CN1524793A - Process for preparing nanometer titanium dioxide - Google Patents
Process for preparing nanometer titanium dioxide Download PDFInfo
- Publication number
- CN1524793A CN1524793A CNA031510140A CN03151014A CN1524793A CN 1524793 A CN1524793 A CN 1524793A CN A031510140 A CNA031510140 A CN A031510140A CN 03151014 A CN03151014 A CN 03151014A CN 1524793 A CN1524793 A CN 1524793A
- Authority
- CN
- China
- Prior art keywords
- ammonium chloride
- acid ester
- titanic acid
- organic amine
- hour
- 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
Images
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
A process for preparing titanium oxide comprising the steps of, filling alcoholic solution of titanium acid ester into the aqueous solution of ammonium chloride, reacting 0.5-5 hours, adding small amount of organic amine, stewing, heating for vacuum distillation, drying and sintering the dried solid. The invention can effectively prevent the nano particle sintering during burning, thus increasing the disparity of the nano particles.
Description
Technical field
The present invention relates to a kind of preparation method of nano titanium oxide.
Background technology
Titanium dioxide is a kind of important chemical material, all is widely used in every field, as can be used as the additive of cosmetics additive, paint additive, fabric post-treatment, be used for absorbing ultraviolet ray, and photocatalyst.
Many patents and document disclose preparation method separately, disclose a kind of preparation method of nano titanium oxide as Chinese patent CN1217297A, and it is raw material that this patent adopts titanium sulfate, titanyl sulfate, metatitanic acid, complex process, production cost height; Patent CN1248550A has reported a kind of method, the expensive raw material price that is adopted, and application number 00127426.0 discloses a kind of preparation method of nano titanium oxide, and the nano titanium oxide of production is reunited easily.
Summary of the invention
The technical issues that need to address of the present invention are the preparation methods that disclose a kind of nano titanium oxide, to overcome the complex process that prior art exists, production cost height, the defective that nano titanium oxide is reunited easily.
Method of the present invention comprises the steps:
(1) alcoholic solution of titanic acid ester is added the aqueous solution of ammonium chloride, preferably drip with slow speed, the dropping time is 0.5-5 hour, reacts 0.5-5 hour, adds a small amount of organic amine, leaves standstill 5-10 hour;
(2) alcohol, water and other volatizable material in the system are removed in heating underpressure distillation, the solids of evaporation back gained, and playing a main component is the compound and the chloride solid of titanium and hydrogen and oxygen, under 70～100 ℃ dry 2-6 hour; Steam thing and reclaim after condensation, its main component is alcohol, water mixture, obtains alcohol after distillation, and it can reply use;
(3) solid after the oven dry carries out roasting, and roasting time is 1-6 hour, and temperature obtains anatase titanium dioxide when being 400-500 ℃, and particle diameter is 10-100nm; Be rutile-type when temperature is 700-1000 ℃, particle diameter is 10-100nm.The condensation of gas that produces during roasting is collected, and can obtain ammonium chloride after treatment, can reply use.
The titanic acid ester of the preferred carbochain C2 of the titanic acid ester of being addressed～C6, most preferably tetrabutyl titanate;
The alcohol of being addressed is the unit alcohol of carbochain C1～C6, a kind of or its mixture in particular methanol, ethanol or the butanols;
The organic amine of being addressed comprises triethylamine, a kind of or its mixture in Monoethanolamine MEA BASF, diethanolamine, trolamine or the nitrilotriacetic acid(NTA).
The concentration of titanic acid ester alcoholic solution is preferably 0.01mol/L-10mol/L;
The weight concentration of the aqueous solution of ammonium chloride is preferably 0.01% to state of saturation;
The mol ratio of ammonium chloride and titanic acid ester is: ammonium chloride: titanic acid ester=0.01: 1～50: 1.
The add-on of organic amine is 0.01～10% of an aqueous ammonium chloride solution weight.
The present invention utilizes distillation and the thermolysis gasification of ammonium chloride when roasting, the sintering of nano particle in the time of can effectively preventing roasting, the organic amine compound that has body structure by the adding molecule, can increase the dispersiveness of nano particle, in the heating vacuum distillation process, recovery and the answer that can adopt conventional way to carry out alcoholic solvent are used, the gas that produces during roasting carries out condensation and collects, can obtain ammonium chloride after treatment, can reply use, thereby reduce production costs; Consider the answer use of solvent alcohol and ammonium chloride, formed the production process that cleans, had tangible suitability for industrialized production prospect.
Description of drawings
Fig. 1 is the electromicroscopic photograph of nanometer anatase titania of the present invention.
Fig. 2 is the electromicroscopic photograph of rutile type nano titanic oxide of the present invention.
Embodiment
Embodiment 1
With 200ml concentration is the aqueous solution that the ethanolic soln of the tetrabutyl titanate of 0.10mol/L is added dropwise to 250ml12% ammonium chloride, and the dropping time is 1 hour, reacts 4 hours, adds the 1.9g triethylamine, leaves standstill 10 hours;
Be heated to and reflux and underpressure distillation, drying is 8 hours under 80 ℃;
Solid after the oven dry carried out roasting 3 hours, and temperature is 450 ℃, obtains anatase titanium dioxide, and particle diameter is 10-60nm.Its electromicroscopic photograph is seen Fig. 1.
Embodiment 2
With 200ml concentration is the aqueous solution that the butanol solution of the tetrabutyl titanate of 0.80mol/L is added dropwise to 250ml35% ammonium chloride, and the dropping time is 2 hours, reacts 5 hours, adds the 5g Monoethanolamine MEA BASF, leaves standstill 10 hours;
Be heated to and reflux and underpressure distillation, drying is 8 hours under 80 ℃;
Solid after the oven dry carried out roasting 3 hours, and temperature is 950 ℃, obtains rutile titanium dioxide, and particle diameter is 40-90nm.Its electromicroscopic photograph is seen Fig. 2.
Claims (12)
1. the preparation method of a nano titanium oxide is characterized in that, comprises the steps:
(1) alcoholic solution of titanic acid ester is added the aqueous solution of ammonium chloride, reacted 0.5-5 hour, add a small amount of organic amine, leave standstill;
(2) heating underpressure distillation, drying;
(3) solid after the oven dry carries out roasting at a certain temperature.
2. method according to claim 1 is characterized in that, the alcoholic solution of titanic acid ester is added dropwise to the aqueous solution of ammonium chloride, and the time is 0.5-5 hour.
3. method according to claim 1 is characterized in that, the add-on of organic amine is 0.01～10% of an aqueous ammonium chloride solution.
4. method according to claim 1 is characterized in that, descends dry 2-6 hour at 70～100 ℃ after the heating underpressure distillation.
5. method according to claim 1 is characterized in that, maturing temperature is 400-500 ℃.
6. method according to claim 1 is characterized in that, maturing temperature is 700-1000 ℃.
7. method according to claim 1 is characterized in that the titanic acid ester of being addressed is the titanic acid ester of carbochain C2～C6.
8. method according to claim 1 is characterized in that, the alcohol of being addressed is the unit alcohol of carbochain C1～C6.
9. method according to claim 1 is characterized in that, the organic amine of being addressed comprises a kind of or its mixture in triethylamine, Monoethanolamine MEA BASF, diethanolamine, trolamine or the nitrilotriacetic acid(NTA).
10. method according to claim 1, it is characterized in that, the concentration of titanic acid ester alcoholic solution is 0.01mol/L-10mol/L, and the mass concentration of the aqueous solution of ammonium chloride is 0.01% to state of saturation, and the mol ratio of ammonium chloride and titanic acid ester is: ammonium chloride: titanic acid ester=0.01: 1～50: 1.
11. method according to claim 1 is characterized in that, the alcoholic solvent of dissolving phthalate reclaims to be reused.
12. method according to claim 1 is characterized in that, ammonium chloride reclaims to be reused.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03151014 CN1276876C (en) | 2003-09-17 | 2003-09-17 | Process for preparing nanometer titanium dioxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03151014 CN1276876C (en) | 2003-09-17 | 2003-09-17 | Process for preparing nanometer titanium dioxide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1524793A true CN1524793A (en) | 2004-09-01 |
| CN1276876C CN1276876C (en) | 2006-09-27 |
Family
ID=34286858
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 03151014 Expired - Fee Related CN1276876C (en) | 2003-09-17 | 2003-09-17 | Process for preparing nanometer titanium dioxide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1276876C (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1317194C (en) * | 2005-11-17 | 2007-05-23 | 上海交通大学 | Process for preparing anatase type nano crystal TiO2 solar energy cell material |
| CN100347090C (en) * | 2006-01-19 | 2007-11-07 | 清华大学 | Synthesis of TiO2 nanometer particles and bars |
| CN100434517C (en) * | 2006-07-07 | 2008-11-19 | 中国科学院上海硅酸盐研究所 | Method for reversiblely assembling enzyme using nano sheet-like TiO2 |
-
2003
- 2003-09-17 CN CN 03151014 patent/CN1276876C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1317194C (en) * | 2005-11-17 | 2007-05-23 | 上海交通大学 | Process for preparing anatase type nano crystal TiO2 solar energy cell material |
| CN100347090C (en) * | 2006-01-19 | 2007-11-07 | 清华大学 | Synthesis of TiO2 nanometer particles and bars |
| CN100434517C (en) * | 2006-07-07 | 2008-11-19 | 中国科学院上海硅酸盐研究所 | Method for reversiblely assembling enzyme using nano sheet-like TiO2 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1276876C (en) | 2006-09-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108772108B (en) | Visible light response titanium dioxide nanowire/metal organic framework/carbon nanofiber membrane and preparation method and application thereof | |
| KR20100121623A (en) | Process for the preparation of titanium dioxide with nanometric dimensions and controlled shape | |
| CN101851343B (en) | Composite film with photocatalytic oxidability and preparation method thereof | |
| CN108499611A (en) | A kind of preparation method of metal organic frame load nano-titanium dioxide photocatalysis agent | |
| CN101665679A (en) | Preparation method of carbon-based titanium dioxide composite material of complex porous structure | |
| Zhao et al. | Studies of electrospinning process of zirconia nanofibers | |
| CN108654586B (en) | Graphitized mesoporous carbon-TiO2Composite photocatalytic material and preparation method and application thereof | |
| CN103332737B (en) | Preparation method of titanium dioxide nano-powder | |
| CN1958460A (en) | Low temperature method for preparing Nano powder | |
| Liu et al. | Preparation of hollow ceramic photocatalytic membrane grafted with silicon-doped TiO2 nanorods and conversion of high-concentration NO | |
| CN1200881C (en) | Preparation method of titanium oxide nano fibre | |
| CN1276876C (en) | Process for preparing nanometer titanium dioxide | |
| CN112210890A (en) | Preparation method of iron-based metal organic framework material fiber, product and application thereof | |
| CN115155572A (en) | Chlorine-resistant high-thermal-stability catalyst for removing volatile organic compounds by oxidation and preparation method thereof | |
| CN107216250A (en) | A kind of method that utilization polyethylene terephthalate waste material prepares Di-2-ethylhexyl terephthalate | |
| CN106669660A (en) | Hierarchical-structure MnOx/TiO2 nanofiber catalyst for acetone oxidation and preparation method of hierarchical-structure MnOx/TiO2 nanofiber catalyst | |
| Liu et al. | Fabrication and photocatalytic properties of flexible BiOI/SiO2 hybrid membrane by electrospinning method | |
| CN106693696A (en) | Nanometer photocatalytic anti-haze gauze | |
| FI117754B (en) | Titanium dioxide product, process for its preparation and use as a photocatalyst | |
| CN101073769A (en) | Method for producing nano-titanic oxide light catalyst by steam hydrolysis | |
| CN1118322C (en) | Process for preparing modified titanium dioxide nano photocatalysis material | |
| CN100588447C (en) | Titania nanotube/pipe/high-efficiency glass fiber filter in situ synthesis supporting method | |
| CN110560171A (en) | Composite nanofiber with desulfurization performance and preparation method and application thereof | |
| CN1220185A (en) | Titanium dioxide photocatalyst and preparation method thereof | |
| CN103908957A (en) | Preparation method of C-TixZr(1-x)O2 nano particle catalyst for degrading methylbenzene |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20060927 Termination date: 20091019 |