CN102126750A - Preparation method of anatase nano titanium dioxide - Google Patents
Preparation method of anatase nano titanium dioxide Download PDFInfo
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- CN102126750A CN102126750A CN 201010616269 CN201010616269A CN102126750A CN 102126750 A CN102126750 A CN 102126750A CN 201010616269 CN201010616269 CN 201010616269 CN 201010616269 A CN201010616269 A CN 201010616269A CN 102126750 A CN102126750 A CN 102126750A
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Abstract
The invention discloses a preparation method of anatase nano titanium dioxide. The method comprises the following steps of: adding titanium tetrachloride or other titanium alkoxides and a catalyst into an organic solvent, adding a crystal form control agent and heating to 50-300 DEG C; preserving heat for 0.5-5 hours to obtain titanium oxide bulk gel; putting the titanium oxide bulk gel into a drier for drying; putting dried powder into water and adding the crystal form control agent; heating to over 50 DEG C and preserving heat for over 1.5 hours; separating nano titanium dioxide particles out by using a centrifuge; soaking the separated nano titanium dioxide particles in the organic solvent, fully stirring and separating nano titanium dioxide particles out by using a high-speed centrifuge; and soaking water-washed nano titanium dioxide particles in purified water and adding a dispersion stabilizer. By adopting the method, the nano titanium dioxide particles do not need to be dried or separated and are directly separated in liquid by using the centrifuge, so that the nano titanium dioxide particles have high dispersity in liquid.
Description
Technical field
The present invention relates to the preparation method of anatase-type nanometer titanium dioxide.
Background technology
In the prior art, following method preparation is adopted in the preparation of anatase-type nanometer titanium dioxide usually:
Gas phase hydrolysis method:
Gas phase hydrolysis method utilizes nitrogen, oxygen or air to do carrier gas, and TiCl4 or titanium alkoxide steam and water vapour are imported reactor respectively, carries out moment and mixes quick hydrolysis reaction.Wait crystal formation and the particle diameter of regulating nanometer Ti O2 by the residence time, concentration, flow velocity and the temperature of reaction that changes all gases.
Liquid phase method:
Sol-gel method is a raw material with titanium alkoxide Ti (OR) 4, through hydrolysis and polycondensation process and gelation gradually can obtain nanometer Ti O2 particle through cryodrying, sintering processes again.Product purity height, the particle diameter that this method makes is little, size is even, the sintering temperature of dry back particle self is low; But expensive raw material price, production cost height, coking property is poor between the gel particle, shrinks big when product is dry.
Chemical precipitation method:
Chemical precipitation method adds Ti OSO4 with precipitation agent, and in H2 Ti O3 or TiCl 4 solution, post precipitation is heat-treated.
Hydrolysis method:
Hydrolysis method is a raw material with titanium tetrachloride or titanium alkoxide, makes nanometer Ti O2 through hydrolysis, neutralization, washing, oven dry and roasting.Product purity height, particle diameter that this method makes are even; But hydrolysis rate is fast, the reaction difficulty is controlled, cost is big, energy consumption is high, be difficult to suitability for industrialized production.
Hydrothermal method:
Hydrothermal method is with Ti OSO4, and TiCl 4 or Ti (OR) 4 is raw material, under the High Temperature High Pressure in the aqueous solution synthesis of nano Ti O2.
Nano titanium oxide can not be made pulverulence, can not be in good distribution after the drying; Cost is higher.
Summary of the invention
The objective of the invention is to,, provide a kind of preparation method of anatase-type nanometer titanium dioxide at the above-mentioned defective of prior art.
A kind of preparation method of anatase-type nanometer titanium dioxide is provided, comprises the steps:
1) reaction: in titanium tetrachloride or other titanium alkoxide and catalyzer adding organic solvent, add the crystal formation control agent, be heated to 50-300 ℃; Kept 0.5-5 hour, and obtained the block gel of titanium oxide;
2) oven dry: the block gel of titanium oxide is put into drying machine dry;
3) hydrolysis: the powder after will drying is put into water, adds the crystal formation control agent; Be heated to more than 50 ℃, keep more than 1.5 hours;
4) separate: isolate nano-titania particle with whizzer;
5) washing: isolated nano-titania particle is soaked with organic solvent, and fully stir, and then isolate nano-titania particle with supercentrifuge; This step can repeatedly repeat as required;
6) disperse: the nano-titania particle after will washing is soaked in the pure water, and adds dispersion stabilizer.
Present technique similar and liquid phase method and hydrolysis method, but with any all different, and overcome its shortcoming.
Advantage of the present invention: particle diameter is little, may command, and the nano-titania particle aggregate particle size is the 5-50 nanometer.Crystal formation is controlled well, and Detitanium-ore-type is 100% in the nano-titania particle.Less investment, low for equipment requirements, energy consumption is low.Pollute and lack, use the acidic liquid during except that cleaning, pollution-free substantially.
Effect of the present invention: air purification function: can degrade and eliminate all organic pollutants and part inorganic pollutant in the air.Sterilizing function: can kill bacteriums such as intestinal bacteria, staphylococcus aureus, the harmful mixture that discharges on simultaneously can also the decomposing bacteria dead volume.Self-cleaning function: nano titanium oxide has Superhydrophilic, can prevent absorption such as oil smoke, vehicle exhaust.Water purification function: the organic objectionable impurities in the energy degradation water, thus purify water.Increase the function of negative oxygen ion concentration: nano titanium oxide can produce negative oxygen ion under illumination, can increase negative oxygen ion concentration in the forest as thunderstorm, thereby make air more pure and fresh; Can be used as purple light absorbers; Can be used as the additive of fungicidal paint, light catalyzed coating, chalking paint.
Main component of the present invention is anatase-type nanometer titanium dioxide, solvent (water or other organic solvents).
After the nano titanium oxide absorb light energy, the electronics in the valence band will be excited to conduction band, forms electronegative high reactivity electronics e-, produces the hole h+ of positively charged simultaneously on valence band.Under effect of electric field, electronics separates with the hole, moves to the different positions of particle surface.Thermodynamic argument shows, the h+ that is distributed in the surface can change into (.OH) free radical with being adsorbed on TiO2 surface OH-and H2O molecular oxygen, and the oxidation capacity of .OH free radical is the strongest in the oxygenant that exists in the water body, can oxidation also decompose various organic pollutants (formaldehyde, benzene, TVOC etc.) and bacterium and part inorganic pollutant (ammonia, NOX etc.), and be innoxious substances such as CO2, H2O eventual degradation.Because .OH radical pair reactant non-selectivity almost, thus in photochemical catalysis decisive role.In addition, many organic oxidizing potentials are more negative than the valence band current potential of TiO2, can directly be the oxidation of h+ institute.And the highly active e-side in TiO2 surface has very strong reducing power, can reduce and remove metal ion in the water body.Use above principle photocatalyst and be widely used in fields such as sterilization, deodorizing, purifying air, sewage disposal.
Similar liquid phase method of present technique and hydrolysis method, but with any all different, and overcome its shortcoming.Sol-gel method (liquid phase method) is a raw material with titanium alkoxide Ti (OR) 4, through hydrolysis and polycondensation process and gelation gradually can obtain the nano TiO 2 particle through cryodrying, sintering processes again.
Hydrolysis method is a raw material with titanium tetrachloride or titanium alkoxide, makes nanometer Ti O2 through hydrolysis, neutralization, washing, oven dry and roasting.
The particle diameter that liquid phase method and hydrolysis method are produced is bigger, and wayward, and the nano-titania particle of producing is difficult for disperseing.Present technique is with in titanium tetrachloride or other titanium alkoxide and the catalyzer adding organic solvent, controls reaction by adding the crystal formation control agent.Present technique must be with the dry separation of nano-titania particle; Be directly in liquid, to separate by whizzer; So nano-titania particle dispersed fine in liquid.
Embodiment
Embodiment one: 1) titanium tetrachloride or other titanium alkoxide and catalyzer (sodium sulphate) and acid reactant (example hydrochloric acid, acetate) are added in the organic solvent, add crystal formation control agent (if biphosphate is received, sodium bicarbonate), be heated to 50 ℃; Kept 4 hours, and obtained the block gel of titanium oxide;
2) oven dry: the block gel of titanium oxide is put into drying machine dry;
3) hydrolysis: the powder after will drying is put into water, adds the crystal formation control agent; Be heated to more than 50 ℃, keep more than 1.5 hours;
4) separate: isolate nano-titania particle with whizzer;
5) washing: isolated nano-titania particle is soaked with organic solvent, and fully stir, and then isolate nano-titania particle with supercentrifuge; This step can repeatedly repeat as required;
6) disperse: the nano-titania particle after will washing is soaked in the pure water, and adds dispersion stabilizer.
Embodiment two: a kind of preparation method of anatase-type nanometer titanium dioxide is provided, comprises the steps:
1) reaction: titanium tetrachloride or other titanium alkoxide and reactant, catalyzer are added in the organic solvent, and interpolation crystal formation control agent is heated to 150 ℃; Kept 3 hours, and obtained the block gel of titanium oxide;
2) oven dry: the block gel of titanium oxide is put into drying machine dry;
3) hydrolysis: the powder after will drying is put into water, adds the crystal formation control agent; Be heated to more than 50 ℃, keep more than 1.5 hours;
4) separate: isolate nano-titania particle with whizzer;
5) washing: isolated nano-titania particle is soaked with organic solvent, and fully stir, and then isolate nano-titania particle with supercentrifuge; This step can repeatedly repeat as required;
6) disperse: the nano-titania particle after will washing is soaked in the pure water, and adds dispersion stabilizer.
Embodiment three: a kind of preparation method of anatase-type nanometer titanium dioxide is provided, comprises the steps:
1) reaction: titanium tetrachloride or other titanium alkoxide and reactant, catalyzer are added in the organic solvent, and interpolation crystal formation control agent is heated to 200 ℃; Kept 2 hours, and obtained the block gel of titanium oxide;
2) oven dry: the block gel of titanium oxide is put into drying machine dry;
3) hydrolysis: the powder after will drying is put into water, adds the crystal formation control agent; Be heated to more than 150 ℃, keep more than 1.5 hours;
4) separate: isolate nano-titania particle with whizzer;
5) washing: isolated nano-titania particle is soaked with organic solvent, and fully stir, and then isolate nano-titania particle with supercentrifuge; This step can repeatedly repeat as required;
6) disperse: the nano-titania particle after will washing is soaked in the pure water, and adds dispersion stabilizer.
Claims (3)
1. the preparation method of an anatase-type nanometer titanium dioxide is characterized in that, comprises the steps:
1) reaction: in titanium tetrachloride or other titanium alkoxide and catalyzer adding organic solvent, add the crystal formation control agent, be heated to 50-300 ℃; Kept 0.5-5 hour, and obtained the block gel of titanium oxide;
2) oven dry: the block gel of titanium oxide is put into drying machine dry;
3) hydrolysis: the powder after will drying is put into water, adds the crystal formation control agent; Be heated to more than 50 ℃, keep more than 1.5 hours;
4) separate: isolate nano-titania particle with whizzer;
5) washing: isolated nano-titania particle is soaked with organic solvent, and fully stir, and then isolate nano-titania particle with supercentrifuge; This step can repeatedly repeat as required;
6) disperse: the nano-titania particle after will washing is soaked in the pure water, and adds dispersion stabilizer.
2. the preparation method of anatase-type nanometer titanium dioxide according to claim 1 is characterized in that, comprises the steps:
1) reaction: titanium tetrachloride or other titanium alkoxide and reactant, catalyzer are added in the organic solvent, and interpolation crystal formation control agent is heated to 50 ℃; Kept 5 hours, and obtained the block gel of titanium oxide;
2) oven dry: the block gel of titanium oxide is put into drying machine dry;
3) hydrolysis: the powder after will drying is put into water, adds the crystal formation control agent; Be heated to more than 50 ℃, keep more than 1.5 hours;
4) separate: isolate nano-titania particle with whizzer;
5) washing: isolated nano-titania particle is soaked with organic solvent, and fully stir, and then isolate nano-titania particle with supercentrifuge; This step can repeatedly repeat as required;
6) disperse: the nano-titania particle after will washing is soaked in the pure water, and adds dispersion stabilizer.
3. the preparation method of anatase-type nanometer titanium dioxide according to claim 1 is characterized in that, comprises the steps:
1) reaction: titanium tetrachloride or other titanium alkoxide and reactant, catalyzer are added in the organic solvent, and interpolation crystal formation control agent is heated to 150 ℃; Kept 3 hours, and obtained the block gel of titanium oxide;
2) oven dry: the block gel of titanium oxide is put into drying machine dry;
3) hydrolysis: the powder after will drying is put into water, adds the crystal formation control agent; Be heated to more than 50 ℃, keep more than 1.5 hours;
4) separate: isolate nano-titania particle with whizzer;
5) washing: isolated nano-titania particle is soaked with organic solvent, and fully stir, and then isolate nano-titania particle with supercentrifuge; This step can repeatedly repeat as required;
6) disperse: the nano-titania particle after will washing is soaked in the pure water, and adds dispersion stabilizer.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102329546A (en) * | 2011-10-26 | 2012-01-25 | 东莞市明天纳米科技有限公司 | Wall paint containing nano-titanium dioxide and preparation method for wall paint |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2568626Y (en) * | 2002-08-22 | 2003-08-27 | 西北有色金属研究院 | Appts. for prepn. of anatase type nano titania sol |
| CN1593749A (en) * | 2004-07-05 | 2005-03-16 | 华东理工大学 | Process for preparing nanometer titanium dioxide membrane photocatalyst |
| US20090291044A1 (en) * | 2008-05-26 | 2009-11-26 | Korea Research Institute Of Chemical Technology | ANATASE TYPE TiO2 NANORODS AND ITS PREPARATION METHOD |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2568626Y (en) * | 2002-08-22 | 2003-08-27 | 西北有色金属研究院 | Appts. for prepn. of anatase type nano titania sol |
| CN1593749A (en) * | 2004-07-05 | 2005-03-16 | 华东理工大学 | Process for preparing nanometer titanium dioxide membrane photocatalyst |
| US20090291044A1 (en) * | 2008-05-26 | 2009-11-26 | Korea Research Institute Of Chemical Technology | ANATASE TYPE TiO2 NANORODS AND ITS PREPARATION METHOD |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102329546A (en) * | 2011-10-26 | 2012-01-25 | 东莞市明天纳米科技有限公司 | Wall paint containing nano-titanium dioxide and preparation method for wall paint |
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Address after: 523000 No. 29 Dazhou Industrial North Road, Shangjia Community, Wanjiang Street, Dongguan City, Guangdong Province Patentee after: Guangdong Modern Coatings Technology Co., Ltd. Address before: 523000 Shangjia Community Industrial Zone, Wanjiang District, Dongguan City, Guangdong Province Patentee before: Dongguan Tomorrow Nano Science and Technology Co., Ltd. |