CN102126749A - Titanium dioxide nano powder and preparation method thereof - Google Patents
Titanium dioxide nano powder and preparation method thereof Download PDFInfo
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- CN102126749A CN102126749A CN2011100760364A CN201110076036A CN102126749A CN 102126749 A CN102126749 A CN 102126749A CN 2011100760364 A CN2011100760364 A CN 2011100760364A CN 201110076036 A CN201110076036 A CN 201110076036A CN 102126749 A CN102126749 A CN 102126749A
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Abstract
The invention relates to titanium dioxide nano powder and a preparation method thereof. The technical scheme comprises the following steps of: mixing 10 to 40 weight percent of titanium dioxide, 20 to 50 weight percent of boric acid and 20 to 40 weight percent of alkali carbonate; heating to the temperature of between 900 and 1,100 DEG C at the heating rate of 5 to 15 DEG C/minute; preserving the heat for 0.5 to 3 hours to obtain a uniform melt; cooling the uniform melt by a double-roller cooling method to obtain amorphous glass flakes, or performing water quenching on the uniform melt to obtain amorphous glass particles; preserving the heat of the amorphous glass flakes or the amorphous glass particles at the temperature of between 500 and 620 DEG C for 0.5 to 3 hours; and washing with diluted acid and deionized water and drying to obtain the titanium dioxide nano powder. The powder and the preparation method have the characteristics of simple process, low cost and controllable preparation process and contribute to environmental friendliness; the prepared powder has the particle diameter of between 20 and 80nm; and a powder product has high purity and uniform particle size distribution.
Description
Technical field
The invention belongs to the titanium dioxide powder technical field.Be specifically related to a kind of nano TiO 2 powder and preparation method thereof.
Background technology
Nano titanium oxide relies on excellent photocatalysis performance, thermal property, mechanical property and electric property etc., is with a wide range of applications at numerous areas such as photochemical catalysis, sewage disposal, gas sweetening, makeup, modified paint and fine ceramics.
At present, the method for preparing nano titanium oxide has a lot, can be divided into solid phase method, vapor phase process, liquid phase method etc. according to physical properties.These methods all come with some shortcomings to some extent.Solid phase method such as ball milled, mechanical crushing method etc., though can obtain the titanium dioxide granule of nano particle size, process such as grain growth, reunion is difficult to control in preparation process, will greatly influence its physical and chemical performance and practical application subsequently.Liquid phase method such as hydrothermal method, sol-gel method, the precipitator method etc., raw material sources are extensive, with low cost, also are convenient to scale operation, but liquid phase method easily causes local granule excessive concentration in the reaction process, particle size and distribution of shapes are unequal, influence the performance and the range of application of product.And liquid phase method is in preparation process, and the acid of adding for regulation system pH value, alkali etc. not only increased the complexity of production process and the cost of preparing product, and reacted wastewater can pollute to surrounding enviroment.Vapor phase process such as sputtering method, plasma method, laser chemistry method etc., though be swift in response, vapor phase process all has very high requirement to equipment configuration, type of heating and feeding manner etc., and further scale operation also need solve a series of equipment and engineering problem.
In sum, at present at the preparation method of nano TiO 2 powder, there are complex process, cost height, preparation process and nano-powder particle size and pattern is wayward, easily cause defective such as environmental pollution.
Summary of the invention
The present invention is intended to overcome the deficiency that prior art exists, and purpose provides that a kind of technology is simple, cost is low, preparation process is controlled and helps the preparation method of the nano TiO 2 powder of environment protection; Nano TiO 2 powder purity height and even particle size distribution with this method preparation.
For achieving the above object, technical scheme of the present invention is: earlier the titanium dioxide of 10～40wt%, the boric acid of 20～50wt% and the alkaline carbonate of 20～40wt% are mixed, be heated to 900～1100 ℃ with 5～15 ℃/minute temperature rise rates, be incubated 0.5～3 hour, obtain even melt; Again even melt is adopted the cooling of pair roller method of cooling, obtain the amorphous glass scale, or more even melt is carried out shrend, obtain the amorphous glass particle; Then amorphous glass scale or amorphous glass particle being incubated 0.5～3 hour under 500～620 ℃ of conditions, is that 10% diluted acid and deionized water wash with volume content successively, and drying promptly gets nano TiO 2 powder.
In the technique scheme: the waste water that washing process produced is after distillation, and the gained powder reuses as raw material by stoichiometry; Alkaline carbonate is a yellow soda ash or for salt of wormwood or be the mixture of yellow soda ash and salt of wormwood;
Diluted acid is a dilute hydrochloric acid or for dilute acetic acid or be the mixture of dilute hydrochloric acid and dilute acetic acid.
Because adopt technique scheme, nano TiO 2 powder preparation method's provided by the present invention outstanding feature is:
1, preparation technology is simple, does not need expensive equipment, and raw material is easy to obtain;
2, preparation process is easy to control, and parameters such as crystal formation, grain morphology and particle diameter can be regulated by changing thermal treatment temp and time, make anatase-like titanium dioxide nanometer powder or red schorl type titanium oxide nano powder, and particle diameter is 20～80nm;
3, utilize separating out of glass network structure control nanocrystal, particle is separate existence in crystallisation process;
4, powder product purity height, even particle size distribution;
5, help environment protection, the waste water that produces in the powder washing process powder preparing that is used for capable of circulation.
Therefore, the present invention has the advantages that technology is simple, cost is low, preparation process is controlled and help environment protection, prepared powder product purity height and even particle size distribution.
Embodiment
The present invention will be further described below in conjunction with embodiment, is not the restriction to its protection domain.
Embodiment 1
A kind of nano TiO 2 powder and preparation method thereof.Earlier the titanium dioxide of 10～19wt%, the boric acid of 41～50wt% and the yellow soda ash of 35～40wt% are mixed, be heated to 900～1000 ℃, be incubated 0.5～1.5 hour, obtain even melt with 5～10 ℃/minute temperature rise rates; Again even melt is obtained the amorphous glass particle after shrend; Then the amorphous glass particle being incubated 0.5～1.5 hour under 500～570 ℃ of conditions, is that 10% dilute hydrochloric acid and deionized water wash with volume content successively, and drying promptly gets anatase-like titanium dioxide nanometer powder.
The waste water that above-mentioned washing process produced is after distillation, and the gained powder reuses as raw material by stoichiometry.
The particle diameter of present embodiment 1 prepared anatase-like titanium dioxide nanometer powder is 50～80nm, this powder product purity height and even particle size distribution.
Embodiment 2
A kind of nano TiO 2 powder and preparation method thereof.Earlier the titanium dioxide of 18～36wt%, the boric acid of 33～50wt% and the salt of wormwood of 30～40wt% are mixed, be heated to 1000～1100 ℃, be incubated 1～3 hour, obtain even melt with 10-15 ℃/minute temperature rise rate; Again even melt is adopted the cooling of pair roller method of cooling to obtain the amorphous glass scale; Then the amorphous glass scale being incubated 1～3 hour under 580～620 ℃ of conditions, is that 10% dilute acetic acid and deionized water wash with volume content successively, and drying promptly gets red schorl type titanium oxide nano powder.
The waste water that above-mentioned washing process produced is after distillation, and the gained powder reuses as raw material by stoichiometry.
The particle diameter of present embodiment 2 prepared red schorl type titanium oxide nano powders is 30～70nm, this powder product purity height and even particle size distribution.
Embodiment 3
A kind of nano TiO 2 powder and preparation method thereof.Earlier the titanium dioxide of 35～40wt%, the boric acid of 25～40wt% and the salt of wormwood of 20～35wt% are mixed with yellow soda ash, be heated to 950～1100 ℃, be incubated 2～3 hours, obtain even melt with 8-12 ℃/minute temperature rise rate; Again even melt is adopted the cooling of pair roller method of cooling to obtain the amorphous glass scale, then the amorphous glass scale is incubated 0.5～1 hour under 500～550 ℃ of conditions, be that 10% the dilute hydrochloric acid and the mixing solutions and the deionized water of dilute acetic acid wash successively with volume content, dry, promptly get anatase-like titanium dioxide nanometer powder
In the present embodiment 3: the waste water that washing process produced is after distillation, and the gained powder reuses as raw material by stoichiometry; The mol ratio of salt of wormwood and yellow soda ash is (4: 6)～(7: 3); The volume ratio of dilute hydrochloric acid and dilute acetic acid is (3: 7)～(7: 3).
The particle diameter of present embodiment 3 prepared anatase-like titanium dioxide nanometer powders is 20～50nm, this powder product purity height and even particle size distribution.
Embodiment 4
A kind of nano TiO 2 powder and preparation method thereof.Earlier the titanium dioxide of 30～40wt%, the boric acid of 20～32wt% and the yellow soda ash of 30～40wt% are mixed, be heated to 900～1050 ℃, be incubated 0.5～1 hour, obtain even melt with 10-15 ℃/minute temperature rise rate; Again even melt is obtained the amorphous glass particle after shrend; Then the amorphous glass particle being incubated 0.5～1 hour under 500～530 ℃ of conditions, is that 10% dilute hydrochloric acid and deionized water wash with volume content successively, and drying promptly gets anatase-like titanium dioxide nanometer powder,
The waste water that above-mentioned washing process produced is after distillation, and the gained powder reuses as raw material by stoichiometry.
The particle diameter of present embodiment 4 prepared anatase-like titanium dioxide nanometer powders is 30～60nm, this powder product purity height and even particle size distribution.
This embodiment has following positively effect:
1, preparation technology is simple, does not need expensive equipment, and raw material is easy to obtain;
2, preparation process is easy to control, and parameters such as crystal formation, grain morphology and particle diameter can be regulated by changing thermal treatment temp and time, make anatase-like titanium dioxide nanometer powder or red schorl type titanium oxide nano powder, and particle diameter is 20～80nm;
3, utilize separating out of glass network structure control nanocrystal, particle is separate existence in crystallisation process;
4, powder product purity height, even particle size distribution;
5, help environment protection, the waste water that produces in the powder washing process powder preparing that is used for capable of circulation.
This embodiment has the advantages that technology is simple, cost is low, preparation process is controlled and help environment protection, prepared powder product purity height and even particle size distribution.
Claims (4)
1. the preparation method of a nano TiO 2 powder, it is characterized in that earlier the titanium dioxide of 10～40wt%, the boric acid of 20～50wt% and the alkaline carbonate of 20～40wt% being mixed, be heated to 900～1100 ℃ with 5～15 ℃/minute temperature rise rates, be incubated 0.5～3 hour, obtain even melt; Again even melt is adopted the cooling of pair roller method of cooling, obtain the amorphous glass scale, or more even melt is carried out shrend, obtain the amorphous glass particle; Then amorphous glass scale or amorphous glass particle being incubated 0.5～3 hour under 500～620 ℃ of conditions, is that 10% diluted acid and deionized water wash with volume content successively, and drying promptly gets nano TiO 2 powder.
2. the preparation method of nano TiO 2 powder according to claim 1 is characterized in that described alkaline carbonate is a yellow soda ash or for salt of wormwood or be the mixture of yellow soda ash and salt of wormwood.
3. the preparation method of nano TiO 2 powder according to claim 1 is characterized in that described diluted acid is a dilute hydrochloric acid or for dilute acetic acid or be the mixture of dilute hydrochloric acid and dilute acetic acid.
4. according to the prepared nano TiO 2 powder of preparation method of each described nano TiO 2 powder in the claim 1～3.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103508489A (en) * | 2012-06-21 | 2014-01-15 | 深圳富泰宏精密工业有限公司 | Nanometer titanium dioxide preparation apparatus and preparation method for nanometer titanium dioxide dioxideby using same |
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| JP2004174747A (en) * | 2002-11-25 | 2004-06-24 | Fuji Photo Film Co Ltd | Inkjet recording sheet |
| CN1569646A (en) * | 2003-09-30 | 2005-01-26 | 河北理工学院 | Method for preparing TiO2 nano materials by fusion-split phase method |
| CN101564688A (en) * | 2009-02-24 | 2009-10-28 | 福建工程学院 | Method for preparing titanic oxide nano composited tube |
| CN101654280A (en) * | 2009-08-25 | 2010-02-24 | 苏州大学 | Preparation method of titanium dioxide nano powder |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004174747A (en) * | 2002-11-25 | 2004-06-24 | Fuji Photo Film Co Ltd | Inkjet recording sheet |
| CN1569646A (en) * | 2003-09-30 | 2005-01-26 | 河北理工学院 | Method for preparing TiO2 nano materials by fusion-split phase method |
| CN101564688A (en) * | 2009-02-24 | 2009-10-28 | 福建工程学院 | Method for preparing titanic oxide nano composited tube |
| CN101654280A (en) * | 2009-08-25 | 2010-02-24 | 苏州大学 | Preparation method of titanium dioxide nano powder |
Non-Patent Citations (1)
| Title |
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| 《功能材料》 20051130 Zhang Wen-li et al. Effects of heat treatment temperature on the preparation of nanometer TiO2 by melt-phase separation process 第1802-1805页 1-4 第36卷, 第11期 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103508489A (en) * | 2012-06-21 | 2014-01-15 | 深圳富泰宏精密工业有限公司 | Nanometer titanium dioxide preparation apparatus and preparation method for nanometer titanium dioxide dioxideby using same |
| CN103508489B (en) * | 2012-06-21 | 2016-08-10 | 深圳富泰宏精密工业有限公司 | Nano titanium oxide preparation facilities and apply the method that this device prepares nano titanium oxide |
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