CN113443650B - Method for preparing nano titanate by utilizing self-release of crystal water - Google Patents
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Abstract
The invention relates to a method for preparing nano titanate by utilizing self-release of crystal water. Dissolving a titanium source in a solvent, adding metal and non-metal salt containing crystal water according to a target product, and fully dissolving to form a uniform system; promoting the crystal water of the salt to be released automatically under the assistance of microwave uniform heating, and realizing the uniform hydrolysis of the titanium source and the in-situ doping of the metal oxide; centrifuging the precipitate, washing with water and alcohol for several times, and vacuum drying to obtain nanometer titanate; and further carrying out high-temperature grinding treatment to obtain nano titanate powder. According to the method, crystal water of the salt is automatically released to serve as a water source for titanium hydrolysis, and meanwhile, metal hydroxide generated during water release reacts with high-activity primary titanium to prepare the nano titanate with small size and uniform appearance in situ. The technical scheme of the invention has the advantages of simple and rapid preparation process, high yield, low energy consumption, short reaction time, relatively low reaction temperature and the like, and is favorable for industrial production and application.
Description
Technical Field
The invention belongs to the technical field of material preparation and application, and relates to a method for preparing nano titanate by self-releasing of crystal water.
Background
Titanate as a functional material has unique microstructure and a plurality of special properties, and has important significance in industrial application. At present, the solid phase sintering technology is mainly adopted for preparing titanate in the prior art, but the method is difficult to obtain a product with high purity and uniform grain size. To solve this problem, researchers have proposed the use of homogeneous co-precipitation methods to prepare titanate materials. However, the titanium source is very sensitive to water source, the hydrolysis process is severe, and the process of firstly hydrolyzing to generate a precipitator and then uniformly coprecipitating cannot be met. This either fails to control the rate of hydrolysis of the titanium source, resulting in a product that is prone to agglomeration and non-uniform in size, or fails to complete the bonding of the reaction materials at the molecular level, thereby affecting the quality of the product. Therefore, it is of great significance to find a precipitant suitable for the uniform coprecipitation process of preparing titanate.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a method for preparing nano titanate by utilizing crystal water self-release, which is a coprecipitation method with green and environment-friendly production process, simplicity, high efficiency, uniform product size and low cost, and can be used for preparing nano titanate photocatalyst and titanate fluorescent material.
The technical scheme for realizing the aim of the invention is to provide a method for preparing nano titanate by utilizing crystal water self-release, which comprises the following steps:
(1) Dissolving one of tetrabutyl titanate and titanium tetrachloride serving as a titanium source in an organic alcohol solvent with the boiling point higher than 100 ℃ to prepare a titanium source stock solution with the concentration of 0.1-1.0 mol/L;
(2) Dissolving metal salt and non-metal salt containing crystal water in a titanium source stock solution to obtain a precursor; the non-metal salt containing crystal water is one of hydrazine hydrate, oxalic acid dihydrate and citric acid monohydrate; the metal salt containing the crystal water is soluble salt containing the crystal water of pentahydrate or more;
(3) Placing the precursor obtained in the step (2) in a microwave reactor, and reacting for 30-120 min under the conditions that the power is 500-1000W and the temperature is 110-200 ℃ to obtain a precipitate;
(4) And (4) centrifuging the precipitate, washing with water and alcohol for several times, and drying in vacuum to obtain the nano titanate.
The organic alcohol solvent comprises one of ethylene glycol, n-butyl alcohol, glycerol and polyethylene glycol.
In the technical scheme of the invention, the nano titanate obtained in the step (4) is ground into powder, then is placed in a muffle furnace, is gradually heated to 500-1000 ℃ at the rate of 4 ℃ per minute in the air atmosphere, is cooled to room temperature along with the furnace after heat preservation treatment is carried out for 60-180 min, and is ground to obtain the nano titanate powder.
The invention is based on the principle that: the nature of the crystal water is water molecules bound in the compound, and at normal temperature, the crystal water exists in the crystal and forms a coordination compound with other components. When the temperature rises, crystal water is slowly separated out, which is quite similar to the process of slowly generating a precipitator in a uniform coprecipitation method; the crystal water which is precipitated slowly can well play a role in controlling the hydrolysis rate of the titanium source, which is also against the original intention of controlling the reaction speed. In view of the above, the present invention provides a method of a self-releasing crystal water assisted uniform coprecipitation method, in which a salt compound containing crystal water is simultaneously used as a water source and a metal cation source, and in a heating process, the compound containing crystal water slowly releases crystal water to promote hydrolysis of a titanium source and a hydrogen oxidation reaction of metal cations to be simultaneously performed on a molecular layer, thereby obtaining titanate through a uniform coprecipitation process. In order to promote the reaction, microwave heating is assisted in the uniform coprecipitation process, so that reactants are uniformly heated, and the preparation period is greatly shortened.
The invention overcomes the problems of strict and harsh preparation conditions of nano titanate, long reaction time, complex process and the like which are not beneficial to wide application, and provides a novel green and environment-friendly simple, efficient and uniform coprecipitation method with low cost. The method utilizes the crystal water self-release of the salt as the water source for titanium hydrolysis, and simultaneously the metal hydroxide generated during the water release reacts with the high-activity nascent titanium to prepare the nano titanate with small size and uniform appearance in situ.
Compared with the prior art, the invention has the beneficial effects that: the crystal water of the salt is automatically released to serve as a water source for titanium hydrolysis, and meanwhile, metal hydroxide generated during water release reacts with high-activity primary titanium to prepare nano titanate with small size and uniform appearance in situ; the method has the advantages of simple and rapid preparation process, high yield, low energy consumption, short reaction time, relatively low reaction temperature and the like, and is favorable for industrial production and application. The nanometer titanate sheet layer with the average thickness of less than 10nm is obtained, the morphology is uniform, and the dispersibility is good. The titanate prepared by the preparation method has an ultra-large specific surface area, and excellent catalytic performance and fluorescence performance.
Drawings
FIG. 1 is a scanning electron microscope image of the product obtained in each step of the process of preparing nano-titanate in example 1 of the present invention;
FIG. 2 is an SEM magnified view of a sample prepared at a solid phase sintering temperature of 600 ℃ in example 1 of the present invention;
FIG. 3 shows Bi prepared in example 1 of the present invention 12 TiO 20 A Transmission Electron Microscope (TEM) image of the sample;
FIG. 4 shows Bi prepared in example 1 of the present invention 12 TiO 20 An energy spectrum analysis (EDS) profile of the sample;
FIG. 5 is an X-ray diffraction pattern of nano-titanate prepared in example 1 of the present invention;
fig. 6, 7 and 8 are graphs showing the photocatalytic performance of the nano-titanate prepared in example 1 of the present invention.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
The technical solution of the present invention is further described with reference to the accompanying drawings and specific embodiments.
Example 1
100 mL glycol is measured and poured into a beaker, and 16.296 g Bi (NO) is weighed according to the stoichiometric ratio of 12 3 ) 3 ·5H 2 O and 1 mL C 16 H 36 O 4 Ti and they were slowly added to ethylene glycol and stirred to form a clear solution. Subsequently, the above solution was poured into a three-necked flask, heated by microwave at 150 ℃ for 120min at 800W to give a turbid solution, and centrifuged to give a precipitate. Washing the precipitate with deionized water and ethanol for 3 times respectively, drying in a 60 ℃ oven, and fully grinding to 1 h to obtain precursor powder. Spreading the precursor powder in a crucible, placing the crucible in a muffle furnace, and heating at 4 deg.C per minute in air atmosphereAt a rate of 600 ℃ and held at that temperature for 2 hours. Cooling to room temperature along with the furnace to obtain Bi 12 TiO 20 Yellow powder. The product was ground and stored in a desiccator.
Referring to fig. 1, which is a scanning electron microscope image of a product obtained in each step in the preparation process of this example, wherein (a) is an SEM spectrogram of a precursor; (b) preparing a sample SEM spectrogram by a solid-phase sintering method; (c) is SEM spectrogram of a sample at 550 ℃; (d) SEM spectrogram of a sample at 600 ℃; (e) SEM spectrum of 650 deg.C sample;
referring to fig. 2, it is an SEM magnified view of a sample prepared at 600 ℃ in this example, and it can be seen that the sample has a nano-scale sheet structure.
Referring to FIG. 3, bi prepared in this example 12 TiO 20 And (3) a Transmission Electron Microscope (TEM) image of the sample, wherein the sample is of a nanoscale lamellar structure.
Referring to FIG. 4, bi prepared in this example 12 TiO 20 The energy spectrum analysis (EDS) chart of the sample shows that the ratio of Bi element to Ti element in the element ratio is close to 12:1, it was confirmed that the prepared sample was Bi 12 TiO 20 And (4) phase.
Referring to fig. 5, it is an X-ray diffraction pattern of nano-titanate prepared in this example; (a) Is Bi 12 TiO 20 An X-ray powder diffraction pattern of the sample; (b) Is alpha-Bi 2 O 3 Diffraction peak magnifications at 26.9 ° and 28.0 °; (c) Is alpha-Bi 2 O 3 Diffraction peak magnifications at 33.0 ° and 33.2 °; (d) Bi at 600 DEG C 12 TiO 20 Refining the X-ray diffraction spectrum of the sample; the X-ray diffraction pattern shows that: when the temperature rises to 600 ℃, monoclinic phase alpha-Bi 2 O 3 The corresponding diffraction peak disappears completely, and the cubic phase pure phase Bi is proved to be obtained 12 TiO 20 . The map is completely matched with the JCPDS card number PDF #78-1158 map. The temperature was further raised to 650 ℃ and no new diffraction peak was generated in the sample. XRD result proves that pure phase Bi is obtained for preparation at 600 DEG C 12 TiO 20 The lowest temperature of (c).
See FIGS. 6, 7 and 8, respectivelyThe photocatalytic performance effect graph of nano titanate provided in this example is shown in fig. 6, which is Bi 12 TiO 20 Degrading the ultraviolet-visible absorption spectrogram of the MO aqueous solution by the sample under the irradiation of visible light; FIG. 7 is a graph comparing degradation rate curves for different samples; figure 8 is a graph of degradation kinetics for different samples. The result shows that the best catalytic degradation effect is achieved at 600 ℃, and the degradation rate of the organic dye methyl orange MO can reach 96.43% at 120 min.
Example 2
100 mL ethylene glycol is measured and poured into a beaker, and (0.01-x) mol of La (NO) is weighed according to the stoichiometric ratio 3 ) 3 ·6H 2 O and xmol Tb (NO) 3 ) 3 (x = 0.005) and added to ethylene glycol and stirred well. Dropwise adding 0.01mol C into the solution according to the stoichiometric ratio of the La to the Ti of 1:1 16 H 36 O 4 Ti and stirring was continued until the solution was clear. The solution was poured into a three-necked flask and heated by microwave at 180 ℃ and 800W for 30 min to obtain a cloudy solution. And centrifuging the turbid solution to obtain precipitates, respectively cleaning the precipitates for 3 times by using deionized water and absolute ethyl alcohol, then putting the precipitates into a 60 ℃ drying oven for drying, and fully grinding to obtain precursor powder. And heating the precursor powder to 900 ℃ at the heating rate of 4 ℃ per minute in a reducing atmosphere, and preserving the heat for 3 hours. Naturally cooling to room temperature to obtain La 2 Ti 2 O 7 : xTb 3+ Sample powder.
Example 3
100 mL glycerol is measured and poured into a beaker, and (0.01-x) mol of La (NO) is weighed according to the stoichiometric ratio 3 ) 3 ·6H 2 O and xmol Tb (NO) 3 ) 3 (x = 0.005) and added to glycerol and stirred well. 0.01mol C16H is dropwise added into the solution according to the stoichiometric ratio 1:1 of La and Ti elements 36 O 4 And Ti, slowly adding a small amount of hydrazine hydrate into the solution to adjust the pH value to 9-10, and continuing stirring until the solution is clear. The solution was poured into a three-necked flask and heated by microwave at 180 ℃ and 800W for 30 min to obtain a cloudy solution. Centrifuging the turbid solution to obtainAnd (3) precipitating, washing the precipitate for 3 times by using deionized water and absolute ethyl alcohol respectively, then putting the precipitate into a 60 ℃ oven for drying, and fully grinding to obtain precursor powder. And heating the precursor powder to 900 ℃ at the heating rate of 4 ℃ per minute in a reducing atmosphere, and preserving the heat for 3 hours. Naturally cooling to room temperature to obtain La 2 Ti 2 O 7: xTb 3+ Sample powder.
Claims (1)
1. A method for preparing nano titanate by utilizing crystal water self-release is characterized by comprising the following steps:
(1) Dissolving one of tetrabutyl titanate and titanium tetrachloride serving as a titanium source in an organic alcohol solvent with the boiling point higher than 100 ℃ to prepare a titanium source stock solution with the concentration of 0.1-1.0 mol/L;
(2) Dissolving metal salt and non-metal salt containing crystal water in a titanium source stock solution to obtain a precursor; the non-metal salt containing crystal water is one of hydrazine hydrate, oxalic acid dihydrate and citric acid monohydrate; the metal salt containing the crystal water is soluble salt containing the crystal water of pentahydrate or more;
(3) Putting the precursor obtained in the step (2) into a microwave reactor, and reacting for 30-120 min under the conditions that the power is 500-1000W and the temperature is 110-150 ℃ to obtain a precipitate;
(4) Centrifuging the precipitate, washing with water and alcohol for several times, and vacuum drying to obtain nanometer titanate;
the organic alcohol solvent comprises one of ethylene glycol, n-butyl alcohol, glycerol and polyethylene glycol;
grinding the nano titanate obtained in the step (4) into powder, then placing the powder in a muffle furnace, gradually heating to 650-1000 ℃ at the rate of 4 ℃ per minute in the air atmosphere, carrying out heat preservation treatment for 60-180 min, then cooling to room temperature along with the furnace, and grinding to obtain nano titanate powder;
the nano titanate powder is in a nano scale lamellar structure, and the average thickness is less than 10 nm.
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