CN100384746C - Method for low temperature preparation of P25 type nanometer titanium dioxide - Google Patents
Method for low temperature preparation of P25 type nanometer titanium dioxide Download PDFInfo
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- CN100384746C CN100384746C CNB2005100452936A CN200510045293A CN100384746C CN 100384746 C CN100384746 C CN 100384746C CN B2005100452936 A CNB2005100452936 A CN B2005100452936A CN 200510045293 A CN200510045293 A CN 200510045293A CN 100384746 C CN100384746 C CN 100384746C
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Abstract
The present invention provides a method for preparing P25 type nanometer titanium dioxide at low temperature. The method has the following steps: titanium tetrachloride and a hydrochloric water solution with the pH value of 1.5 to 2.0 are taken according to the volume ratio of 1: 3, and the titanium tetrachloride is dropped in the hydrochloric water solution and stirred for 30 minutes; urea with 1 to 3 times molar ratio of the titanium tetrachloride and ammonium nitrate with 6 to 10 times molar ratio of the titanium tetrachloride are added into the solution, placed in a drying oven after thoroughly stirred, and heated for 20 to 60 minutes at the temperature of 150 to 180 DEG C; the solution is sintered for 5 to 30 minutes at the temperature of 350 to 550 DEG C to manufacture the P25 type titanium oxide powder. The crystal phase form of the titanium oxide manufactured by the present invention is identical to the crystal phase form of the P25 type titanium oxide, and the average particle diameters are smaller than that of the P25 type titanium oxide. Compared with a gas-phase oxidation method, the present invention has the advantages of simple manufacturing process, cheap raw material, high safety, reliability and energy saving.
Description
(1) technical field
The present invention relates to a kind of method of low temperature preparation of P 25 type nanometer titanium dioxide, belong to chemical material technical field.
(2) background technology
Serious day by day along with environmental pollution, the improvement of environmental pollution has become the key subjects that need to be resolved hurrily this century, is subjected to the great attention of various countries.People find the nano-titanium oxide multiple organism of can effectively degrading in the process of seeking efficient and eco-friendly environmental improvement technology, and Industrial Wastewater Treatment, are the most reliable at present a kind of high efficiency photocatalysts.For titania photocatalyst, generally acknowledge in the world at present and the product that generally adopts is the P25 that German Degussa company produces.This product is to adopt vapour phase oxidation process to produce, and its crystalline phase is formed and is about 70% anatase octahedrite, 30% rutile, and median size is about 30nm, and specific surface area is 50m
2g
-1Because its good dispersity, the photocatalytic activity height is widely used in and plays photocatalysis, uvioresistant effect, germicidal action in the nano paint and be used as carrier of photocatalyst.
But, vapour phase oxidation process (being aerosol processing again) obtains product because being the steam hydrolysis that utilizes the oxyhydrogen flame burning to produce, and temperature of reaction up to 1800 ℃ about, this makes production process need relatively harsher experiment condition, can there be certain potential safety hazard in the use of gas, and the high energy consumption that need be very high of temperature of reaction.
(3) summary of the invention:
The present invention is directed to above-mentioned vapour phase oxidation process and produce the deficiency of P25 type nano titanium oxide, a kind of method of low temperature preparation of P 25 type nanometer titanium dioxide is provided, this method technology is simple, save energy, environmental friendliness and prepared titanium oxide have the crystalline phase identical with P25 and form, and less than the median size of P25.
The present invention is realized by following technical scheme:
The method steps of this low temperature preparation of P 25 type nanometer titanium dioxide is as follows:
(1) 1: 3 by volume ratio is measured titanium tetrachloride and the pH value aqueous solution of hydrochloric acid for 1.5-2.0, and titanium tetrachloride is added dropwise to aqueous solution of hydrochloric acid, stirs 30 minutes;
(2) add relative titanium tetrachloride mol ratio 1-3 urea and mol ratio 6-10 ammonium nitrate doubly doubly in above-mentioned solution, put into baking oven after fully stirring, heating is 20-60 minute under 150-180 ℃ of temperature; Then
(3) with above-mentioned solution at 350-550 ℃ of sintering temperature 5-30 minute, can make P25 type Preparation of Nanocrystal TiO.
The crystalline phase of the Preparation of Nanocrystal TiO that obtains by above-mentioned steps is formed and is about 70% anatase octahedrite, 30% rutile, and median size is 10nm-15nm, and specific surface area is 40--45m
2g
-1
The present invention adopts redox combustion method synthetic fast preparation titanium dioxide under low temperature and air atmosphere, and prepared titanium oxide has the crystalline phase identical with P25 to be formed, and reaches the median size less than P25.Compare with vapour phase oxidation process that technology is simple, raw material is cheap, safe and reliable, save energy.
(4) embodiment
Embodiment 1
With 10ml titanium tetrachloride (TiCl
4) be added dropwise to (pH=1.5-2.0) in the 30ml aqueous solution of hydrochloric acid, stir 30min.In above-mentioned solution, add relative TiCl
4The ammonium nitrate that urea that mol ratio is 1.2 times and mol ratio are 7 times is put into baking oven after fully stirring, and heats 40 minutes down at 160 ℃.Then with above-mentioned solution 400 ℃ of following sintering 10 minutes.Can obtain Preparation of Nanocrystal TiO, its crystalline phase is formed and is about 70% anatase octahedrite, 30% rutile, and median size is about 12nm, and specific surface area is about 42m
2g
-1
Embodiment 2
With 10ml TiCl
4Be added dropwise to (pH=1.5-2.0) stirring 30min in the 30ml aqueous solution of hydrochloric acid.In above-mentioned solution, add relative TiCl
4The ammonium nitrate that urea that mol ratio is 3 times and mol ratio are 10 times is put into baking oven after fully stirring, and heats 20 minutes down at 180 ℃.Then with above-mentioned solution 350 ℃ of following sintering 20 minutes.Can obtain Preparation of Nanocrystal TiO, its crystalline phase is formed and is about 70% anatase octahedrite, 30% rutile, and median size is 10nm, and specific surface area is about 45m
2g
-1
Embodiment 3
With 10ml TiCl
4Be added dropwise to (pH=1.5-2.0) stirring 30min in the 20ml aqueous solution of hydrochloric acid.In above-mentioned solution, add relative TiCl
4The ammonium nitrate that urea that mol ratio is 2 times and mol ratio are 8 times is put into baking oven after fully stirring, 150 ℃ of heating 40 minutes.Then with above-mentioned solution 550 ℃ of following sintering 5 minutes.Can obtain Preparation of Nanocrystal TiO, its crystalline phase is formed and is about 70% anatase octahedrite, 30% rutile, and median size is 15nm, and specific surface area is about 40m
2g
-1
Embodiment 4
With 10ml TiCl
4Be added dropwise to (pH=1.5-2.0) stirring 30min in the 20ml aqueous solution of hydrochloric acid.In above-mentioned solution, add relative TiCl
4The ammonium nitrate that urea that mol ratio is 2.5 times and mol ratio are 9 times is put into baking oven after fully stirring, 160 ℃ of heating 40 minutes.Then with above-mentioned solution 500 ℃ of following sintering 10 minutes.Can obtain Preparation of Nanocrystal TiO, its crystalline phase is formed and is about 70% anatase octahedrite, 30% rutile, and median size is 13nm, and specific surface area is about 41m
2g
-1
Claims (2)
1. the method for a low temperature preparation of P 25 type nanometer titanium dioxide, it is characterized in that: the step of this method is as follows:
(1) 1: 3 by volume ratio is measured titanium tetrachloride and the pH value aqueous solution of hydrochloric acid for 1.5-2.0, and titanium tetrachloride is added dropwise to aqueous solution of hydrochloric acid, stirs 30 minutes;
(2) add relative titanium tetrachloride mol ratio 1-3 urea and mol ratio 6-10 ammonium nitrate doubly doubly in above-mentioned solution, put into baking oven after fully stirring, heating is 20-60 minute under 150-180 ℃ of temperature; Then
(3) with above-mentioned solution at 350-550 ℃ of sintering temperature 5-30 minute, can make P25 type Preparation of Nanocrystal TiO.
2. the method for low temperature preparation of P 25 type nanometer titanium dioxide according to claim 1, it is characterized in that: the crystalline phase of the P25 type Preparation of Nanocrystal TiO that makes consists of 70% anatase octahedrite, 30% rutile, median size is 10nm-15nm, and specific surface area is 40--45m
2g
-1
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2005100452936A CN100384746C (en) | 2005-11-30 | 2005-11-30 | Method for low temperature preparation of P25 type nanometer titanium dioxide |
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| CNB2005100452936A CN100384746C (en) | 2005-11-30 | 2005-11-30 | Method for low temperature preparation of P25 type nanometer titanium dioxide |
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| CN1803630A CN1803630A (en) | 2006-07-19 |
| CN100384746C true CN100384746C (en) | 2008-04-30 |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102728350A (en) * | 2012-07-10 | 2012-10-17 | 北京纬纶华业环保科技股份有限公司 | Catalyst for treating industrial waste water by catalytic wet air oxidation (CWAO) |
| CN102887543B (en) * | 2012-11-05 | 2015-01-14 | 西华师范大学 | Environment coordination type preparation method of nano titanium dioxide powder |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06211521A (en) * | 1992-11-30 | 1994-08-02 | Shiseido Co Ltd | Production of low-order titanium oxide-containing pigment |
| JP2000344521A (en) * | 1999-06-03 | 2000-12-12 | Hideaki Tanaka | Titanate paste and titanate liquid processed product |
| US20030103889A1 (en) * | 1999-08-23 | 2003-06-05 | Rotem Amfert Negev Ltd. | Silicon-containing titanium dioxide, method for preparing the same and catalytic compositions thereof |
| KR20040100327A (en) * | 2003-05-22 | 2004-12-02 | 김선재 | Preparation Method of Titanium Dioxide Powder with Large Specific Surface Area Using Indirect Neutralization |
| CN1579946A (en) * | 2003-08-05 | 2005-02-16 | 拉萨绿能科技实业有限公司 | New process for preparing anatase type nano titanium dioxide |
| JP2005138008A (en) * | 2003-11-05 | 2005-06-02 | National Institute For Materials Science | Visible light responding type titanium oxide composite photocatalyst and its manufacturing method |
-
2005
- 2005-11-30 CN CNB2005100452936A patent/CN100384746C/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06211521A (en) * | 1992-11-30 | 1994-08-02 | Shiseido Co Ltd | Production of low-order titanium oxide-containing pigment |
| JP2000344521A (en) * | 1999-06-03 | 2000-12-12 | Hideaki Tanaka | Titanate paste and titanate liquid processed product |
| US20030103889A1 (en) * | 1999-08-23 | 2003-06-05 | Rotem Amfert Negev Ltd. | Silicon-containing titanium dioxide, method for preparing the same and catalytic compositions thereof |
| KR20040100327A (en) * | 2003-05-22 | 2004-12-02 | 김선재 | Preparation Method of Titanium Dioxide Powder with Large Specific Surface Area Using Indirect Neutralization |
| CN1579946A (en) * | 2003-08-05 | 2005-02-16 | 拉萨绿能科技实业有限公司 | New process for preparing anatase type nano titanium dioxide |
| JP2005138008A (en) * | 2003-11-05 | 2005-06-02 | National Institute For Materials Science | Visible light responding type titanium oxide composite photocatalyst and its manufacturing method |
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