CN110550656A - Preparation method of three-phase mixed nano TiO 2 - Google Patents
Preparation method of three-phase mixed nano TiO 2 Download PDFInfo
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- CN110550656A CN110550656A CN201910914944.2A CN201910914944A CN110550656A CN 110550656 A CN110550656 A CN 110550656A CN 201910914944 A CN201910914944 A CN 201910914944A CN 110550656 A CN110550656 A CN 110550656A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
- C01G23/0536—Producing by wet processes, e.g. hydrolysing titanium salts by hydrolysing chloride-containing salts
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C01P2006/00—Physical properties of inorganic compounds
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Abstract
A preparation method of three-phase mixed type nano TiO 2 comprises the steps of (a) hydrolyzing titanium tetrachloride to obtain a titanium oxychloride compound, (b) adding zirconium oxychloride octahydrate powder into the prepared titanium oxychloride solution to form a mixed solution, wherein the molar ratio of the added zirconium oxychloride to the titanium oxychloride is 1.23: 100-1.65: 100, (c) transferring the formed mixed solution into a hydrothermal reaction kettle to react for 5-12 hours at 80-100 ℃ to obtain a nano TiO 2 precipitate, and (d) carrying out centrifugal purification, drying and calcination treatment at 400 ℃ on the obtained precipitate to obtain the three-phase mixed type TiO 2 nano powder, wherein the three-phase mixed type nano TiO 2 prepared by the method is small in grain size, good in thermal stability and high in specific surface area, and has a very wide application prospect in the field of industrial catalysis.
Description
Technical Field
The invention relates to the field of functional materials, in particular to a preparation method of three-phase mixed nano TiO 2.
Background
The titanium dioxide (TiO 2) also called titanium dioxide has quite stable chemical property, is widely applied and occupies an extremely important position in the field of chemical production, since TiO 2 is commercially produced in the early twentieth century, the titanium dioxide is widely applied to the fields of pigment coatings, cosmetics, ceramics and the like due to the advantages of excellent activity, selectivity, poisoning resistance, high-temperature reducibility and the like, more new applications are revealed along with the discovery of the surface effect, the volume effect, the quantum size effect, the macroscopic tunnel effect and other properties of a TiO 2 nano material, and the nano TiO 2 is a new growth point of the titanium industry, so that the production of the nano TiO 2 is bound to go to the industrialized road due to the wide excellent properties and the high profit and has bright prospect.
The TiO 2 has three crystal structures, namely rutile, anatase and brookite, wherein anatase TiO 2 has good catalytic performance but is unstable and is easy to be converted into rutile crystal form after high-temperature calcination, the rutile TiO 2 has low photocatalytic capacity but better physical and chemical stability, and research reports that the catalytic performance of the high-temperature stable mixed crystal TiO 2 is superior to that of a pure phase, because the anatase and brookite crystal forms are unstable and are easy to be converted into rutile after high-temperature calcination, in addition, the TiO 2 powder is easy to agglomerate among nano particles in the high-temperature calcination process, so that the size of the crystal particles is increased, and the specific surface area of the nano particles is greatly reduced, therefore, the high-temperature stable three-phase mixed nano TiO 2 is difficult to obtain.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a preparation method of three-phase mixed nano TiO 2, the prepared mixed nano TiO 2 powder has the advantages of three crystal phases of rutile, anatase and brookite due to small crystal grain size, large specific surface area, difficult sintering during high-temperature calcination and stable high-temperature performance, and the catalytic activity, the oxidation capacity and the chemical stability of the original TiO 2 catalyst can be improved when the mixed nano TiO 2 powder is used for industrial catalysis.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a preparation method of three-phase mixed nano TiO 2 comprises the following steps:
The method comprises the following steps: preparation of titanium oxychloride solution
Titanium tetrachloride is used as an initial raw material, 285-514g of deionized water is added into a 1L three-neck flask under the ice bath condition, 245g of titanium tetrachloride solution is added into the deionized water, magnetic stirring is carried out simultaneously, and nitrogen is continuously introduced into the three-neck flask to prepare the titanium oxychloride solution with the concentration of 2.0-3.6 mol/L.
Step two, preparing zirconium ion doped TiO 2 nano powder
Taking 50g of the solution, respectively adding 81.67-147.19g of deionized water and 0.27-0.66g of zirconium oxychloride octahydrate powder, enabling the molar ratio of zirconium ions to titanium ions to be (1.23-1.65): 100, uniformly mixing the solution, transferring the mixture into a closed hydrothermal reaction kettle, placing the reaction kettle in a vacuum oven, keeping the hydrothermal temperature at 80-100 ℃, reacting for 5-12h to obtain a precipitate TiO 2, cooling the reaction product and the reaction kettle, centrifugally separating the precipitate, sequentially washing the precipitate with distilled water and ethanol for 4-5 times, centrifugally treating the precipitate at 4000-5000rpm, removing supernatant, and finally drying the precipitate at 70 ℃ for 5-8h to obtain the nano TiO 2 powder.
Step three, preparation of three-phase mixed TiO 2 nano powder
And (3) calcining the TiO 2 nano powder prepared in the step two for 4-8h at 400 ℃ in a muffle furnace controlled by temperature programming in an air atmosphere to obtain rutile, anatase and brookite three-phase mixed TiO 2 nano powder, wherein the temperature rise rate of the calcination is 5 ℃/min.
Compared with the traditional method, the invention has the remarkable advantages that:
The anatase and the rutile phases are generated at low temperature, and then part of rutile is converted into the anatase and the brookite through relatively low temperature calcination, so that the formation of the three-phase mixed nano TiO 2 powder is favorably maintained, the high specific surface area of the powder is maintained, and the performance and the chemical stability of the powder in the fields of catalysis, water treatment and the like are improved.
The method has the advantages of low cost, low reaction temperature and good repeatability, the prepared mixed nano TiO 2 powder simultaneously has three crystal phases of rutile, anatase and brookite, the crystal size is small, the specific surface area is large (>60m 2/g), and sintering is not easy to occur after calcination at 400 ℃.
Drawings
Fig. 1 is a Scanning Electron Microscope (SEM) picture of the three-phase mixed nano TiO 2 powder prepared in example 1, wherein the scale is 200 nm.
Fig. 2 is a Scanning Electron Microscope (SEM) picture of the three-phase mixed nano TiO 2 powder prepared in example 1, wherein the scale is 500 nm.
Fig. 3 is an X-ray diffraction (XRD) pattern of the nano TiO 2 powder prepared in example 1 before and after calcination.
Detailed Description
The present invention will be further described with reference to the following examples.
example one
The embodiment comprises the following steps:
(1) Titanium tetrachloride was used as an initial raw material, 285g of deionized water was added to a 1L three-necked flask in an ice bath, and then 245g of a titanium tetrachloride solution was slowly added to the deionized water while magnetic stirring was performed, and nitrogen gas was continuously introduced into the three-necked flask to prepare a titanium oxychloride solution having a concentration of 3.6 mol/L.
(2) And (2) taking 50g of the titanium oxychloride solution prepared in the step (1), respectively adding 147.19g of deionized water and 0.49g of zirconium oxychloride octahydrate powder, enabling the molar ratio of zirconium ions to titanium ions to be 1.23:100, putting the uniformly mixed solution into a sealed hydrothermal reaction kettle, placing the reaction kettle in a vacuum oven, keeping the hydrothermal temperature at 100 ℃, reacting for 6 hours to obtain a precipitate TiO 2, cooling the reaction product and the reaction kettle, centrifugally separating the precipitate, washing the precipitate with distilled water and ethanol for 4-5 times in sequence, centrifuging the precipitate at the rotating speed of 4000rpm, and finally drying the precipitate at 70 ℃ for 5 hours to obtain the nano TiO 2 powder.
(3) calcining the prepared TiO 2 nano powder for 4 hours at 400 ℃ in an air atmosphere by adopting a muffle furnace with temperature programming control, thus obtaining the three-phase mixed TiO 2 nano powder, wherein the temperature raising rate of the calcination is 5 ℃/min.
FIGS. 1 to 3 show the data obtained under the above conditions, it can be seen that the TiO 2 nanopowder doped with zirconium ions is in the form of a two-phase mixed crystal of rutile and anatase (FIG. 3) without calcination, and after calcination at 400 deg.C, it is in the form of a three-phase mixed crystal of rutile, anatase and brookite (FIG. 3), and the crystal size thereof is 13.6nm, and the primary particles after calcination become uniform and large particles and maintain a porous structure, and the specific surface area after calcination is large, and the particles are uniformly dispersed, and the specific surface area is 60.9m 2/g (FIGS. 1 and 2).
Example two
The embodiment comprises the following steps:
(1) titanium tetrachloride was used as an initial raw material, 285g of deionized water was added to a 1L three-necked flask in an ice bath, and then 245g of a titanium tetrachloride solution was slowly added to the deionized water while magnetic stirring was performed, and nitrogen gas was continuously introduced into the three-necked flask to prepare a titanium oxychloride solution having a concentration of 3.6 mol/L.
(2) And (2) taking 50g of the titanium oxychloride solution prepared in the step (1), respectively adding 147.19g of deionized water and 0.60g of zirconium oxychloride octahydrate powder, enabling the molar ratio of zirconium ions to titanium ions to be 1.65:100, putting the uniformly mixed solution into a sealed hydrothermal reaction kettle, placing the reaction kettle in a vacuum oven, keeping the hydrothermal temperature at 90 ℃ and reacting for 6 hours to obtain a precipitate TiO 2, cooling the reaction product and the reaction kettle, centrifugally separating the precipitate, washing the precipitate with distilled water and ethanol for 4-5 times in sequence, centrifuging the precipitate at the rotating speed of 4000rpm, and finally drying the precipitate at 70 ℃ for 5 hours to obtain the nano TiO 2 powder.
(3) Calcining the prepared TiO 2 nano powder for 4 hours at 400 ℃ in an air atmosphere by adopting a muffle furnace with temperature programming control, thus obtaining the three-phase mixed TiO 2 nano powder, wherein the temperature raising rate of the calcination is 5 ℃/min.
the method has the advantages that the calcined TiO 2 nano powder still presents a good rutile, anatase and brookite three-phase mixed crystal form under the conditions of reducing the reaction temperature and increasing the concentration of doped zirconium ions, the primary particle morphology of the sample is still granular and porous, the grain size is 12.2nm, the specific surface area value is 67.7m 2/g, the sample is not easy to sinter at high temperature, and the stability is good.
EXAMPLE III
The embodiment comprises the following steps:
(1) titanium tetrachloride was used as an initial raw material, 285g of deionized water was added to a 1L three-necked flask in an ice bath, and then 245g of a titanium tetrachloride solution was slowly added to the deionized water while magnetic stirring was performed, and nitrogen gas was continuously introduced into the three-necked flask to prepare a titanium oxychloride solution having a concentration of 3.6 mol/L.
(2) Taking 50g of the titanium oxychloride solution prepared in the step (1), respectively adding 147.19g of deionized water and 0.60g of zirconium oxychloride octahydrate powder, enabling the molar ratio of zirconium ions to titanium ions to be 1.65:100, putting the uniformly mixed solution into a sealed hydrothermal reaction kettle, placing the reaction kettle in a vacuum oven, keeping the hydrothermal temperature at 80 ℃, reacting for 12 hours to obtain a precipitate TiO 2, cooling the reaction product and the reaction kettle, centrifugally separating the precipitate, washing the precipitate with distilled water and ethanol for 4-5 times in sequence, centrifuging the precipitate at the rotating speed of 4000rpm, and finally drying the precipitate at 70 ℃ for 5 hours to obtain the nano TiO 2 powder.
(3) calcining the prepared nano powder for 4 hours at 400 ℃ in a muffle furnace with temperature programming control under air atmosphere to obtain three-phase mixed TiO 2 nano powder, wherein the temperature raising rate of the calcination is 5 ℃/min.
The effect of this example is that when the reaction temperature is further lowered and the reaction time is prolonged, the rutile, anatase and brookite three-phase mixed type TiO 2 nano-powder can be obtained after the sample is calcined, the grain size is 12.5nm, the specific surface area is 62.1m 2/g, the morphology of the primary particles is basically kept unchanged, and good high-temperature stability is still maintained.
Claims (2)
1. A preparation method of three-phase mixed nano TiO 2 is characterized by comprising the following steps:
The method comprises the following steps: preparation of titanium oxychloride solution
Using titanium tetrachloride as an initial raw material, adding 285-514g of deionized water into a 1L three-neck flask under the ice bath condition, then adding 245g of titanium tetrachloride solution into the deionized water, carrying out magnetic stirring, and continuously introducing nitrogen into the three-neck flask to prepare titanium oxychloride solution with the concentration of 2.0-3.6 mol/L;
Step two, preparing zirconium ion doped TiO 2 nano powder
Taking 50g of the solution, respectively adding 81.67-147.19g of deionized water and 0.27-0.66g of zirconium oxychloride octahydrate powder, enabling the molar ratio of zirconium ions to titanium ions to be (1.23-1.65): 100, uniformly mixing the solution, transferring the mixture into a closed hydrothermal reaction kettle, placing the reaction kettle in a vacuum oven, keeping the hydrothermal temperature at 80-100 ℃, reacting for 5-12h to obtain a precipitate TiO 2, cooling the reaction product and the reaction kettle, centrifugally separating the precipitate, washing the precipitate for 4-5 times by using distilled water and ethanol in sequence, centrifugally treating the precipitate at 4000-5000rpm, removing supernatant, and finally drying the precipitate at 70 ℃ for 5-8h to obtain nano TiO 2 powder;
Step three, preparation of three-phase mixed TiO 2 nano powder
And (3) calcining the TiO 2 nano powder prepared in the step two for 4-8h at 400 ℃ in a muffle furnace controlled by temperature programming in an air atmosphere to obtain rutile, anatase and brookite three-phase mixed TiO 2 nano powder, wherein the temperature rise rate of the calcination is 5 ℃/min.
2. the method for preparing three-phase mixed nano TiO 2 according to claim 1,
(1) Using titanium tetrachloride as an initial raw material, adding 285g of deionized water into a 1L three-neck flask in an ice bath, then slowly adding 245g of titanium tetrachloride solution into the deionized water, simultaneously carrying out magnetic stirring, and continuously introducing nitrogen into the three-neck flask to prepare titanium oxychloride solution with the concentration of 3.6 mol/L;
(2) Taking 50g of the titanium oxychloride solution prepared in the step (1), respectively adding 147.19g of deionized water and 0.49g of zirconium oxychloride octahydrate powder, enabling the molar ratio of zirconium ions to titanium ions to be 1.23:100, putting the uniformly mixed solution into a sealed hydrothermal reaction kettle, placing the reaction kettle in a vacuum oven, keeping the hydrothermal temperature at 100 ℃, and reacting for 6 hours to obtain a precipitate TiO 2, after cooling a reaction product and the reaction kettle, centrifugally separating the precipitate, washing the precipitate with distilled water and ethanol for 4-5 times in sequence, centrifuging the precipitate at the rotating speed of 4000rpm, and finally drying the precipitate at 70 ℃ for 5 hours to obtain nano TiO 2 powder;
(3) Calcining the prepared TiO 2 nano powder for 4 hours at 400 ℃ in an air atmosphere by adopting a muffle furnace with temperature programming control, thus obtaining the three-phase mixed TiO 2 nano powder, wherein the temperature raising rate of the calcination is 5 ℃/min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113753944A (en) * | 2021-10-14 | 2021-12-07 | 福建贝思科电子材料股份有限公司 | Superfine barium titanate powder and preparation method thereof |
| CN113896231A (en) * | 2020-07-06 | 2022-01-07 | 宁波极微纳新材料科技有限公司 | Preparation method of titanium dioxide material |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113896231A (en) * | 2020-07-06 | 2022-01-07 | 宁波极微纳新材料科技有限公司 | Preparation method of titanium dioxide material |
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| CN113753944A (en) * | 2021-10-14 | 2021-12-07 | 福建贝思科电子材料股份有限公司 | Superfine barium titanate powder and preparation method thereof |
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