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CN113634245B - High-valence metal ion doped SnO 2 Preparation method and application of nano material - Google Patents

High-valence metal ion doped SnO 2 Preparation method and application of nano material Download PDF

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CN113634245B
CN113634245B CN202110771160.6A CN202110771160A CN113634245B CN 113634245 B CN113634245 B CN 113634245B CN 202110771160 A CN202110771160 A CN 202110771160A CN 113634245 B CN113634245 B CN 113634245B
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CN113634245A (en
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高爽
关海涛
李琦
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Southwest Jiaotong University
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    • 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
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    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract

The invention discloses high-valence metal ion doped SnO 2 A nano material and a preparation method and application thereof belong to the technical field of inorganic nonmetal nano material preparation, solar energy utilization and environmental protection. In particular to a technical means of realizing nano SnO by doping high-valence metal ions 2 The regulation of the defect type of the oxide and the surface activation enable the surface of the material to have the capability of activating carbon dioxide. The high-valence metal ion doped SnO 2 The nano material has excellent photocatalytic degradation performance, and the efficiency of photocatalytic reduction of carbon dioxide under the illumination condition is obviously superior to that of undoped SnO 2 The material solves the existing SnO 2 The nanometer material has poor photocatalytic performance, and can be directly applied to the fields of photocatalytic carbon fixation, pollutant degradation in the environment and the like.

Description

High-valence metal ion doped SnO 2 Preparation method and application of nano material
Technical Field
The invention relates to the technical field of inorganic nonmetal nano-material preparation, solar energy utilization and environmental protection, in particular to high-valence metal ion doped SnO 2 A nano material and a preparation method and application thereof.
Background
The progress of human industrial development has placed a great pressure on the world's energy supply and global warming. Researchers in all countries around the world are actively exploring and searching for effective strategies to reduce carbon dioxide into methanol, ethanol, acetaldehyde and compounds thereof by means of photocatalysis technology, and the carbon dioxide can be used as organic industrial fuel and other valuable chemicals. In the process, inexhaustible solar energy can be fully utilized as an energy source, so that the problems of energy crisis and environmental pollutants can be effectively relieved. However, since the C = O double bond has a high bond energy, the carbon dioxide molecule exhibits a rather stable chemical property, so that the conventional photocatalytic material has a difficulty in having a good reduction activity for carbon dioxide. From a kinetic point of view, efficient activation of carbon dioxide by the material surface is generally considered to be a necessary condition to be able to drive the reduction of carbon dioxide. The activated carbon dioxide molecule initiates multiple electron reactions that reduce carbon dioxide, which may involve the transfer of an electron to the carbon dioxide molecule to form electronegative CO 2 * Species of the species. ByThe LUMO state in carbon dioxide is too high and thus transfer of an electron to a carbon dioxide molecule is thermodynamically difficult to achieve. The material can have the capability of providing high-concentration free electrons and the performance of enhancing the adsorption and activation of carbon dioxide molecules by doping high-valence metal ions and forming the defect state of oxygen-rich vacancies, and the activity of the final photocatalytic conversion reaction can be influenced to a certain extent, so that a new process for reducing carbon dioxide under the more environment-friendly and green conditions can be developed.
SnO 2 As a common n-type semiconductor material, the photocatalyst has the advantages of safety, no toxicity and higher chemical stability, and is a green and environment-friendly photocatalyst. But due to SnO 2 Has wider band gap, and can excite the separation of electron-hole pairs under the irradiation of ultraviolet light and generate the electron-hole pairs through optical excitation, so that the electron-hole pairs are easy to recombine, which greatly reduces SnO 2 The light energy utilization rate and the catalytic performance of the catalyst. SnO doped by high valent metal ions 2 The nano material solves the problem of the existing undoped SnO 2 The nanometer material is difficult to activate carbon dioxide and has low efficiency of photocatalytic reduction of carbon dioxide, and has important scientific and practical significance in the field of carbon neutralization.
Disclosure of Invention
The invention aims to provide high-valence metal ion doped SnO 2 Nanometer material and preparation method and application thereof, and realizes nanometer SnO by means of high-valence metal ion doping 2 The regulation of the defect type of the oxide and the surface activation enable the surface of the material to have the capability of activating carbon dioxide. The high valence metal ion is doped with SnO 2 The nano material has excellent photocatalytic degradation performance, and the efficiency of photocatalytic reduction of carbon dioxide under the illumination condition is obviously superior to that of undoped SnO 2 The material solves the existing SnO 2 The nanometer material has poor photocatalytic performance, and can be directly applied to the fields of photocatalytic carbon fixation, pollutant degradation in the environment and the like.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
high-valence metal ion doped SnO 2 Nano material, high priceDoping of metal ions into SnO 2 Partial crystal lattice makes the surface of the material possess the capacity of activating carbon dioxide. The high valence metal ions are one or more of niobium, tantalum, vanadium, tungsten and molybdenum elements.
In the nano material, the atom percentage content of the high valence metal ions is 10-30%.
The high-valence metal ion doped SnO 2 The nanometer material with size less than 1 micron is rutile phase structure.
The high valence metal ion doped SnO 2 The preparation method of the nano material comprises the following steps:
(1) Preparing a reaction precursor: firstly, respectively preparing an ammonium salt solution and a mixed salt solution, wherein the mixed salt solution is a solution containing high-valence metal ions and tin ions, the concentration of ammonium ions in the ammonium salt solution is 0.05-0.24mol/L, and the total concentration of the high-valence metal ions and the tin ions in the mixed salt solution is 0.01-0.8mol/L; and dropwise adding the ammonium salt solution into the mixed salt solution under the stirring condition, and fully stirring to obtain a reaction precursor.
(2) Crystallization reaction: after adjusting a proper pH value, blowing nitrogen for 30min, and then preserving heat for 20-48h at the temperature of 140-230 ℃ to obtain a suspension;
(3) Washing and drying: centrifugally separating the suspension obtained in the step (2), washing the separated powder for 3-5 times by using secondary deionized water, and drying the washed powder for 8-24h at the temperature of 50-80 ℃ to obtain the high-valence metal ion doped SnO 2 And (3) nano materials.
In the step (1), the ammonium salt solution is a solution prepared from ammonium nitrate or ammonium carbonate, the solvent can be alcohol, water and a mixed system of alcohol and water, and the alcohol is one or more of ethanol, ethylene glycol and tert-butyl alcohol; the volume ratio of the ammonium salt solution to the mixed salt solution is controlled to be 1:2.
The high-valence metal ion doped SnO 2 The nano material can be directly used for photocatalytic reduction of carbon dioxide or degradation of organic pollutants in water.
The high-valence metal ion doped SnO 2 The process of applying the nano material to photocatalytic reduction of carbon dioxide comprises the following steps: dispersing the material in water solution containing carbon dioxide, and reducing carbon dioxide into carbon-containing products such as methanol, formaldehyde, formic acid, ethanol, acetaldehyde and acetic acid under illumination for 2-24 hr.
The high-valence doped nano photocatalytic material prepared by the invention is used as a catalyst for photocatalytic reduction of carbon dioxide to obtain a carbon-containing product. The process of applying the photocatalytic material to photocatalytic reduction of carbon dioxide specifically comprises the following steps:
the photocatalytic material is placed in a carbon dioxide water solution containing triethanolamine, and is kept for 30min under the condition of no light and then is kept for 2-24h under the condition of light, so that carbon dioxide is reduced into carbon-containing products such as methanol, formaldehyde, formic acid, ethanol, acetaldehyde, acetic acid and the like.
In the application process, the usage amount of the photocatalytic material is more than 0.02g/m 3 And the concentration of triethanolamine in the solution is 2-20vol.%.
The technical principle of the invention is as follows:
the invention uniformly dopes high-valence metal ions in a tin dioxide bulk phase, and the high-valence metal ions replace Sn under no illumination 4+ The form of the carbon dioxide molecule enters the crystal lattice, a positively charged center is formed on the surface of the crystal lattice, a lone pair of electrons on a carbon atom in the carbon dioxide molecule carries certain negative charge, the electrostatic attraction between the negative charge and the positively charged center formed by doping the high-valence metal on the surface of the tin dioxide probably promotes the adsorption of the carbon dioxide molecule on the surface of a sample, and the generated high-concentration free electrons activate the carbon dioxide molecule to generate electronegative CO 2 * The species immediately reduces the carbon dioxide by multiple electrons under the illumination condition to obtain single-carbon and double-carbon products such as formaldehyde, acetaldehyde, acetic acid and the like, solves the problem of poor adsorption effect of the carbon dioxide and a photocatalyst in the current process of photocatalytic reduction of the carbon dioxide by simulating artificial photosynthesis, and achieves the aim of improving the photocatalytic reaction efficiency.
The invention has the advantages that:
1. the invention prepares high-valence metal ion doped SnO 2 The nano material solves the problem that the adsorption force of carbon dioxide and a photocatalyst is poor in the process of reducing carbon dioxide by using the existing tin dioxide-based material.
2. The high-valence metal ion doped SnO prepared by the invention 2 The material overcomes the defect that noble metal is required to be used as a cocatalyst in the common process of photocatalytic reduction of carbon dioxide.
3. The high-valence metal ion doped SnO prepared by the invention 2 The nanomaterials can reduce carbon dioxide to single and dual carbon products.
4. The high-valence metal ion doped SnO prepared by the invention 2 The rate of degrading RhB of the nano material in one hour reaches 98 percent
Description of the drawings:
FIG. 1 is a graph comparing the X-ray diffraction results of the niobium-doped tin dioxide nanomaterial of example 1 and the pure tin dioxide nanomaterial of comparative example 1.
FIG. 2 is a graph showing the degradation of niobium doped tin dioxide dyes of example 1 and comparative example 1.
FIG. 3 is a graph comparing the niobium doped tin dioxide nanomaterial of example 1 and the product of the reduction of carbon dioxide by light without the addition of a catalyst.
The specific implementation mode is as follows:
the invention is further described with reference to the following figures and examples:
example 1
The photocatalytic material prepared in this embodiment is a niobium element bulk-doped tin dioxide nanomaterial, and the specific process is as follows:
(1) Preparing a reaction precursor: firstly, preparing 0.24mol/L ammonium carbonate salt solution; then preparing a mixed salt solution containing stannous chloride and niobium pentachloride, wherein the concentration of the stannous chloride in the mixed salt solution is 0.08 mol/L, the concentration of the niobium pentachloride is 0.04mol/L, and the solvent is water; dropwise adding an ammonium carbonate salt solution into the mixed salt solution under the stirring condition, and fully stirring to obtain a reaction precursor, wherein the volume ratio of the ammonium carbonate salt solution to the mixed salt solution is 1:2.
(2) And (3) crystallization reaction: the ammonium reaction precursor prepared in the step (1) is added with nitrogen for 30min after the pH value is adjusted to be =2, and then the temperature is kept for 48h at 230 ℃ to obtain suspension;
(3) Washing and drying: centrifugally separating the suspension obtained in the step (2), washing the separated powder for 3-5 times by using secondary deionized water, and drying the washed powder for 8-24h at the temperature of 50-80 ℃ to obtain the high-valence metal ion doped SnO 2 And (3) nano materials.
Comparative example 1
The nano photocatalytic material prepared by the embodiment is a pure tin dioxide nano material, and the specific process is as follows:
(1) Firstly, respectively preparing 0.24mol/L ammonium carbonate salt solution and 0.12mol/L stannous chloride salt solution, dropwise adding the ammonium carbonate salt solution into the stannous chloride salt solution under the stirring condition, and fully stirring to obtain a reaction precursor, wherein the volume ratio of the ammonium carbonate salt solution to the stannous chloride salt solution is 1:2.
(2) Crystallization reaction: the precursor solution prepared in the step (1) is subjected to pH =2 adjustment, nitrogen is blown for 30min, and then heat preservation is carried out for 48h at 230 ℃ to obtain suspension;
(3) Washing and drying: centrifugally separating the suspension obtained in the step (2), washing the separated powder for 3-5 times by using secondary deionized water, and drying the washed powder for 8-24h at the temperature of 50-80 ℃ to obtain the high-valence metal ion doped SnO 2 And (3) nano materials.
FIG. 1 is a graph comparing the X-ray diffraction results of 20at.% niobium doped tin dioxide nanomaterial prepared in example 1 and the pure tin dioxide nanomaterial prepared in comparative example 1, and it can be seen that all samples in example 1 are in the rutile phase, indicating that the niobium is incorporated into the crystal lattice of the rutile phase tin dioxide in a doped form.
Comparing the XRD results of example 1 and comparative example 1 shows that when Nb is added 5+ After doping, the rutile phase tin dioxide lattice expands more significantly, causing the diffraction peak to shift to a lower angle.
Example 2
The photocatalytic material prepared in the example 1 is used for photocatalytic degradation of rhodamine B, and the specific process is as follows:
(1) 25mg of the powder obtained in example 1 were ultrasonically dispersed in 25ml of rhodamine B (RhB) =10ppm aqueous solution, resulting in a suspension. Transferring the suspension into a photocatalytic reactor, stirring in the dark for 30min with a magnetic stirrer, and irradiating with light under a 300W xenon lamp with visible spectrum and intensity of 45mW/cm 2 And (5) visible light illumination is performed for 1h.
(2) After the light irradiation is finished, taking supernatant to measure the concentration of remaining rhodamine B (RhB) in the solution.
Comparative example 2
The photocatalytic material prepared in the comparative example 1 is used for photocatalytic degradation of rhodamine B, and the specific process is the same as that in the example 2.
Comparison of the dye degradation results of example 2 and comparative example 2 shows that the efficiency of degrading rhodamine B by Nb-doped tin dioxide after 1h of visible light irradiation is significantly improved compared with pure phase tin dioxide (fig. 2).
Example 3
The photocatalytic material prepared in example 1 is used for photocatalytic reduction of carbon dioxide, and the specific process is as follows:
1. 8ml of triethanolamine and 72ml of water were added to the Nb-doped tin dioxide material obtained in example 1, followed by ultrasonic dispersion for 15min to obtain a reaction solution.
2. Adding the prepared reaction liquid into a photocatalytic reactor, introducing carbon dioxide at the flow rate of 50-80ml/min for 30min, adsorbing for 30min under the non-illumination condition, and irradiating the reaction liquid for 24h by using a xenon lamp.
Comparative example 3
1. Only 8ml of triethanolamine and 72ml of water were added without adding the catalyst material of example 1, followed by ultrasonic dispersion for 15min to prepare a reaction solution.
2. Adding the prepared reaction liquid into a photocatalytic reactor, introducing carbon dioxide at the flow rate of 50-80ml/min for 30min, adsorbing for 30min under the non-illumination condition, and irradiating the reaction liquid for 24h by using a xenon lamp.
FIG. 3 is a graph comparing the production of carbon dioxide by the reduction of niobium doped tin dioxide nanomaterials and light without the addition of niobium catalyst in the experiments of example 3 and comparative example 3. It can be seen that the niobium doped tin dioxide photocatalytic material is capable of converting carbon dioxide to single and double carbon products, formaldehyde, acetaldehyde and acetic acid, whereas pure tin dioxide material has no product formation.

Claims (5)

1. High-valence metal ion doped SnO 2 The application of the nano material is characterized in that: the high-valence metal ion doped SnO 2 The nano material is directly used for photocatalytic reduction of carbon dioxide;
the nano material is SnO doped with high-valence metal ions 2 Nano material, high valence metal ion doped into SnO 2 Partial crystal lattices enable the surface of the material to have the capability of activating carbon dioxide; the high-valence metal ions are one or more of elements of niobium, tantalum, vanadium, tungsten and molybdenum;
in the nano material, the atom percentage content of high valence metal ions is 10-30%;
the preparation method of the nano material comprises the following steps:
(1) Preparing a reaction precursor: firstly, respectively preparing an ammonium salt solution and a mixed salt solution, wherein the mixed salt solution is a solution containing high-valence metal ions and tin ions, the concentration of ammonium radicals in the ammonium salt solution is 0.05-0.24mol/L, and the total concentration of the high-valence metal ions and the tin ions in the mixed salt solution is 0.01-0.8mol/L; dropwise adding an ammonium salt solution into the mixed salt solution under the stirring condition, and fully stirring to obtain a reaction precursor;
(2) Crystallization reaction: after adjusting a proper pH value, blowing nitrogen for 30min for the reaction precursor prepared in the step (1), and then preserving heat for 20-48h at the temperature of 140-230 ℃ to obtain a suspension;
(3) Washing and drying: centrifugally separating the suspension obtained in the step (2), washing the separated powder for 3-5 times by using secondary deionized water, and drying the washed powder for 8-24h at the temperature of 50-80 ℃ to obtain the high-valence metal ion doped SnO 2 And (3) nano materials.
2. Height according to claim 1Valence metal ion doped SnO 2 The application of the nano material is characterized in that: the SnO 2 The nanometer material has a size smaller than 1 micron and has a rutile phase structure.
3. High-valence metal ion-doped SnO according to claim 1 2 The application of the nano material is characterized in that: in the step (1), the ammonium salt solution is a solution prepared from ammonium nitrate or ammonium carbonate, a solvent is alcohol and/or water, and the alcohol is one or more of ethanol, ethylene glycol and tert-butyl alcohol.
4. High valence metal ion doped SnO according to claim 1 2 The application of the nano material is characterized in that: in the step (1), the volume ratio of the ammonium salt solution to the mixed salt solution is 1:2.
5. High valence metal ion doped SnO according to claim 1 2 The application of the nano material is characterized in that: the high valence metal ion doped SnO 2 The process of applying the nano material to photocatalytic reduction of carbon dioxide comprises the following steps: dispersing the material in water solution containing carbon dioxide, and reducing carbon dioxide into methanol, formaldehyde, formic acid, ethanol, acetaldehyde and acetic acid under illumination for 2-24 hr.
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