CN102086046A - Preparation method of nano-TiO2 lyosol - Google Patents
Preparation method of nano-TiO2 lyosol Download PDFInfo
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- CN102086046A CN102086046A CN2010106162783A CN201010616278A CN102086046A CN 102086046 A CN102086046 A CN 102086046A CN 2010106162783 A CN2010106162783 A CN 2010106162783A CN 201010616278 A CN201010616278 A CN 201010616278A CN 102086046 A CN102086046 A CN 102086046A
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Abstract
The invention discloses a preparation method of nano-TiO2 lyosol. The method comprises the following steps: adding titanium tetrachloride or another titanium alkoxide and catalyst in organic solvent, adding crystalline control agent, heating to 50 DEG C, keeping for 5 hours to obtain titanium oxide massive gel; drying the titanium oxide massive gel in a dryer; placing the dried powder in water, adding crystalline control agent; heating to more than 50 DEG C, keeping for more than 1.5; using a centrifugal machine to separate out nano-TiO2 particles; soaking the separated nano-TiO2 particles in organic solvent, fully stirring, then using a high speed centrifuge to separate out nano-TiO2 particles, wherein the step can be repeated several times according to need; and soaking the rinsed nano-TiO2 particles in purified water, and adding dispersion stabilizer. The prepared nano-TiO2 lyosol can be used to purify the air and degrade and eliminate all the organic pollutants and partial inorganic pollutants in the air; and the nano-TiO2 lyosol also has the function of killing bacteria, namely the lyosol can kill Escherichia coli.
Description
Technical field
The present invention relates to the preparation method of nano titanium oxide lyosol.
Background technology
In the prior art, the preparation method of nano titanium oxide lyosol adopts following method to carry out usually.
1, 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 nano TiO 2 by the residence time, concentration, flow velocity and the temperature of reaction that changes all gases.
2, 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 the nano TiO 2 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.
3, chemical precipitation method
Chemical precipitation method adds TiOSO4 with precipitation agent, and in H2 TiO3 or the TiCl4 solution, post precipitation is heat-treated.
4, hydrolysis method
Hydrolysis method is a raw material with titanium tetrachloride or titanium alkoxide, makes nano TiO 2 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.
5, hydrothermal method
Hydrothermal method is with TiOSO4, and TiCl4 or Ti (OR) 4 is raw material, under the High Temperature High Pressure in the aqueous solution synthesis of nano TiO2.
Adopt the nano titanium oxide lyosol of method for preparing to be acid; Nano-titania particle can not be dispersed in the most organic solvent; When adding alkalescence or other chemical substances in lyosol, nano-titania particle easily flocculates.
Summary of the invention
The objective of the invention is to,, provide a kind of preparation method of new nano titanium oxide lyosol at the above-mentioned defective of prior art.
A kind of preparation method of nano titanium oxide lyosol is provided, comprises the steps:
1) reaction: titanium tetrachloride or other titanium alkoxide are added in the organic solvent with catalyzer (sodium sulfate) and acid reactant (example hydrochloric acid, acetate), add crystal formation control agent (SODIUM PHOSPHATE, MONOBASIC or sodium bicarbonate), 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, is heated to more than 50 ℃, keeps 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.
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 nano TiO 2 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.
Advantage of the present invention: cost is low, particle diameter is little, and the nano-titania particle aggregate particle size is the 2-8 nanometer, and it is wide to absorb the luminous energy wavelength region, crystal formation is controlled well, in the lyosol in the nano-titania particle Detitanium-ore-type be 100%, 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 intestinal bacteria, bacteriums such as 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 oil smoke, absorption such as vehicle exhaust, water purification function: the organic objectionable impurities in the energy degradation water, thereby 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.
The main component of nano titanium oxide lyosol is nano titanium oxide, solvent (water or other organic solvents).Nano-titania particle is positive electricity in liquid phase, particle repels mutually, never precipitates, flocculates under no external force situation.
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.
Embodiment
Embodiment one: the preparation process of nano titanium oxide lyosol:
1) reaction: in titanium tetrachloride or other titanium alkoxide and catalyzer adding organic solvent, add the crystal formation control agent, be 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 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 nano titanium oxide lyosol 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 300 ℃.Kept 0.5 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.
Embodiment three: a kind of preparation method of nano titanium oxide lyosol 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 ℃.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.
Claims (4)
1. the preparation method of a nano titanium oxide lyosol 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, obtain 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 nano titanium oxide lyosol according to claim 1 is characterized in that, 1) and reaction: in titanium tetrachloride or other titanium alkoxide and catalyzer adding organic solvent, add the crystal formation control agent, be heated to 200 ℃, kept 2 hours, obtain 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 nano titanium oxide lyosol according to claim 1 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 300 ℃; Kept 0.5 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.
4. the preparation method of nano titanium oxide lyosol according to claim 1 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 ℃; 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.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105080525A (en) * | 2015-08-17 | 2015-11-25 | 广州叶子环保科技有限公司 | Preparation method of visible light nanometer titania photocatalyst sol |
| CN105831154A (en) * | 2016-04-07 | 2016-08-10 | 济南钛盾生物科技有限公司 | Titanium dioxide antibacterial sol and preparation method thereof |
| CN109107555A (en) * | 2018-08-04 | 2019-01-01 | 山东迅达化工集团有限公司 | The preparation method of titania support |
| CN110436792A (en) * | 2019-08-21 | 2019-11-12 | 吉林大学 | A method of preparing the quartz capillary with titanium dioxide nano-particle coating |
Citations (5)
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| CN1594102A (en) * | 2004-07-05 | 2005-03-16 | 华东理工大学 | Method for preparing titanium dioxide mesoporous material |
| US20060019028A1 (en) * | 2004-07-22 | 2006-01-26 | Yeung King L | Novel TiO2 material and the coating methods thereof |
| CN1778685A (en) * | 2005-10-14 | 2006-05-31 | 浙江大学 | Production of titanium dioxide optical catalyst sol |
| CN101049961A (en) * | 2007-05-18 | 2007-10-10 | 广东省生态环境与土壤研究所 | Method for preparing sol of high active Nano titanium dioxide |
| JP2009227515A (en) * | 2008-03-24 | 2009-10-08 | Teruhisa Yokono | Method for producing titanium oxide particle and titanium oxide particle |
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2010
- 2010-12-31 CN CN2010106162783A patent/CN102086046A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1594102A (en) * | 2004-07-05 | 2005-03-16 | 华东理工大学 | Method for preparing titanium dioxide mesoporous material |
| US20060019028A1 (en) * | 2004-07-22 | 2006-01-26 | Yeung King L | Novel TiO2 material and the coating methods thereof |
| CN1778685A (en) * | 2005-10-14 | 2006-05-31 | 浙江大学 | Production of titanium dioxide optical catalyst sol |
| CN101049961A (en) * | 2007-05-18 | 2007-10-10 | 广东省生态环境与土壤研究所 | Method for preparing sol of high active Nano titanium dioxide |
| JP2009227515A (en) * | 2008-03-24 | 2009-10-08 | Teruhisa Yokono | Method for producing titanium oxide particle and titanium oxide particle |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105080525A (en) * | 2015-08-17 | 2015-11-25 | 广州叶子环保科技有限公司 | Preparation method of visible light nanometer titania photocatalyst sol |
| CN105831154A (en) * | 2016-04-07 | 2016-08-10 | 济南钛盾生物科技有限公司 | Titanium dioxide antibacterial sol and preparation method thereof |
| CN105831154B (en) * | 2016-04-07 | 2018-08-24 | 济南钛盾生物科技有限公司 | A kind of titanium dioxide antibiotic colloidal sol and preparation method thereof |
| CN109107555A (en) * | 2018-08-04 | 2019-01-01 | 山东迅达化工集团有限公司 | The preparation method of titania support |
| CN110436792A (en) * | 2019-08-21 | 2019-11-12 | 吉林大学 | A method of preparing the quartz capillary with titanium dioxide nano-particle coating |
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Application publication date: 20110608 |