CN101007654A - Synthesis method of non-aqueous nanometer anatase titania - Google Patents
Synthesis method of non-aqueous nanometer anatase titania Download PDFInfo
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- CN101007654A CN101007654A CN 200610102309 CN200610102309A CN101007654A CN 101007654 A CN101007654 A CN 101007654A CN 200610102309 CN200610102309 CN 200610102309 CN 200610102309 A CN200610102309 A CN 200610102309A CN 101007654 A CN101007654 A CN 101007654A
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- anatase titania
- butyl titanate
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Abstract
The invention discloses a synthesizing method of non-aqueous system anatase type titanium dioxide, which comprises the following steps: adopting C2-C9 organic acid and butyl titanate as raw material with molar rate at 2-20: 1; reacting under 80-240 deg.c for 8-24h; washing through alcohol for 3-6 times; drying under 80-160 deg.c; obtaining the product.
Description
Technical field
The invention belongs to the preparation method of titanium dioxide, specifically is exactly to utilize a kind of simple method to prepare the titanium dioxide of anatase octahedrite at non-aqueous system.
Technical background
Nano-TiO
2Be one of important inorganic chemical industry material, Japanese Patent is announced prepared nano-TiO first
2Grain be 15～50nm through scope.Nano-TiO
2Not only have nano material integral surface effect, volume effect and Kubo effect, and have many general T iO that are different from
2Property, as quantum size effect, anti-uv-ray is strong, chemically reactive height, good dispersity etc.Nano-TiO
2All have wide practical use in fields such as fine ceramics, catalyzer, transmitter, ultraviolet screening agent, photocells.Therefore, nano-TiO
2Preparation, application and development become the focus of material science research.
TiO
2Three kinds of crystalline forms are arranged: anatase octahedrite, rutile and brookite, and the TiO of anatase octahedrite
2Generally acknowledged and had best photoelectricity and photochemical properties.At present, anatase octahedrite TiO
2Synthetic method mainly be vapor phase process and liquid phase method.Germany Degauss company and Japanese Sharp company mainly are with vapor phase process synthesis of nano TiO
2But, the method complex process, the temperature of reaction height, investment is big.Japan ridge village oil refinery company and Massachusetts Institute Technology prepare nano-TiO with liquid phase method in aqueous systems
2, these methods make preparation technology very complicated, and the reaction times are longer, the TiO that obtains owing to will control the hydrolysis of titanium precursor body
2Need just can obtain the TiO of advantages of good crystallization through high-temperature post-treatment
2
Summary of the invention
The object of the invention provides the anatase octahedrite TiO that a kind of raw material is simple, easy and simple to handle, pollution-free, productive rate is high
2Synthetic method.
The object of the present invention is achieved like this: utilize the presoma of titanium and organic acid to be raw material, then reacting by heating for some time in reactor, just can obtain the good anatase octahedrite TiO of crystallization after the oven dry
2
The inventive method is as follows:
Organic acid and tetra-n-butyl titanate with C2～C9 are raw material, and organic acid and the mol ratio of tetra-n-butyl titanate are to mix at 2～20: 1, and 80～240 ℃ of reactions 8～24 hours, alcohol was washed 3～6 times, 80～160 ℃ of oven dry, promptly gets anatase titania then.
The organic acid of aforesaid C2～C9 is acetate (acetic acid), propionic acid, butyric acid, valeric acid, caproic acid, enanthic acid, sad or n-nonanoic acid.
The present invention compared with prior art has following advantage:
1. raw material is simple, easy and simple to handle, reaction conditions is gentle, productive rate is high;
2. control the hydrolysis of titanium precursor body by reaction oneself;
3. react the by product environmentally safe that generates, secondary valence value height;
4. the product degree of crystallinity height that obtains.
Embodiment
Embodiment 1
Is to be transferred in the reactor after mixing at 2: 1 with acetic acid and tetra-n-butyl titanate with mol ratio, 100 ℃ of reactions 12 hours, reactant is given a baby a bath on the third day after its birth time with alcohol, 100 ℃ of oven dry, promptly obtains the anatase titania material then.
Embodiment 2
Is to be transferred in the reactor after mixing at 4: 1 with acetic acid and tetra-n-butyl titanate with mol ratio, 80 ℃ of reactions 12 hours, reactant is given a baby a bath on the third day after its birth time with alcohol, 120 ℃ of oven dry, promptly obtains the anatase titania material then.
Embodiment 3
Is to be transferred in the reactor after mixing at 4: 1 with butyric acid and tetra-n-butyl titanate with mol ratio, 120 ℃ of reactions 14 hours, reactant is given a baby a bath on the third day after its birth time with alcohol, 120 ℃ of oven dry, promptly obtains the anatase titania material then.
Embodiment 4
Is to be transferred in the reactor after mixing at 6: 1 with caproic acid and tetra-n-butyl titanate with mol ratio, 140 ℃ of reactions 12 hours, reactant is given a baby a bath on the third day after its birth time with alcohol, 80 ℃ of oven dry, promptly obtains the anatase titania material then.
Embodiment 5
Is to be transferred in the reactor after mixing at 8: 1 with sad and tetra-n-butyl titanate with mol ratio, 160 ℃ of reactions 16 hours, reactant is given a baby a bath on the third day after its birth time with alcohol, 140 ℃ of oven dry, promptly obtains the anatase titania material then.
Embodiment 6
Is to be transferred in the reactor after mixing at 4: 1 with sad and tetra-n-butyl titanate with mol ratio, 140 ℃ of reactions 16 hours, reactant is given a baby a bath on the third day after its birth time with alcohol, 100 ℃ of oven dry, promptly obtains the anatase titania material then.
Embodiment 7
Is to be transferred in the reactor after mixing at 8: 1 with capric acid and tetra-n-butyl titanate with mol ratio, 160 ℃ of reactions 12 hours, reactant is given a baby a bath on the third day after its birth time with alcohol, 120 ℃ of oven dry, promptly obtains the anatase titania material then.
Embodiment 8
Is to be transferred in the reactor after mixing at 20: 1 with acetic acid and tetra-n-butyl titanate with mol ratio, 160 ℃ of reactions 10 hours, reactant is given a baby a bath on the third day after its birth time with alcohol, 120 ℃ of oven dry, promptly obtains the anatase titania material then.
Claims (2)
1, a kind of non-aqueous nanometer anatase titania synthetic method is characterized in that comprising the steps:
Organic acid and tetra-n-butyl titanate with C2～C9 are raw material, and organic acid and the mol ratio of tetra-n-butyl titanate are to mix at 2～20: 1, and 80～240 ℃ of reactions 8～24 hours, alcohol was washed 3-6 time, 80～160 ℃ of oven dry, promptly gets anatase titania then.
2, a kind of non-aqueous nanometer anatase titania synthetic method as claimed in claim 1, the organic acid that it is characterized in that described C2～C9 is acetic acid, propionic acid, butyric acid, valeric acid, caproic acid, enanthic acid, sad or n-nonanoic acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101023097A CN100453466C (en) | 2006-12-20 | 2006-12-20 | Synthesis method of non-aqueous nanometer anatase titania |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101023097A CN100453466C (en) | 2006-12-20 | 2006-12-20 | Synthesis method of non-aqueous nanometer anatase titania |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101007654A true CN101007654A (en) | 2007-08-01 |
| CN100453466C CN100453466C (en) | 2009-01-21 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2006101023097A Expired - Fee Related CN100453466C (en) | 2006-12-20 | 2006-12-20 | Synthesis method of non-aqueous nanometer anatase titania |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103553125A (en) * | 2013-10-22 | 2014-02-05 | 渤海大学 | Method for preparing small particle size anatase nano TiO2 |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006103999A (en) * | 2004-10-01 | 2006-04-20 | Murata Mfg Co Ltd | Method of manufacturing titanium oxide fine particle |
| CN100445209C (en) * | 2005-07-28 | 2008-12-24 | 同济大学 | Preparation method of new type nano-titanium dioxide powder |
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2006
- 2006-12-20 CN CNB2006101023097A patent/CN100453466C/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103553125A (en) * | 2013-10-22 | 2014-02-05 | 渤海大学 | Method for preparing small particle size anatase nano TiO2 |
| CN103553125B (en) * | 2013-10-22 | 2015-09-16 | 渤海大学 | Prepare the method for small particle size anatase-type nanometer titanium dioxide |
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| Publication number | Publication date |
|---|---|
| CN100453466C (en) | 2009-01-21 |
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Granted publication date: 20090121 Termination date: 20121220 |