390958 A CN202210390958 A CN 202210390958A CN 114849692 B CN114849692 B CN 114849692B
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tio
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titanium dioxide
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CN114849692A (en
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乔秀清
王紫昭
李晨
侯东芳
李东升
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China Three Gorges University CTGU
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    • 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
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/24—Chromium, molybdenum or tungsten
    • B01J23/28—Molybdenum
    • 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
    • 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
    • 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
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
    • C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
    • C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
    • C01B3/042—Decomposition of water
    • C—CHEMISTRY; METALLURGY
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
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    • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/02—Processes for making hydrogen or synthesis gas
    • C01B2203/0266—Processes for making hydrogen or synthesis gas containing a decomposition step
    • C01B2203/0277—Processes for making hydrogen or synthesis gas containing a decomposition step containing a catalytic decomposition step
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/10—Catalysts for performing the hydrogen forming reactions
    • C01B2203/1041—Composition of the catalyst
    • 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
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    • 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
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    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
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    • Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy

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Abstract

The application discloses a TiO 2 ‑C‑MoO 2 A preparation method and application of a nanocomposite, belonging to the field of nanomaterial preparation. The application adopts a one-step high-temperature calcination process, uniformly mixes P25, an organic carbon source and inorganic Mo salt according to a proportion, and carries out pyrolysis reaction under a high-temperature condition by adjusting the proportion of the three to obtain TiO 2 ‑C‑MoO 2 The nano composite material is then used in the fields of photocatalysis hydrogen production and sewage treatment. The application adopts a one-step synthesis method to prepare TiO 2 ‑C‑MoO 2 The nano composite material has simple process, economy and environmental protection, and is suitable for mass production. Meanwhile, the prepared TiO 2 ‑C‑MoO 2 The nanocomposite has better dispersibility, can greatly improve the photocatalytic activity of P25, has good application prospect, and is favorable for wide popularization and application.

Description

TiO (titanium dioxide) 2 -C-MoO 2 Preparation method and application of nanocomposite
Technical Field
The application relates to a TiO 2 -C-MoO 2 A preparation method and application of a nanocomposite, belonging to the field of functional nanomaterial preparation.
Background
With the development of economy, the problems of energy crisis, environmental pollution and the like generated by the excessive use of traditional fossil energy become worldwide challenges. Currently, a recognized problem in various countries that addresses these two challenges is the development of clean energy sources, such as solar, wind, tidal, and the like. Wherein, the solar energy is inexhaustible clean energy, and the solar energy is fully utilized to generate the clean energy and simultaneously removeThe removal of environmental pollution generated in industrial production is a very promising technology. The key to realize solar energy utilization is a semiconductor photocatalysis technology. The photocatalysis technology utilizes the semiconductor oxide material to be excited under the illumination effect to generate photo-generated electrons and holes, the photo-generated electrons can be transferred to the conduction band position of the semiconductor, the electrons on the conduction band have stronger reducibility, and H can be generated + Reduction to H 2 Or reducing heavy metal ions; the photo-generated holes are transferred to the valence band, and the holes on the valence band and the generated hydroxyl free radicals have stronger oxidizing capability, so that the photo-generated holes can effectively oxidize and decompose organic matters, kill bacteria and eliminate peculiar smell. The photocatalysis technology can directly utilize solar energy, has mild reaction conditions, is economical, has no secondary pollution to products, and has incomparable advantages compared with the traditional chemical catalysis technology, adsorption technology and biological catalysis technology. While the key to promoting the application of photocatalytic technology is the development of highly efficient photocatalytic materials.
Currently, the best photocatalytic material for commercial use is P25. P25 is titanium dioxide formed by mixing two crystal phases of anatase and rutile. The nanometer glass is widely applied to nanometer paint, air purifier, self-cleaning glass, ceramics and the like. The modified polyurethane foam has wide application in the fields of antibiosis and mildew prevention, exhaust purification, deodorization, water treatment, pollution prevention, weather resistance and aging resistance, automotive finishing paint and the like, and has wide application prospects in the fields of environment, information, materials, energy, medical treatment, sanitation and the like. However, currently widely used TiO 2 The wide forbidden bandwidth of the solar energy collector can not absorb visible light, and the ultraviolet light in sunlight only accounts for 5 percent, so that the TiO 2 The quantum efficiency of (2) is low and the photocatalytic activity is limited. Although many semiconductor materials have been demonstrated to have visible light photocatalytic activity, they have been difficult to be practically used due to low activity or due to susceptibility to photo-etching. Thus, for TiO 2 The photocatalytic material is modified and designed, and the improvement of the visible light absorption performance, the quantum yield and the stability of the photocatalytic material is a hot spot for research in the current photocatalytic field.
For TiO 2 The problems are that the methods such as nonmetal, metal doping, morphology regulation, heterojunction structure and the like can improve the pair performanceResearch on the response of visible light is receiving attention. Wherein the construction of a heterojunction has proven to be an effective way of increasing the efficiency of the separation of photogenerated electrons and holes. At present, more TiO 2 The base heterojunction material has been constructed, and the photocatalytic activity is greatly improved. However, currently reported TiO 2 The preparation process of the base heterojunction material is mostly a hydrothermal/solvothermal method, the flow is complex, the conductivity of the obtained composite material is low, and the performance of the heterojunction material is limited. Thus, a simple and effective TiO was developed 2 Modification method of base heterojunction material to obtain TiO with excellent catalytic performance and good stability 2 The photocatalytic material has important application value and economic benefit.
Disclosure of Invention
In view of the shortcomings of the prior art, the application aims to provide a TiO 2 -C-MoO 2 The preparation method of the nanocomposite material can realize TiO by a simple high-temperature calcination method without any additive and redundant process 2 -C-MoO 2 Preparation of nanocomposite materials.
TiO prepared by the application 2 -C-MoO 2 Nanocomposite is made of TiO 2 Nanoparticles, C interface layer and MoO 2 Nanoparticle composition with C interface layer at TiO 2 With MoO 2 The nano particles play a role in electron transmission and promote TiO 2 With MoO 2 Charge migration therebetween.
TiO (titanium dioxide) 2 -C-MoO 2 The preparation method of the nanocomposite adopts a one-step high-temperature calcination method, and comprises the following steps:
a certain amount of P25, an organic carbon source and inorganic Mo salt are ground and mixed uniformly according to a proportion, and then the obtained mixture is subjected to high-temperature pyrolysis reduction reaction in inert atmosphere to obtain TiO 2 -C-MoO 2 A nanocomposite.
Preferably, the organic carbon source is predominantly citric acid, in the process described above.
Preferably, the inorganic Mo salt is mainly ammonium molybdate.
Preferably, the titanium dioxide (model P25) has a mass ratio of organic carbon source to inorganic Mo salt of 2:1:0.5 to 2:1:1.5.
preferably, the inert atmosphere is argon, the high-temperature calcination temperature is 700-900 ℃, and the reaction time is 1-4 hours.
TiO prepared by the application 2 -C-MoO 2 Compared with the prior art, the nanocomposite has the beneficial effects that:
the obtained TiO 2 -C-MoO 2 The nanocomposite has a closely contacted interface structure, and the particles have small size and uniform distribution. The adopted process flow is simple, the equipment requirement is low, the energy consumption and the reaction cost are reduced, the method is nontoxic and harmless, meets the environment-friendly requirement, and is easy to realize industrialization.
Drawings
Fig. 1: tiO prepared for example 1 2 -C-MoO 2 XRD pattern of nanocomposite.
Fig. 2: tiO prepared for example 1 2 -C-MoO 2 Raman spectra of nanocomposite materials.
Fig. 3: tiO prepared for example 1 2 -C-MoO 2 Scanning electron microscope pictures of the nanocomposite, a is a low-power SEM picture, and b is a high-power SEM picture.
Fig. 4: tiO prepared for example 1 2 -C-MoO 2 Photo-catalytic hydrogen production pattern of nanocomposite.
Fig. 5: tiO prepared for example 1 2 -C-MoO 2 A graph of the stability of hydrogen in water by photocatalytic decomposition of the nanocomposite.
Fig. 6: tiO prepared for example 3 2 -C-MoO 2 Photocatalytic reduction Cr performance profile for nanocomposite.
Detailed Description
The present application is further illustrated below in conjunction with specific embodiments, it being understood that these embodiments are meant to be illustrative of the application and not limiting the scope of the application, and that modifications of the application, which are equivalent to those skilled in the art to which the application pertains, fall within the scope of the application defined in the appended claims after reading the application.
Example 1
Uniformly mixing 2 g of P25,1g of citric acid and x g of ammonium molybdate (x=0.5, 1, 1.5), then preserving the heat of the mixed powder for 1h at 200 ℃ in Ar atmosphere, and then heating to 800 ℃ for 2h to obtain TiO 2 -C-MoO 2 The nanocomposite, three samples were labeled TCM 2:1:0.5, TCM 2:1:1, TCM 2:1:1.5, respectively. For comparison, the sample obtained at an amount of 0 of ammonium molybdate was labeled TiO 2 -C。
TiO prepared as described above 2 -C-MoO 2 XRD diffraction patterns of the nanocomposite are shown in figure 1, and the XRD diffraction patterns are compared with that of a standard sample TiO 2 With MoO 2 XRD diffraction peak contrast analysis of (1) shows that the composite nano material contains TiO 2 MoO (MoO) 2 And (3) nanoparticles. Raman spectroscopy analysis of TCM 2:1:1 samples (fig. 2) indicated that amorphous carbon was present in the nanocomposite. The scanning electron microscope of the TCM 2:1:1 sample is shown in fig. 3, and as can be seen from fig. 3a and an enlarged view of fig. 3b, the composite nano material is in nano size, and the particle size distribution is uniform.
Samples of TCM 2:1:0.5, TCM 2:1:1 and TCM 2:1:1.5 prepared in 20 and mg were placed in a photocatalytic reaction vessel, 8 ml of lactic acid and 80 ml of aqueous solution were added into the reaction vessel, and a photocatalytic hydrogen production test was performed under a xenon lamp light source equipped with a 420 nm filter. The hydrogen production performance is shown in fig. 4. It can be seen that the pure P25 has a photocatalytic hydrogen production performance of substantially 0, and the TiO is obtained after adding citric acid 2 The hydrogen production of the-C is 20 mu mol/g h, and MoO is added 2 After that, tiO 2 -C-MoO 2 The photocatalytic hydrogen production activity of the nanocomposite is obviously improved, wherein when the mass of ammonium molybdate is 1g, the obtained nanocomposite (TCM 2:1:1) has the highest photocatalytic hydrogen production activity of 500 mu mol/g.h, which is 25 times that of the nanocomposite without ammonium molybdate. But further increase MoO 2 After the content of (2), the performance is significantly reduced, possibly in excess of MoO 2 The absorption of light by the material is suppressed and the generation of photo-generated electrons is reduced. Subsequently we performed a cyclic stability assay on TCM 2:1:1 for this example. And after the hydrogen production test is finished every 3 hours, exhausting and vacuumizing the system, and then continuing to produce hydrogen next time. The cycle experiment shows that after 27 hoursThe original photocatalytic activity can be maintained after illumination (9 cycles) (fig. 5), which shows that the catalyst has better stability.
Example 2
Uniformly mixing citric acid (x= 0,0.5,1,1.5) of P25 and x g of 2 g with ammonium molybdate of 1g, then preserving heat of the mixed powder for 1h at 150 ℃ under Ar atmosphere, and then heating to 820 ℃ for 2h to obtain the nanocomposite. When the content of citric acid is 0, the obtained product is TiO 2 -MoO 2 After the citric acid is added into the nanocomposite, a Raman spectrum peak of C appears in the product, which proves that TiO is generated 2 -C-MoO 2 A nanocomposite.
The prepared nanocomposite of 20 and mg was subjected to a photocatalytic hydrogen production test, and the test procedure was the same as in example 1. When the content of citric acid is 0, the obtained TiO 2 -MoO 2 The photocatalytic hydrogen production activity of the nanocomposite is close to P25, basically 0, and TiO 2 -C-MoO 2 The photocatalytic hydrogen production activity of the nanocomposite is obviously improved, and when the quality of the citric acid is 0.5,1 and 1.5, the obtained hydrogen production amounts are 245 mu mol/g h,500 mu mol/g h and 678 mu mol/g.h respectively. Wherein when the mass of the citric acid is 1g, the obtained nanocomposite has the highest photocatalytic hydrogen production activity.
Example 3
Uniformly mixing 2 g P25,1g citric acid and x g ammonium molybdate (x= 0.4,0.6,0.8,1,1.2,1.4), then preserving the heat of the mixed powder for 1h at 200 ℃ under Ar atmosphere, and then heating to 850 ℃ for 2h to obtain TiO 2 -C-MoO 2 A nanocomposite. The resulting samples are individually labeled TCM 2:1:0.4,TCM 2:1:0.6,TCM 2:1:0.8,TCM 2:1:1,TCM 2:1:1.2,TCM 2:1:1.4.
The prepared TiO 2 -C-MoO 2 The nanocomposite is used for photocatalytic reduction of hexavalent cadmium ions. 10 mg of the nanocomposite was added to 50 mg/L dichromate solution. Stirring in a darkroom for 40 min, irradiating the solution under 500W xenon lamp, centrifuging 5 ml suspension every 2 min to obtain supernatantAnd carrying out ultraviolet-visible absorption spectrum test on the liquid to obtain data of photocatalytic reduction of hexavalent Cr. The experimental results are shown in FIG. 6, tiO 2 -C-MoO 2 The time required for completely reducing hexavalent Cr into trivalent Cr ions by the nanocomposite is different, and the time required for TCM 2:1:1.2 samples is shortest, and only about 10 minutes is required.
Example 4
Uniformly mixing citric acid (x= 0.5,1,1.5,2,2.5) of P25 and x g of 2 g with ammonium molybdate of 1g, then preserving heat of the mixed powder for 1h at 150 ℃ under Ar atmosphere, and then heating to 850 ℃ for 2h to obtain the nanocomposite.
The prepared TiO 2 -C-MoO 2 The nanocomposite is used for experiments of photocatalytic degradation of methyl orange. The nanocomposite of 3 mg was added to 100 mg/L methyl orange solution. After stirring in a darkroom for 40 minutes, the solution was irradiated under a xenon lamp light source, and the concentration of methyl orange was recorded by taking a suspension of 5 ml every 2 minutes. The experimental results showed that the time required to completely degrade methyl orange was 24 min,21min,16 min,18 min,20 min when the citric acid content was 0.5,1,1.5,2,2.5.

Claims (7)

1. TiO (titanium dioxide) 2 -C-MoO 2 The application of the nano composite material in promoting the photocatalytic material to decompose the water into hydrogen is characterized in that the TiO 2 -C-MoO 2 The preparation method of the nanocomposite comprises the following steps: grinding and mixing a certain amount of titanium dioxide, an organic carbon source and inorganic Mo salt according to a proportion, and then carrying out high-temperature pyrolysis reduction reaction on the obtained mixture in inert atmosphere to obtain TiO 2 -C-MoO 2 A nanocomposite.
2. TiO (titanium dioxide) 2 -C-MoO 2 Application of nanocomposite material in photocatalytic reduction of hexavalent cadmium ions is characterized in that TiO 2 -C-MoO 2 The preparation method of the nanocomposite comprises the following steps: grinding and mixing a certain amount of titanium dioxide, an organic carbon source and inorganic Mo salt according to a certain proportion, and then making the obtained mixture in inert atmosphereHigh-temperature pyrolysis reduction reaction to obtain TiO 2 -C-MoO 2 A nanocomposite.
3. The use according to claim 1 or 2, wherein the organic carbon source is citric acid.
4. Use according to claim 1 or 2, characterized in that the inorganic Mo salt is ammonium molybdate.
5. Use according to claim 1 or 2, characterized in that the mass ratio of titanium dioxide, organic carbon source and inorganic Mo salt is 2:1:0.5 to 2:1:1.5.
6. the use according to claim 1 or 2, wherein the inert atmosphere is argon, the high temperature calcination temperature is 700 ℃ to 900 ℃, and the reaction time is 1 to 4 hours.
7. The use according to claim 1 or 2, wherein the TiO 2 -C-MoO 2 The particle size of the nanocomposite is 10-100 nm.
CN202210390958.0A 2022-04-14 2022-04-14 TiO (titanium dioxide) 2 -C-MoO 2 Preparation method and application of nanocomposite Active CN114849692B (en)

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