CN110627115A - Titanium dioxide mesoporous sphere and preparation method thereof - Google Patents
Titanium dioxide mesoporous sphere and preparation method thereof Download PDFInfo
- Publication number
- CN110627115A CN110627115A CN201910623382.6A CN201910623382A CN110627115A CN 110627115 A CN110627115 A CN 110627115A CN 201910623382 A CN201910623382 A CN 201910623382A CN 110627115 A CN110627115 A CN 110627115A
- Authority
- CN
- China
- Prior art keywords
- reaction
- precipitate
- titanium dioxide
- transferring
- mesoporous
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/08—Drying; Calcining ; After treatment of titanium oxide
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
- C01P2004/34—Spheres hollow
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- 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
Abstract
The invention discloses a preparation method of a titanium dioxide mesoporous sphere, which mainly comprises the following steps of 1) adding 0.05-5mL of a hydrolytic agent into 30mL of a solvent, and uniformly mixing; 2) adding 0.1-5.0mL of titanium salt, and uniformly mixing to obtain a reaction solution; 3) transferring the reaction liquid into a 50mL reaction kettle, and carrying out solvothermal reaction for 1-48 hours at the temperature of 100-220 ℃; 4) after the reaction is finished, naturally cooling the kettle to room temperature, centrifugally separating the obtained product, washing the product with ethanol to obtain white precipitate, and naturally drying the white precipitate; 5) transferring the precipitate into a muffle furnace, and calcining the precipitate at the high temperature of 500 ℃ in the air for 2 hours to obtain TiO2A mesoporous sphere. Also discloses that the diameter of the product is 0.5-10 μm, and the wall thickness is 0.2-3 μm.
Description
Technical Field
The invention relates to the preparation in the field of materials, in particular to a template-free method for preparing TiO2A mesoporous ball and a preparation method thereof.
Background
TiO since the beginning of the nineteenth century2Has become a commodity, and is widely used as a pigment, a sun-screening agent, a paint, a toothpaste ingredient and the like[1]. In 1972, Fujishima and Honda discovered TiO2The electrode can decompose water under the irradiation of ultraviolet rays to obtain hydrogen and oxygen[2]Thus raising the hot tide of research on it. Due to TiO2Has the characteristics of very stable structure, no toxicity, low cost and the like, and is widely appliedIs applied to various fields. Preparation of TiO with special morphology2It is important to adapt to different applications. Most common TiO2The shapes of the nano-particles are nano-particles, spheres, mesoporous structures, nano-wires, nano-sheets and the like. The mesoporous structure has a large specific surface area, provides a sufficient interface for the reaction, and can also be used as a carrier for supporting a catalyst, thus attracting much attention of researchers. In general, researchers will add additives or templates to prepare TiO2Mesoporous spheres, e.g. S.Eiden-Assmann et al with Pluronic PE 6400 organic additive, produced TiO2Well ball[3]The method not only makes the preparation process complicated, but also increases the preparation cost. The method can prepare TiO by a template-free method under the condition of no additive2The method is simple, rapid and effective, and is hopeful to be amplified to large-scale production.
[1]Chen X,Mao S S.Titanium dioxide nanomaterials:synthesis,properties,modifications,and applications.Chemical reviews,2007,107(7):2891-2959.
[2]Fujishima A,Honda K.Electrochemical photolysis of water at a semiconductor electrode.Nature,1972(238):37-38.
[3]Eiden-Assmann,S.,J.Widoniak,and G.Maret."Synthesis and characterization of porous and nonporous monodisperse colloidalTiO2particles."Chemistry of Materials,2004,16(1):6-11.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a titanium dioxide mesoporous sphere and a preparation method thereof.
The invention aims to solve the technical problems mentioned in the background technology and is realized by the following technical scheme: a preparation method of titanium dioxide mesoporous spheres comprises the following steps:
1) adding 0.05-5mL of hydrolytic agent into 30mL of solvent, and uniformly mixing;
2) adding 0.1-5.0mL of titanium salt, and uniformly mixing to obtain a reaction solution;
3) transferring the reaction liquid into a 50mL reaction kettle, and carrying out solvothermal reaction for 1-48 hours at the temperature of 100-220 ℃;
4) after the reaction is finished, naturally cooling the kettle to room temperature, centrifugally separating the obtained product, washing the product with ethanol to obtain white precipitate, and naturally drying the white precipitate;
5) transferring the precipitate into a muffle furnace, and calcining the precipitate at the high temperature of 500 ℃ in the air for 2 hours to obtain TiO2A mesoporous sphere.
Preferably, the hydrolytic agent in the step 1) is one or a mixture of more of LiCl, NaCl, KCl and RbCl solution.
Preferably, 0.01 to 1.00 mol/L.
Preferably, the solvent in step 1) is selected from any one or more of methanol, ethanol, isopropanol, n-propanol and n-butanol.
Preferably, the titanium salt in step 2) is selected from any one of ethyl titanate, isopropyl titanate or butyl titanate.
The second technical proposal of the invention is that the diameter of the pore spheres in the titanium dioxide prepared by the preparation method is 0.5-10 μm, and the wall thickness is 0.2-3 μm.
Advantageous effects
The invention has the beneficial effects that 1, TiO can be prepared by a one-step solvothermal method2A mesoporous sphere; 2. no template is required to be added in the preparation process; 3. the preparation process needs no surfactant and organic additive 4, and the method is fast, simple and low in cost.
Drawings
FIG. 1 is TiO2Scanning electron microscope pictures of the mesoporous spheres.
FIG. 2 is TiO2The X-ray diffraction spectrum of the mesoporous spheres is that the prepared material is anatase TiO2。
Detailed Description
The invention is further described below with reference to the following figures and specific examples. It is to be understood that the embodiments discussed herein are for illustrative purposes only and that modifications or changes in light thereof will be suggested to persons skilled in the art and are to be included within the purview of the appended claims.
Example 1
Adding 0.05mL and 0.1mol/L LiCl into 30mL of ethanol solution, uniformly mixing, adding 0.5mL of isopropyl titanate, uniformly mixing, transferring the reaction solution into a 50mL reaction kettle, reacting for 24 hours at 150 ℃, naturally cooling the kettle to room temperature after the reaction is finished, separating the obtained product through centrifugation, washing for 3 times by using ethanol at the rotation speed of 10000 r/min to obtain white precipitate, and naturally drying. Then transferring the precipitate into a muffle furnace, and calcining the precipitate at the high temperature of 500 ℃ in the air for 2 hours to obtain TiO2A mesoporous sphere.
Example 2
Adding 0.05mL and 0.1mol/L NaCl into 30mL ethanol solution, uniformly mixing, adding 0.5mL isopropyl titanate, uniformly mixing, transferring the reaction solution into a 50mL reaction kettle, reacting for 24 hours at 150 ℃, naturally cooling the kettle to room temperature after the reaction is finished, separating the obtained product through centrifugation, washing for 3 times by using ethanol at the rotation speed of the centrifuge of 10000 r/min to obtain white precipitate, and naturally drying. Then transferring the precipitate into a muffle furnace, and calcining the precipitate at the high temperature of 500 ℃ in the air for 2 hours to obtain TiO2A mesoporous sphere.
Example 3
Adding 0.05mL and 0.1mol/L KCl into 30mL of ethanol solution, uniformly mixing, adding 0.5mL of isopropyl titanate, uniformly mixing, transferring the reaction solution into a 50mL reaction kettle, reacting for 24 hours at 150 ℃, naturally cooling the kettle to room temperature after the reaction is finished, separating the obtained product through centrifugation, washing for 3 times by using ethanol at the rotation speed of 10000 r/min to obtain white precipitate, and naturally drying. Then transferring the precipitate into a muffle furnace, and calcining the precipitate at the high temperature of 500 ℃ in the air for 2 hours to obtain TiO2A mesoporous sphere.
Example 4
Adding 0.05mL and 0.1mol/L RbCl into 30mL of ethanol solution, uniformly mixing, adding 0.5mL of isopropyl titanate, uniformly mixing, transferring the reaction solution into a 50mL reaction kettle, reacting for 24 hours at 150 ℃, naturally cooling the kettle to room temperature after the reaction is finished, separating the obtained product through centrifugation, and transferring a centrifuge into a reactorRotating at 10000 r/min, washing with ethanol for 3 times to obtain white precipitate, and naturally drying. Then transferring the precipitate into a muffle furnace, and calcining the precipitate at the high temperature of 500 ℃ in the air for 2 hours to obtain TiO2A mesoporous sphere.
Example 5
Adding 0.1mL and 0.1mol/L KCl into 30mL of ethanol solution, uniformly mixing, adding 0.5mL of isopropyl titanate, uniformly mixing, transferring the reaction solution into a 50mL reaction kettle, reacting for 24 hours at 150 ℃, naturally cooling the kettle to room temperature after the reaction is finished, separating the obtained product through centrifugation, washing for 3 times by using ethanol at the rotation speed of 10000 r/min to obtain white precipitate, and naturally drying. Then transferring the precipitate into a muffle furnace, and calcining the precipitate at the high temperature of 500 ℃ in the air for 2 hours to obtain TiO2A mesoporous sphere.
Example 6
Adding 0.1mL and 0.1mol/L KCl into 30mL of ethanol solution, uniformly mixing, adding 1mL of isopropyl titanate, uniformly mixing, transferring the reaction solution into a 50mL reaction kettle, reacting at 200 ℃ for 24 hours, naturally cooling the kettle to room temperature after the reaction is finished, separating the obtained product through centrifugation, washing for 3 times by using ethanol at the rotation speed of the centrifuge of 10000 r/min to obtain white precipitate, and naturally drying. Then transferring the precipitate into a muffle furnace, and calcining the precipitate at the high temperature of 500 ℃ in the air for 2 hours to obtain TiO2A mesoporous sphere.
Example 7
Adding 0.1mL and 0.5mol/L KCl into 30mL of ethanol solution, uniformly mixing, adding 1mL of isopropyl titanate, uniformly mixing, transferring the reaction solution into a 50mL reaction kettle, reacting at 200 ℃ for 24 hours, naturally cooling the kettle to room temperature after the reaction is finished, separating the obtained product through centrifugation, washing for 3 times by using ethanol at the rotation speed of the centrifuge of 10000 r/min to obtain white precipitate, and naturally drying. Then transferring the precipitate into a muffle furnace, and calcining the precipitate at the high temperature of 500 ℃ in the air for 2 hours to obtain TiO2A mesoporous sphere.
Example 8
Adding 0.5mL of KCl with the concentration of 0.1mol/L into 30mL of ethanol solution, and mixing uniformlyAdding 1mL of isopropyl titanate, uniformly mixing, transferring the reaction solution into a 50mL reaction kettle, reacting for 24 hours at 200 ℃, naturally cooling the kettle to room temperature after the reaction is finished, separating the obtained product through centrifugation, washing for 3 times by using ethanol at the rotation speed of the centrifuge of 10000 r/min to obtain white precipitate, and naturally drying. Then transferring the precipitate into a muffle furnace, and calcining the precipitate at the high temperature of 500 ℃ in the air for 2 hours to obtain TiO2A mesoporous sphere.
Example 9
Adding 0.1mL and 0.1mol/L KCl into 30mL of ethanol solution, uniformly mixing, adding 1mL of butyl titanate, uniformly mixing, transferring the reaction solution into a 50mL reaction kettle, reacting at 200 ℃ for 24 hours, naturally cooling the kettle to room temperature after the reaction is finished, separating the obtained product through centrifugation, washing for 3 times by using ethanol at the rotation speed of the centrifuge of 10000 r/min to obtain white precipitate, and naturally drying. Then transferring the precipitate into a muffle furnace, and calcining the precipitate at the high temperature of 500 ℃ in the air for 2 hours to obtain TiO2A mesoporous sphere.
As shown in FIG. 1, is TiO2Scanning electron microscope pictures of the mesoporous spheres.
As shown in FIG. 2, is TiO2The X-ray diffraction spectrum of the mesoporous spheres is that the prepared material is anatase TiO2。
Table 1 TiO prepared in example2Size parameter of mesoporous ball
- -: indicating that it is not available.
While the present invention has been described with reference to the accompanying drawings, the present invention is not limited to the above-described embodiments, which are illustrative only and not restrictive, and various modifications which do not depart from the spirit of the present invention and which are intended to be covered by the claims of the present invention may be made by those skilled in the art.
Claims (6)
1. The preparation method of the titanium dioxide mesoporous spheres is characterized by comprising the following steps:
1) adding 0.05-5mL of hydrolytic agent into 30mL of solvent, and uniformly mixing;
2) adding 0.1-5.0mL of titanium salt, and uniformly mixing to obtain a reaction solution;
3) transferring the reaction liquid into a 50mL reaction kettle, and carrying out solvothermal reaction for 1-48 hours at the temperature of 100-220 ℃;
4) after the reaction is finished, naturally cooling the kettle to room temperature, centrifugally separating the obtained product, washing the product with ethanol to obtain white precipitate, and naturally drying the white precipitate;
5) transferring the precipitate into a muffle furnace, and calcining the precipitate at the high temperature of 500 ℃ in the air for 2 hours to obtain TiO2A mesoporous sphere.
2. The method for preparing the mesoporous titania spheres of claim 1, wherein the hydrolysis agent in step 1) is one or more of LiCl, NaCl, KCl and RbCl solution.
3. The method for preparing titanium dioxide mesoporous spheres according to claim 2, wherein the concentration of the titanium dioxide mesoporous spheres is 0.01-1.00 mol/L.
4. The method for preparing the titanium dioxide mesoporous spheres as claimed in claim 1, wherein the solvent in the step 1) is selected from any one or more of methanol, ethanol, isopropanol, n-propanol and n-butanol.
5. The method for preparing titanium dioxide mesoporous spheres according to claim 1, wherein the titanium salt in the step 2) is selected from any one of ethyl titanate, isopropyl titanate or butyl titanate.
6. The titanium dioxide mesoporous spheres prepared by the method according to claims 1 to 5, wherein the mesoporous spheres have a diameter size of 0.5 to 10 μm and a wall thickness of 0.2 to 3 μm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910623382.6A CN110627115B (en) | 2019-07-11 | 2019-07-11 | Titanium dioxide mesoporous sphere and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910623382.6A CN110627115B (en) | 2019-07-11 | 2019-07-11 | Titanium dioxide mesoporous sphere and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110627115A true CN110627115A (en) | 2019-12-31 |
| CN110627115B CN110627115B (en) | 2022-05-20 |
Family
ID=68969252
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910623382.6A Active CN110627115B (en) | 2019-07-11 | 2019-07-11 | Titanium dioxide mesoporous sphere and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110627115B (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102324311A (en) * | 2011-07-04 | 2012-01-18 | 武汉大学 | Method for preparing bifunctional DSSC (dye-sensitized solar cell) photo-anode |
| CN102718256A (en) * | 2012-06-23 | 2012-10-10 | 三峡大学 | Preparation method for titania microspheres with adjustable grain sizes |
| CN102786083A (en) * | 2012-06-08 | 2012-11-21 | 合肥工业大学 | Preparation method of titanium dioxide nano hollow ball |
-
2019
- 2019-07-11 CN CN201910623382.6A patent/CN110627115B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102324311A (en) * | 2011-07-04 | 2012-01-18 | 武汉大学 | Method for preparing bifunctional DSSC (dye-sensitized solar cell) photo-anode |
| CN102786083A (en) * | 2012-06-08 | 2012-11-21 | 合肥工业大学 | Preparation method of titanium dioxide nano hollow ball |
| CN102718256A (en) * | 2012-06-23 | 2012-10-10 | 三峡大学 | Preparation method for titania microspheres with adjustable grain sizes |
Also Published As
| Publication number | Publication date |
|---|---|
| CN110627115B (en) | 2022-05-20 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106732617B (en) | A kind of ZnO/Cu2O heterojunction photocatalysis material and preparation method thereof | |
| TWI458685B (en) | Titanium dioxide nanopowder and manufacturing method thereof | |
| CN106475127A (en) | A kind of nitrogen-doped graphene quantum dot/mesopore titania photocatalyst and preparation method thereof | |
| Pan et al. | Hydrous TiO2 spheres: An excellent platform for the rational design of mesoporous anatase spheres for photoelectrochemical applications | |
| CN114832863B (en) | Hierarchical pore metal organic framework material and preparation method and application thereof | |
| Wang et al. | Titanocene dichloride (Cp 2 TiCl 2) as a precursor for template-free fabrication of hollow TiO 2 nanostructures with enhanced photocatalytic hydrogen production | |
| CN113275011B (en) | Preparation method of cuprous oxide photocatalyst with flower-ball-shaped multi-stage structure | |
| CN103691415A (en) | High-crystallinity titanium dioxide-silica nano composite material with regular mesoporous structure as well as preparation method and application thereof | |
| CN105664969B (en) | A kind of titanium dioxide-platinum-cobaltosic oxide tri compound catalysis material and preparation method thereof | |
| CN113736094B (en) | Synthesis method of hierarchical porous ZIF-9 | |
| CN104998629B (en) | A kind of core shell structure SiO2‑TiO2Composite nano materials and its preparation method and application | |
| CN104628263B (en) | A kind of method preparing Indium sesquioxide. octahedron nano-crystal film | |
| CN107930611A (en) | A kind of carbon dots titanium dioxide hollow microballoon composite nano-catalyst and preparation method and application | |
| CN108262041A (en) | A kind of one pot of method for preparing high activity gold/zinc oxide compound nano cluster of room temperature | |
| CN112354559B (en) | Two-dimensional receptor molecule/hierarchical pore TiO 2 Composite photocatalyst, preparation method and photocatalytic application thereof | |
| CN108046340B (en) | Method for preparing cobaltosic oxide multi-layer hollow nanospheres without template | |
| CN110627115B (en) | Titanium dioxide mesoporous sphere and preparation method thereof | |
| CN110064752B (en) | Preparation method of mesoporous metal platinum nanospheres | |
| CN108295897A (en) | A kind of compounded visible light photocatalyst Ag2CO3/TiO2/UIO-66-(COOH)2And organic matter degradation application | |
| CN112439429B (en) | Cadmium sulfide particles with cage-shaped structure and preparation method and application thereof | |
| CN108927202B (en) | g-C3N4Nanobelt and preparation method and application thereof | |
| CN108033482B (en) | Method for preparing indium oxide hollow nanospheres and product | |
| CN112978794B (en) | Method for aqueous phase synthesis of mesoporous titanium dioxide material | |
| CN113353967B (en) | Multi-morphology Cu 2 Controllable synthesis method and application of O | |
| CN113087013B (en) | Titanium dioxide and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |