KR20140092483A - Conversion method of crystal shape to control titanium dioxide - Google Patents
Conversion method of crystal shape to control titanium dioxide Download PDFInfo
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- KR20140092483A KR20140092483A KR1020120157548A KR20120157548A KR20140092483A KR 20140092483 A KR20140092483 A KR 20140092483A KR 1020120157548 A KR1020120157548 A KR 1020120157548A KR 20120157548 A KR20120157548 A KR 20120157548A KR 20140092483 A KR20140092483 A KR 20140092483A
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- titanium dioxide
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- titanate
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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
- B82Y40/00—Manufacture or treatment of nanostructures
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- 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
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- 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
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
Description
And a method for converting crystal form of titanium dioxide using a hydrothermal synthesis method.
Titanium dioxide is used in many premises because it is not corrosive by light and is biologically and chemically safe. Typically used as a raw material for photocatalyst. The titanium dioxide has a band gap energy of about 3eV and emits electrons (e - ) and electrons (h +) pairs when energy is received from the outside. Therefore, when used in a photocatalyst, it is an ingredient capable of decomposing organic matters and self-cleaning by causing oxidation and reduction reactions. The smaller the particle size, the more efficient it is known to exhibit.
Titanium dioxide is typically anatase and rutile. Double anatase is known to be superior to photosensitized rutile. Therefore, anatase is widely used as a photocatalyst and other materials for application to photosensitivity.
Currently produced titanium dioxide is manufactured and sold only in a simple form controlled by the particle size of nano size. Therefore, various studies have been carried out in order to make the desired particle size and particle shape, but since there is no commercial production, it is required to manufacture titanium dioxide whose grain size or particle shape is controlled.
The present invention can provide a method for efficiently synthesizing wire-shaped titanium dioxide having a nano-scale in which the surface area of titanium dioxide is enlarged by utilizing commercially available titanium dioxide.
The present invention provides a method for producing titanium dioxide powder from titanium dioxide in the form of a nanowire with a surface area enlarged. In addition, titanium dioxide nanowires whose surface area is enlarged can be used in application fields such as catalyst materials and electrode materials for solar cells.
1 shows a process for synthesizing nano-wire titanium dioxide in a titanium dioxide powder.
Fig. 2 shows X-ray diffraction analysis of recrystallized titanium dioxide (b) obtained by hydrothermal synthesis of titanium dioxide powder (a), pickling and sintering.
3 is a Scanning Electron Microscope (SEM) photograph of titanium dioxide (b) in the form of a wire finally synthesized from the titanium dioxide powder (a).
The particle shape conversion method of the titanium dioxide of the present invention will be described in detail below with reference to the accompanying drawings.
The present invention relates to a method of synthesizing titanium dioxide having a wire shape by utilizing nano-sized amorphous titanium dioxide, comprising the steps of mixing titanium dioxide with an aqueous solution of sodium hydroxide and charging it into a hydrothermal synthesis reactor; A hydrothermal synthesis reaction step; Filtering and acid washing and washing the reaction-completed material; And heating the sample.
The first embodiment of the present invention relates to a method for producing sodium titanate, comprising the steps of charging a sample containing titanium dioxide powder and sodium hydroxide solution into a hydrothermal reactor, hydrothermally reacting the sample to produce sodium titanate (Na 2 Ti 3 O 7 ) , Washing the hydrothermally reacted sample with an acid, washing with water and drying to produce hydrogentitanate (H 2 Ti 3 O 7 ), and sintering the hydrogentitanate in an electric furnace And a method for producing the titanium dioxide nanowire.
A second embodiment of the present invention relates to a method of manufacturing a titanium dioxide nanowire according to the first embodiment, wherein the hydrogen peroxide is further added in the charging step.
In a third embodiment of the present invention, in the first embodiment, the hydrothermal reaction is hydrothermally treated at a temperature of 105 to 250 ° C for 6 to 72 hours, thereby producing a titanium dioxide nanowire.
The fourth embodiment of the present invention relates to a method of manufacturing a titanium dioxide nanowire according to the first embodiment, wherein the sintering step sintering at a temperature of 300 to 600 ° C for 3 hours.
A fifth embodiment of the present invention relates to a process for producing a titanium dioxide nanowire according to the first embodiment, wherein the acid is hydrochloric acid or nitric acid in the hydrogel titanate production step.
A sixth embodiment of the present invention is the method according to the first embodiment, wherein the acid washing step stheres the hydrothermally reacted sample in the acid at room temperature for 1 to 6 hours will be.
A seventh embodiment of the present invention relates to a method of manufacturing a titanium dioxide nanowire according to the first embodiment, wherein the titanium dioxide powder has a diameter of 10 to 20 nm.
Each of the above-described steps will be described in detail below.
Step 1: Mixing titanium dioxide powder and sodium hydroxide solution and hydrothermal reactor Charging
The titanium dioxide powder is charged into a sodium hydroxide solution. At this time, hydrogen peroxide is added to promote the oxidation of the titanium dioxide powder. The oxidation of the titanium dioxide powder is promoted by the hydrogen peroxide, and the dissolution of the titanium dioxide is smoothly performed. The sample is put into a reaction vessel made of Teflon and placed in a hydrothermal reactor made of steel.
Step 2: hydrothermal synthesis reaction
The hydrothermal reactor charged with the sample is hydrothermally treated at 105 to 250 ° C for 6 to 72 hours. In this reaction, water molecules are present as a vapor, and a critical condition is created inside the reactor. Under these conditions, titanium dioxide reacts as shown in equation (1). The metal titanium reacts with the sodium present in the solution as it dissolves to produce sodium titanate (Na 2 Ti 3 O 7 ). The resulting sodium titanates are entangled with the nanowires.
TiO 2 + 4H 2 O 2 + 2NaOH? Na 2 Ti 3 O 7 + 5H 2 O (1)
Step 3: Pickling and washing of the reactants
The sample prepared above is stitched for 1 to 6 hours in a solution of hydrochloric acid or nitric acid at room temperature in order to remove impurities such as sodium by sodium hydroxide which is initially added. In this process, an ion exchange reaction occurs between sodium ions (Na + ) and hydrogen ions (H + ) as shown in Equation (2). Hydrogen titanate (H 2 Ti 3 O 7 ) Chemical changes occur. The sodium-dehydrogenated titanate is washed three times with distilled water to remove the hydrochloric acid remaining in the sample. The washed sample is dried in a dryer for 24 hours to remove residual moisture. In the above process, the complex compound of titanium and sodium is substituted with a complex compound of hydrogen and titanium to produce a precursor of titanium dioxide. The removed sodium can be removed in a sodium chloride (NaCl) aqueous solution. The formation of the hydrogenated titanium compound synthesized through the above process can be confirmed in FIG.
Na 2 Ti 3 O 7 (s) + 2HCl (1)? H 2 Ti 3 O 7 (s) + Na + (aq) + Cl - (aq) (2)
Step 4: Sintering of the prepared titanium dioxide precursor
The prepared hydrogenated titanate sample is sintered in an electric furnace at 300-600 ° C for 3 hours. In this process, hydrogen is decomposed into water vapor together with oxygen, and the titanate is finally synthesized into a single phase anatase.
H 2 Ti 3 O 7 ? 3TiO 2 (S) + H 2 O (g) (thermal conversion)
Hereinafter, the present invention will be described in more detail with reference to Examples, but the present invention is not limited to the following Examples. In one embodiment, titanium dioxide in the form of a wire was produced through the following steps.
Example One
① Mixing titanium dioxide powder and sodium hydroxide solution and charging the hydrothermal reactor
The titanium dioxide powder is charged into a 10 mol / L sodium hydroxide solution. Titanium dioxide powder (STO 1 , made in Japan) having a diameter of 10 to 20 nm was used. At this time, 30% hydrogen peroxide is added to promote the oxidation of the metal powder. The oxidation of the metal powder is promoted by the hydrogen peroxide, and the titanium metal dissolves smoothly. The sample is placed in a Teflon reaction vessel and placed in a steel hydrothermal synthesis reactor.
② hydrothermal synthesis reaction
The hydrothermal reactor charged with the sample is hydrothermally treated at 200 o C for 48 hours. In this reaction, water molecules are present as a vapor, and a critical condition is created inside the reactor. Under this condition, the titanium dioxide reacts with the sodium present in the solution while dissolving to produce sodium titanate (Na 2 Ti 3 O 7 ).
③ Pickling and washing of reactants
The sample prepared above was dissolved in 0.1 mol / l hydrochloric acid for 1 hour in order to remove impurities such as sodium by sodium hydroxide which was initially added. In this process, sodium ion (Na + ) and hydrogen ion (H + ) undergo an ion exchange reaction, in which a chemical change occurs with hydrogen tetitanate (H 2 Ti 3 O 7 ). The sodium-dehydrogenated titanate is washed three times with distilled water to remove the hydrochloric acid remaining in the sample. The washed sample is dried in a dryer for 24 hours to remove residual moisture. In the above process, the complex compound of titanium and sodium is substituted with the complex compound of hydrogen and titanium, and the precursor of titanium dioxide is produced. The removed sodium can be removed in a sodium chloride (NaCl) aqueous solution.
④ Sintering of the titanium dioxide precursor prepared above
The prepared hydrogentitanate sample is sintered in a 500 ° C sintering furnace for 3 hours. In this process, hydrogen is decomposed into water vapor together with oxygen, and titanate is finally synthesized with titanium dioxide. The final product produced is titanium dioxide in the form of a wire.
Claims (7)
Subjecting the sample to hydrothermal reaction to produce sodium titanate (Na 2 Ti 3 O 7 );
Washing the hydrolyzed sample with an acid, washing with water and drying to produce hydrogentitanate (H 2 Ti 3 O 7 ); And
And sintering the hydrogenated titanate in an electric furnace
A method for producing titanium dioxide nanowires.
Wherein the hydrogen peroxide is further added in the charging step.
Wherein the hydrothermal reaction is hydrothermally treated at a temperature of 105 to 250 ° C for 6 to 72 hours.
Wherein the sintering step is performed at a temperature of 300 to 600 ° C for 3 hours.
Wherein the acid is hydrochloric acid or nitric acid in the hydrogel titanate production step.
Wherein the acid washing step is to stir the hydrolyzed sample in the acid at room temperature for 1 to 6 hours.
Wherein the titanium dioxide powder has a diameter of 10 to 20 nm.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109326790A (en) * | 2018-08-30 | 2019-02-12 | 中国石油天然气股份有限公司 | A kind of 1-dimention nano threadiness sodium titanate and its preparation method and application |
| CN109713314A (en) * | 2019-01-02 | 2019-05-03 | 江西正拓新能源科技股份有限公司 | Flexible titanium dioxide/silicon/silicon dioxide lithium ion cell electrode preparation method |
| CN111634942A (en) * | 2020-05-25 | 2020-09-08 | 海南大学 | Preparation method of titanium dioxide nanowire array with slender branches |
| US11565944B2 (en) | 2018-08-30 | 2023-01-31 | Petrochina Company Limited | Process for preparing titanic acid salt, titanic acid, and titanium oxide having controllable particle size and hierarchical structure |
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2012
- 2012-12-28 KR KR1020120157548A patent/KR20140092483A/en not_active Application Discontinuation
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109326790A (en) * | 2018-08-30 | 2019-02-12 | 中国石油天然气股份有限公司 | A kind of 1-dimention nano threadiness sodium titanate and its preparation method and application |
| CN109326790B (en) * | 2018-08-30 | 2021-08-03 | 中国石油天然气股份有限公司 | One-dimensional nano linear sodium titanate and preparation method and application thereof |
| US11565944B2 (en) | 2018-08-30 | 2023-01-31 | Petrochina Company Limited | Process for preparing titanic acid salt, titanic acid, and titanium oxide having controllable particle size and hierarchical structure |
| CN109713314A (en) * | 2019-01-02 | 2019-05-03 | 江西正拓新能源科技股份有限公司 | Flexible titanium dioxide/silicon/silicon dioxide lithium ion cell electrode preparation method |
| CN109713314B (en) * | 2019-01-02 | 2021-06-11 | 江西正拓新能源科技股份有限公司 | Preparation method of flexible titanium dioxide/silicon dioxide lithium ion battery electrode |
| CN111634942A (en) * | 2020-05-25 | 2020-09-08 | 海南大学 | Preparation method of titanium dioxide nanowire array with slender branches |
| CN111634942B (en) * | 2020-05-25 | 2021-06-22 | 海南大学 | Preparation method of titanium dioxide nanowire array with slender branches |
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