CN114849692A - TiO 2 2 -C-MoO 2 Preparation method and application of nano composite material - Google Patents

TiO 2 2 -C-MoO 2 Preparation method and application of nano composite material Download PDF

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CN114849692A
CN114849692A CN202210390958.0A CN202210390958A CN114849692A CN 114849692 A CN114849692 A CN 114849692A CN 202210390958 A CN202210390958 A CN 202210390958A CN 114849692 A CN114849692 A CN 114849692A
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tio
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CN114849692B (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
    • 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
    • C01B2203/02—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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    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
    • 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W10/00—Technologies for wastewater treatment
    • Y02W10/30—Wastewater or sewage treatment systems using renewable energies
    • Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy

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Abstract

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

Description

TiO 2 2 -C-MoO 2 Preparation method and application of nano composite material
Technical Field
The invention relates to a TiO compound 2 -C-MoO 2 A method for preparing a nano composite material and application thereof, belonging to the field of power generationCan be used in the field of nano material preparation.
Background
With the development of economy, problems such as energy crisis and environmental pollution caused by excessive use of traditional fossil energy become challenges worldwide. Currently, the problem recognized by various countries to solve these two challenges is to develop clean energy sources, such as solar energy, wind energy, tidal energy, etc. Among them, solar energy is an inexhaustible clean energy, and it is a very promising technology to fully utilize solar energy to generate clean energy and simultaneously remove environmental pollution generated in industrial production. The key to realizing solar energy utilization is the semiconductor photocatalysis technology. The photocatalysis technology utilizes a semiconductor oxide material to be excited under the action of illumination to generate photoproduction electrons and holes, the photoproduction electrons can be transferred to the position of a conduction band of a semiconductor, the electrons on the conduction band have strong reducibility, and H can be converted + Reduction to produce H 2 Or reducing heavy metal ions; the photoproduction holes are transferred to the valence band, and the holes on the valence band and the generated hydroxyl free radicals have strong oxidizing capability, so that organic matters can be effectively oxidized and decomposed, bacteria can be killed, and peculiar smell can be eliminated. The photocatalysis technology can directly utilize solar energy, has mild and economic reaction conditions and no secondary pollution of products, and has incomparable advantages compared with the traditional chemical catalysis technology, adsorption technology and biological catalysis technology. The key to promoting the application of photocatalytic technology is the development of efficient photocatalytic materials.
Currently, the best commercially available photocatalytic material is P25. P25 is titanium dioxide formed by mixing two crystal phases of anatase and rutile. The coating is widely applied to nano coatings, air purifiers, self-cleaning glass, ceramics and the like at present. The paint has wide application in the fields of antibiosis, mildew prevention, exhaust purification, deodorization, water treatment, antifouling, weather resistance, ageing resistance, automobile finish paint and the like, and has wide application prospect in the fields of environment, information, materials, energy, medical treatment, sanitation and the like. However, TiO is currently in common use 2 Has a wide forbidden band width, so that the TiO material cannot absorb visible light, and the ultraviolet light in the sunlight only accounts for 5 percent, so that the TiO material has high absorption rate and high absorption rate 2 The quantum efficiency is low and the photocatalytic activity is limited.Although many semiconductor materials have been proven to have photocatalytic activity of visible light, they are difficult to be put into practical use because of their low activity or susceptibility to photo-corrosion. Thus, for TiO 2 The modification design of the photocatalytic material to improve the visible light absorption performance, quantum yield and stability of the photocatalytic material is a hotspot of current research in the field of photocatalysis.
For TiO 2 The research on the response of the method to visible light can be improved by methods such as nonmetal, metal doping, morphology regulation, heterojunction structure and the like. Wherein heterojunctions are constructed, have proven to be an effective method of increasing the efficiency of the separation of photogenerated electrons and holes. At present, more TiO is available 2 The base heterojunction material is constructed, and the photocatalytic activity is greatly improved. However, TiO is currently reported 2 Most of preparation processes of the base heterojunction material are hydrothermal/solvothermal methods, the process is complex, and the obtained composite material is low in conductivity and limits the performance exertion of the heterojunction material. Thus, a simple and effective TiO was developed 2 The TiO with excellent catalytic performance and good stability obtained by the modification method of the base heterojunction material 2 The photocatalytic material has important application value and economic benefit.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide TiO 2 -C-MoO 2 The preparation method of the nano composite material can realize TiO through a simple high-temperature calcination method without any additive and redundant process 2 -C-MoO 2 And (3) preparing the nano composite material.
TiO prepared by the invention 2 -C-MoO 2 The nano composite material is made of TiO 2 Nanoparticles, C interface layer and MoO 2 Nano-particle composition, wherein a C interface layer is positioned on TiO 2 With MoO 2 The nano particles play a role in electron transmission and promote TiO 2 With MoO 2 With charge migration in between.
TiO 2 2 -C-MoO 2 The preparation method of the nano composite material adopts a one-step high-temperature calcination method, and comprises the following steps:
grinding and uniformly mixing a certain amount of P25, an organic carbon source and inorganic Mo salt in proportion, and then carrying out high-temperature pyrolysis reduction reaction on the obtained mixture in an inert atmosphere to obtain TiO 2 -C-MoO 2 A nanocomposite material.
In the method as described above, preferably, the organic carbon source is mainly citric acid.
Preferably, the inorganic Mo salt is predominantly ammonium molybdate.
Preferably, the mass ratio of the titanium dioxide (model P25) to the inorganic Mo salt is 2:1: 0.5-2: 1: 1.5.
preferably, the inert atmosphere is argon, the high-temperature calcination temperature is 700-900 ℃, and the reaction time is 1-4 h.
TiO prepared by the invention 2 -C-MoO 2 Compared with the prior art, the nano composite material has the beneficial effects that:
the resulting TiO 2 -C-MoO 2 The nano composite material has a close contact interface structure, and the particle size is small and the distribution is uniform. The adopted process flow is simple, the equipment requirement is low, so that the energy consumption and the reaction cost are reduced, the method is non-toxic and harmless, the environment-friendly requirement is met, and the industrialization is easy to realize.
Drawings
FIG. 1: TiO prepared for example 1 2 -C-MoO 2 XRD pattern of the nanocomposite.
FIG. 2: TiO prepared for example 1 2 -C-MoO 2 Raman spectra of the nanocomposites.
FIG. 3: TiO prepared for example 1 2 -C-MoO 2 And (3) scanning electron microscope pictures of the nano composite material, wherein 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 The photocatalytic hydrogen production diagram of the nano composite material.
FIG. 5: TiO prepared for example 1 2 -C-MoO 2 The hydrogen stability chart of the water produced by photocatalytic decomposition of the nano composite material.
FIG. 6: TiO prepared for example 3 2 -C-MoO 2 The photocatalytic reduction Cr performance diagram of the nano composite material.
Detailed Description
The present invention is further illustrated by the following examples, which are intended to be purely exemplary and are not intended to limit the scope of the invention, as various equivalent modifications of the invention will occur to those skilled in the art upon reading the present disclosure and fall within the scope of the appended claims.
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 temperature of the mixed powder for 1h at 200 ℃ under Ar atmosphere, and then heating to 800 ℃ for 2h to obtain TiO 2 -C-MoO 2 Three samples of the nanocomposite are respectively marked as TCM 2:1:0.5, TCM 2:1:1 and TCM 2:1: 1.5. For comparison, the sample obtained with an ammonium molybdate amount of 0 is labeled as TiO 2 -C。
TiO prepared as described above 2 -C-MoO 2 The XRD diffraction pattern of the nanocomposite is shown in figure 1, and is compared with that of a standard sample TiO 2 With MoO 2 The XRD diffraction peak contrast analysis shows that the composite nano material contains TiO 2 And MoO 2 And (3) nanoparticles. Raman spectroscopy analysis of the TCM 2:1:1 sample (fig. 2) showed the presence of amorphous carbon 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 its enlarged view 3b, the composite nanomaterial is of nanometer size and the particle size distribution is uniform.
20 mg of the prepared TCM 2:1:0.5, TCM 2:1:1 and TCM 2:1:1.5 samples are placed in a photocatalytic reaction vessel, 8 ml of lactic acid and 80 ml of aqueous solution are added into the reaction vessel, and a photocatalytic hydrogen production test is carried out under a xenon lamp light source with a 420 nm optical filter. The hydrogen production performance is shown in FIG. 4. It can be seen that pure P25 photocatalytic hydrogen production performance is basically 0, and TiO obtained after citric acid is added 2 Hydrogen production of-C20. mu. mol/g.h, MoO added 2 Then, TiO 2 2 -C-MoO 2 The photocatalytic hydrogen production activity of the nano composite material is obviously improved, wherein when the mass of ammonium molybdate is 1g, the obtained nano composite materialThe composite material (TCM 2:1: 1) has the highest photocatalytic hydrogen production activity of 500 mu mol/g.h, which is 25 times that of the composite material without ammonium molybdate. But further increase MoO 2 After the content of (A), the properties are significantly reduced, possibly by an excess of MoO 2 Absorption of light by the material is inhibited, thereby reducing the generation of photo-generated electrons. We then performed a cycle stability assay for this ratio of TCM 2:1:1. And after the hydrogen production test is finished every 3h, exhausting and vacuumizing the system, and then continuing to produce hydrogen next time. The cycle experiment shows that the original photocatalytic activity can be still maintained after 27 hours (9 cycles) of illumination (figure 5), which shows that the catalyst has better stability.
Example 2
2 g of citric acid P25 and x g (x =0, 0.5, 1 and 1.5) and 1g of ammonium molybdate are uniformly mixed, then the mixed powder is firstly subjected to heat preservation for 1h at the temperature of 150 ℃ in Ar atmosphere, and then is heated to 820 ℃ and subjected to heat preservation for 2h, so that the nano composite material is obtained. When the content of citric acid is 0, the obtained product is TiO 2 -MoO 2 After the nano composite material is added with citric acid, the Raman spectrum peak of C appears in the product, which proves that TiO is generated 2 -C-MoO 2 A nanocomposite.
20 mg of the nanocomposite prepared above was subjected to a photocatalytic hydrogen production test in the same manner as in example 1. When the citric acid content is 0, the obtained TiO 2 -MoO 2 The photocatalytic hydrogen production activity of the nano composite material is close to P25 and is basically 0, and TiO 2 -C-MoO 2 The photocatalytic hydrogen production activity of the nano composite material is obviously improved, and when the mass 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 nano composite material has the highest photocatalytic hydrogen production activity.
Example 3
Uniformly mixing 2 g of P25 and 1g of citric acid with x g of ammonium molybdate (x =0.4, 0.6, 0.8, 1, 1.2 and 1.4), then preserving the temperature of the mixed powder for 1h at 200 ℃ under Ar atmosphere, heating to 850 ℃ and preserving the temperature for 2h to obtain TiO 2 -C-MoO 2 Nanocomposite material. The obtained samples are respectively marked as TCM 2:1:0.4, TCM 2:1:0.6, TCM 2:1:0.8, TCM 2:1:1, TCM 2:1:1.2 and TCM 2:1: 1.4.
The prepared TiO is 2 -C-MoO 2 The nano composite material is used for photocatalytic reduction of hexavalent cadmium ions. 10 mg of the nanocomposite was added to 50 mg/L of the dichromate solution. And stirring in a dark room for 40 minutes, irradiating the solution under a 500W xenon lamp light source, centrifuging 5 ml of suspension every 2 min, and performing ultraviolet-visible absorption spectrum test on the obtained supernatant to obtain the data of the photocatalytic reduction of hexavalent Cr. The results of the experiment are shown in FIG. 6, TiO 2 -C-MoO 2 The time required for the nano composite material to completely reduce the hexavalent Cr into the trivalent Cr ions is different, and the time required by a TCM 2:1:1.2 sample is the shortest and only needs about 10 min.
Example 4
2 g of P25, x g citric acid (x =0.5, 1, 1.5, 2, 2.5) and 1g of ammonium molybdate are uniformly mixed, then the mixed powder is firstly kept at 150 ℃ for 1h under Ar atmosphere, and then heated to 850 ℃ for 2h, thus obtaining the nano composite material.
Preparing the obtained TiO 2 -C-MoO 2 The nano composite material is used for an experiment of photocatalytic degradation of methyl orange. 3 mg of the nanocomposite was added to a 100 mg/L methyl orange solution. After stirring in a dark room for 40 minutes, the solution was irradiated under a xenon lamp light source, and 5 ml of a suspension was taken every 2 min to record the concentration of methyl orange. The experiment result shows that when the content of the citric acid is 0.5, 1, 1.5, 2 and 2.5, the time required for completely degrading the methyl orange is 24 min, 21min, 16 min, 18 min and 20 min respectively.

Claims (7)

1. TiO 2 2 -C-MoO 2 The preparation method of the nano composite material is characterized by comprising the following steps: grinding and uniformly 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 an inert atmosphere to obtain TiO 2 -C-MoO 2 A nanocomposite material.
2. The TiO of claim 1 2 -C-MoO 2 The preparation method of the nano composite material is characterized in that the organic carbon source is mainly citric acid.
3. The TiO of claim 1 2 -C-MoO 2 A process for the preparation of a nanocomposite, characterized in that the inorganic Mo salt is mainly ammonium molybdate.
4. The TiO of claim 1 2 -C-MoO 2 The preparation method of the nano composite material is characterized in that the mass ratio of titanium dioxide, an organic carbon source and inorganic Mo salt is 2:1: 0.5-2: 1: 1.5.
5. the TiO of claim 1 2 -C-MoO 2 The preparation method of the nano composite material is characterized in that the inert atmosphere is argon, the high-temperature calcination temperature is 700-900 ℃, and the reaction time is 1-4 h.
6. A TiO prepared as described in claims 1 to 5 2 -C-MoO 2 The nano composite material is characterized in that the particle size of the obtained nano composite material is 10-100 nm.
7. A TiO prepared as described in claims 1 to 5 2 -C-MoO 2 The application of the nano composite material in promoting the photocatalytic material to decompose water to produce hydrogen or treating sewage.
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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