CN113443650A - Method for preparing nano titanate by utilizing self-release of crystal water - Google Patents
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- B82Y40/00—Manufacture or treatment of nanostructures
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/74—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing arsenic, antimony or bismuth
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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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.
According to the technical scheme, the nano-titanate obtained in the step (4) is ground into powder, then the powder is placed in a muffle furnace, the temperature is gradually increased to 500-1000 ℃ at the rate of 4 ℃ per minute in the air atmosphere, the temperature is kept for 60-180 min, then the powder is cooled to room temperature along with the furnace, and grinding is carried out 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 released automatically to serve as a water source for titanium hydrolysis, and simultaneously, 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 lamella with the average thickness of less than 10 nm 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 invention12TiO20A Transmission Electron Microscope (TEM) image of the sample;
FIG. 4 shows Bi prepared in example 1 of the present invention12TiO20An 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 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 of ethylene glycol is weighed and poured into a beaker, and 16.296 g of Bi (NO) are respectively weighed according to the stoichiometric ratio of Bi to Ti (12: 1)3)3·5H2O and 1 mL C16H36O4Ti 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 ℃ under 800W for 120min to obtain a turbid solution, and centrifuged to obtain a precipitate. And washing the precipitate for 3 times by using deionized water and ethanol respectively, then putting the precipitate into a 60 ℃ oven for drying, and fully grinding the precipitate for 1 hour to obtain precursor powder. The precursor powder is flatly laid in a crucible, the crucible is placed in a muffle furnace, and the temperature is raised to 600 ℃ at the rate of 4 ℃ per minute in the air atmosphere and is kept for 2 hours. Cooling to room temperature along with the furnace to obtain Bi12TiO20Yellow 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) SEM spectrogram of a sample at 550 ℃; (d) SEM spectrogram of a sample at 600 ℃; (e) SEM spectrogram 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 example12TiO20And (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 example12TiO20Energy spectrum analysis (EDS) profile of the sample, canThe ratio of Bi element to Ti element in the element ratio is close to 12:1, it was confirmed that the prepared sample was Bi12TiO20And (4) phase(s).
Referring to fig. 5, it is an X-ray diffraction pattern of nano-titanate prepared in this example; (a) is Bi12TiO20An X-ray powder diffraction pattern of the sample; (b) is alpha-Bi2O3Diffraction peak magnifications at 26.9 ° and 28.0 °; (c) is alpha-Bi2O3Diffraction peak magnifications at 33.0 ° and 33.2 °; (d) bi at 600 DEG C12TiO20Refining the X-ray diffraction spectrum of the sample; the X-ray diffraction pattern shows that: when the temperature rises to 600 ℃, monoclinic phase alpha-Bi2O3The corresponding diffraction peak disappears completely, and the cubic phase pure phase Bi is proved to be obtained12TiO20. 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 C12TiO20The lowest temperature of (c).
Referring to fig. 6, 7 and 8, there are graphs illustrating the photocatalytic performance effect of nano-titanate provided in this embodiment, respectively, wherein fig. 6 is Bi12TiO20Degrading 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 catalyst has the best catalytic degradation effect at 600 ℃, and the degradation rate of the organic dye methyl orange MO can reach 96.43% at 120 min.
Example 2
100 mL of ethylene glycol is measured and poured into a beaker, and (0.01-x) mol of La (NO) is weighed according to the stoichiometric ratio3)3·6H2O 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 La to Ti of 1:116H36O4Ti and stirring is continued until the solution is clear. Pouring the solution into a three-neck flask, and carrying out microwave heating for 30 min at 180 ℃ under 800W to obtain a turbid solution. For turbidityAnd centrifuging the solution to obtain precipitates, respectively washing 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 La2Ti2O7: xTb3+Sample powder.
Example 3
100 mL of glycerol was measured and poured into a beaker, and (0.01-x) mol of La (NO) was weighed in a stoichiometric ratio3)3·6H2O 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 of the La to the Ti element of 1:136O4And 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. Pouring the solution into a three-neck flask, and carrying out microwave heating for 30 min at 180 ℃ under 800W to obtain a turbid 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 La2Ti2O7: xTb3+Sample powder.
Claims (3)
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) 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.
2. The method for preparing nano titanate by using crystal water self-release as claimed in claim 1, wherein: the organic alcohol solvent comprises one of ethylene glycol, n-butanol, glycerol and polyethylene glycol.
3. The method for preparing nano titanate by using crystal water self-release as claimed in claim 1, wherein: and (3) grinding the nano titanate obtained in the step (4) into powder, then placing the powder in a muffle furnace, gradually heating to 500-1000 ℃ 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.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115321488A (en) * | 2022-06-30 | 2022-11-11 | 苏州大学 | Method for preparing self-dispersed nano metal oxide |
| CN115611300A (en) * | 2022-08-09 | 2023-01-17 | 南京大学 | Method for preparing hydrotalcite in one step without solvent |
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| CN102351242A (en) * | 2011-08-17 | 2012-02-15 | 南京师范大学 | Solvent-thermal method for preparing single-phase bismuth titanate Bi2Ti2O7 |
| CN103611480A (en) * | 2013-12-06 | 2014-03-05 | 河南师范大学 | Method for preparing homogenesis yolk-shell structure titanium dioxide microsphere |
| CN104445382A (en) * | 2014-12-03 | 2015-03-25 | 北方民族大学 | Method for preparing Bi12TiO20 nano-powder by virtue of microwave-assisted sol-gel method |
| CN112480917A (en) * | 2020-12-14 | 2021-03-12 | 苏州美纳福健康科技有限公司 | Europium-doped zinc orthotitanate red fluorescent powder with hexagonal prism morphology and preparation method thereof |
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- 2021-07-12 CN CN202110786466.9A patent/CN113443650B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102351242A (en) * | 2011-08-17 | 2012-02-15 | 南京师范大学 | Solvent-thermal method for preparing single-phase bismuth titanate Bi2Ti2O7 |
| CN103611480A (en) * | 2013-12-06 | 2014-03-05 | 河南师范大学 | Method for preparing homogenesis yolk-shell structure titanium dioxide microsphere |
| CN104445382A (en) * | 2014-12-03 | 2015-03-25 | 北方民族大学 | Method for preparing Bi12TiO20 nano-powder by virtue of microwave-assisted sol-gel method |
| CN112480917A (en) * | 2020-12-14 | 2021-03-12 | 苏州美纳福健康科技有限公司 | Europium-doped zinc orthotitanate red fluorescent powder with hexagonal prism morphology and preparation method thereof |
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| Title |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115321488A (en) * | 2022-06-30 | 2022-11-11 | 苏州大学 | Method for preparing self-dispersed nano metal oxide |
| CN115321488B (en) * | 2022-06-30 | 2023-10-27 | 苏州大学 | Method for preparing self-dispersion nano metal oxide |
| CN115611300A (en) * | 2022-08-09 | 2023-01-17 | 南京大学 | Method for preparing hydrotalcite in one step without solvent |
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