CN101279766A - Preparation of spherical nano-titanic oxide - Google Patents
Preparation of spherical nano-titanic oxide Download PDFInfo
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- CN101279766A CN101279766A CNA2008100180526A CN200810018052A CN101279766A CN 101279766 A CN101279766 A CN 101279766A CN A2008100180526 A CNA2008100180526 A CN A2008100180526A CN 200810018052 A CN200810018052 A CN 200810018052A CN 101279766 A CN101279766 A CN 101279766A
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Abstract
Disclosed is a process for preparing a spherical nano-titanium dioxide, which takes citric acid, titanium sulfate and polyethylene glycol as materials and adopts a mixture of deionized water and absolute ethyl alcohol mixture as a solvent to prepare a precursor, and a spherical nano-titanium dioxide powder is prepared through the gelatinization by a water bath at a temperature of 80 DEG C, drying and foaming at a temperature of 140 DEG C and calcinations at a temperature of between 600 and 900 DEG C, and sizes of the crystal grains are between 100 and 300nm. The titanium dioxide particles prepared by the invention are all complete solid ball bodies with smooth surfaces, high purity and good dispersity, and the process has advantages of short preparation cycle, rather high yield, simple process, small equipment investment and low cost.
Description
Technical field
The present invention relates to a kind of preparation method of titanium dioxide powder, particularly the preparation method of spherical nano TiO 2 powder.
Background technology
Nano titanium oxide not only is widely used in fields such as coating, filler, plastics, makeup, also is applied to fields such as electronic material, photoelectrocatalysis agent, transmitter, semi-conductor, display material.Particularly for gentle version indicating meter, titanium dioxide granule dielectric coefficient height, specific refractory power height, color and luster is pure white, chemical stability good, it is a kind of ideal white colour developing particle, and, spherical solid titanium dioxide granule electrophoresis resistance is little, can avoid owing to the inconsistent particle spin that causes of actual center gravity and profile center, more help colour developing and the electrophoresis of particle in solution, studies show that, as electric ink white colour developing particle, the grain-size optimum value of titanium dioxide granule is between 200～500nm.In addition, because the specific surface area of nano titanium oxide is big, very easily reunite, can nano titanium oxide effectively disperse to become key issue.At present, spherical TiO
2The preparation method of powder is a lot, comprises alkoxide sol-gel method, hydrothermal method, hydrolysis method, precipitator method or the like, and wherein most widely used is alkoxide sol-gel method.Though sol-gel method has the good advantage of purity high uniformity, its reaction cost height is difficult to industrial production.
Summary of the invention
The object of the present invention is to provide the preparation method of a kind of powder regular shape of preparing, good dispersity, the simple spherical nano TiO 2 of processing unit.
For achieving the above object, the concrete steps that the present invention adopts are: at first with deionized water and dehydrated alcohol by 1.5～2.3: 1 volume ratio is made into ethanolic soln; The ethanolic soln of at room temperature getting 100ml then mixes to the titanium sulfate of the citric acid that wherein adds 12-17g, 2-3g and the polyoxyethylene glycol of 3.5-5.6g, after the stirring and dissolving, is evaporated to white wet gel 80 ℃ of water-baths; Wet gel is carried out drying foaming 5 hours in 130 ℃～140 ℃ stove, form the xerogel of brownish black; Again xerogel is put into kiln and calcine, the control calcining temperature is 600～900 ℃, and calcining at constant temperature was taken out after 5 hours, obtained spherical solid nano-titanium dioxide powder.
Production technique of the present invention is simple, easy to operate, preparation cycle is short, productive rate is higher (owing to there is not impurity such as introducing chlorion in this preparation process, need not the suction filtration cleaning to remove impurity, can shorten preparation cycle, Lian Jia titanium sulfate will all be converted into titanium dioxide in addition), facility investment is few, cost is low, and (employed material purity is higher in preparation for the purity height of prepared titanium dioxide powder, do not introduce impurity in the preparation process, and used organic substance citric acid, polyoxyethylene glycol is after playing a role, can carbonization in calcination process and remove), citric acid and titanium ion are by the structure of two carboxyls and two chelate rings of a hydroxyl formation, the unsaturated link(age) of titanium ion is at first by the ethanol molecule coordination in the citric acid complex, if there is not ethanol in the solution, then this unsaturated link(age) is had the encirclement of polar water molecules.Because what use during the preparation precursor is the mixing solutions of deionized water and dehydrated alcohol, ethanol molecule combines with the unsaturated link(age) of titanium ion in the complex compound, and in calcination process, the alcoholic acid charing can hinder TiO
2The reunion of powder is so have better dispersiveness and homogeneity.
Its grain-size is the complete solid sphere of 100～300nm, and spherome surface is smooth.Through TG-DTA curve and XRD analysis as can be known, change to anatase titanium dioxide by amorphous in the time of 500 ℃, change to rutile-type by Detitanium-ore-type in the time of 800 ℃.
Embodiment
Embodiment 1, at first deionized water and dehydrated alcohol is made into ethanolic soln by 1.5: 1 volume ratio; The ethanolic soln of at room temperature getting 100ml then mixes to the titanium sulfate of the citric acid that wherein adds 17g, 3g and the polyoxyethylene glycol of 3.5g, after the stirring and dissolving, is evaporated to white wet gel 80 ℃ of water-baths; Wet gel is carried out drying foaming 5 hours in 135 ℃ stove, form the xerogel of brownish black; Again xerogel is put into kiln and calcine, the control calcining temperature is 900 ℃, and calcining at constant temperature was taken out after 5 hours, obtained spherical solid nano-titanium dioxide powder.
Embodiment 2, at first deionized water and dehydrated alcohol are made into ethanolic soln by 1.8: 1 volume ratio; The ethanolic soln of at room temperature getting 100ml then mixes to the titanium sulfate of the citric acid that wherein adds 15g, 2g and the polyoxyethylene glycol of 4g, after the stirring and dissolving, is evaporated to white wet gel 80 ℃ of water-baths; Wet gel is carried out drying foaming 5 hours in 138 ℃ stove, form the xerogel of brownish black; Again xerogel is put into kiln and calcine, the control calcining temperature is 700 ℃, and calcining at constant temperature was taken out after 5 hours, obtained spherical solid nano-titanium dioxide powder.
Embodiment 3, at first deionized water and dehydrated alcohol are made into ethanolic soln by 2.0: 1 volume ratio; The ethanolic soln of at room temperature getting 100ml then mixes to the titanium sulfate of the citric acid that wherein adds 13g, 2.6g and the polyoxyethylene glycol of 5g, after the stirring and dissolving, is evaporated to white wet gel 80 ℃ of water-baths; Wet gel is carried out drying foaming 5 hours in 130 ℃ stove, form the xerogel of brownish black; Again xerogel is put into kiln and calcine, the control calcining temperature is 600 ℃, and calcining at constant temperature was taken out after 5 hours, obtained spherical solid nano-titanium dioxide powder.
Embodiment 4, at first deionized water and dehydrated alcohol are made into ethanolic soln by 2.3: 1 volume ratio; The ethanolic soln of at room temperature getting 100ml then mixes to the titanium sulfate of the citric acid that wherein adds 12g, 2.3g and the polyoxyethylene glycol of 5.6g, after the stirring and dissolving, is evaporated to white wet gel 80 ℃ of water-baths; Wet gel is carried out drying foaming 5 hours in 140 ℃ stove, form the xerogel of brownish black; Again xerogel is put into kiln and calcine, the control calcining temperature is 800 ℃, and calcining at constant temperature was taken out after 5 hours, obtained spherical solid nano-titanium dioxide powder.
Claims (5)
1, a kind of preparation method of spherical nano TiO 2 is characterized in that:
1) at first with deionized water and dehydrated alcohol by 1.5～2.3: 1 volume ratio is made into ethanolic soln;
2) ethanolic soln of at room temperature getting 100ml then mixes to the titanium sulfate of the citric acid that wherein adds 12-17g, 2-3g and the polyoxyethylene glycol of 3.5-5.6g, after the stirring and dissolving, is evaporated to white wet gel 80 ℃ of water-baths;
3) wet gel is carried out drying foaming 5 hours in 130 ℃～140 ℃ stove, form the xerogel of brownish black;
4) again xerogel is put into kiln and calcine, the control calcining temperature is 600～900 ℃, and calcining at constant temperature was taken out after 5 hours, obtained spherical solid nano-titanium dioxide powder.
2, the preparation method of spherical nano TiO 2 according to claim 1 is characterized in that: at first deionized water and dehydrated alcohol are made into ethanolic soln by 1.5: 1 volume ratio; The ethanolic soln of at room temperature getting 100ml then mixes to the titanium sulfate of the citric acid that wherein adds 17g, 3g and the polyoxyethylene glycol of 3.5g, after the stirring and dissolving, is evaporated to white wet gel 80 ℃ of water-baths; Wet gel is carried out drying foaming 5 hours in 135 ℃ stove, form the xerogel of brownish black; Again xerogel is put into kiln and calcine, the control calcining temperature is 900 ℃, and calcining at constant temperature was taken out after 5 hours, obtained spherical solid nano-titanium dioxide powder.
3, the preparation method of spherical nano TiO 2 according to claim 1 is characterized in that: at first deionized water and dehydrated alcohol are made into ethanolic soln by 1.8: 1 volume ratio; The ethanolic soln of at room temperature getting 100ml then mixes to the titanium sulfate of the citric acid that wherein adds 15g, 2g and the polyoxyethylene glycol of 4g, after the stirring and dissolving, is evaporated to white wet gel 80 ℃ of water-baths; Wet gel is carried out drying foaming 5 hours in 138 ℃ stove, form the xerogel of brownish black; Again xerogel is put into kiln and calcine, the control calcining temperature is 700 ℃, and calcining at constant temperature was taken out after 5 hours, obtained spherical solid nano-titanium dioxide powder.
4, the preparation method of spherical nano TiO 2 according to claim 1 is characterized in that: at first deionized water and dehydrated alcohol are made into ethanolic soln by 2.0: 1 volume ratio; The ethanolic soln of at room temperature getting 100ml then mixes to the titanium sulfate of the citric acid that wherein adds 13g, 2.6g and the polyoxyethylene glycol of 5g, after the stirring and dissolving, is evaporated to white wet gel 80 ℃ of water-baths; Wet gel is carried out drying foaming 5 hours in 130 ℃ stove, form the xerogel of brownish black; Again xerogel is put into kiln and calcine, the control calcining temperature is 600 ℃, and calcining at constant temperature was taken out after 5 hours, obtained spherical solid nano-titanium dioxide powder.
5, the preparation method of spherical nano TiO 2 according to claim 1 is characterized in that: at first deionized water and dehydrated alcohol are made into ethanolic soln by 2.3: 1 volume ratio; The ethanolic soln of at room temperature getting 100ml then mixes to the titanium sulfate of the citric acid that wherein adds 12g, 2.3g and the polyoxyethylene glycol of 5.6g, after the stirring and dissolving, is evaporated to white wet gel 80 ℃ of water-baths; Wet gel is carried out drying foaming 5 hours in 140 ℃ stove, form the xerogel of brownish black; Again xerogel is put into kiln and calcine, the control calcining temperature is 800 ℃, and calcining at constant temperature was taken out after 5 hours, obtained spherical solid nano-titanium dioxide powder.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101798110A (en) * | 2010-04-08 | 2010-08-11 | 复旦大学 | Preparation method of spherical nanometer titanium dioxide |
| CN102328952A (en) * | 2011-06-30 | 2012-01-25 | 北京大学 | Preparation method for spherical lithium titanate material |
| CN105753046A (en) * | 2016-05-05 | 2016-07-13 | 陕西科技大学 | Preparation method of porous TiO2 bulk material |
| CN105948805A (en) * | 2016-05-05 | 2016-09-21 | 陕西科技大学 | Preparation method of titanium dioxide porous material |
| CN115159993A (en) * | 2022-05-06 | 2022-10-11 | 云南纳诺电子新材料有限公司 | Preparation method of titanium dioxide for MLCC |
| CN116986626A (en) * | 2023-06-16 | 2023-11-03 | 核工业理化工程研究院 | Post-treatment method for germanium tetrafluoride to germanium dioxide reaction |
-
2008
- 2008-04-25 CN CNA2008100180526A patent/CN101279766A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101798110A (en) * | 2010-04-08 | 2010-08-11 | 复旦大学 | Preparation method of spherical nanometer titanium dioxide |
| CN102328952A (en) * | 2011-06-30 | 2012-01-25 | 北京大学 | Preparation method for spherical lithium titanate material |
| CN102328952B (en) * | 2011-06-30 | 2014-03-26 | 北京大学 | Preparation method for spherical lithium titanate material |
| CN105753046A (en) * | 2016-05-05 | 2016-07-13 | 陕西科技大学 | Preparation method of porous TiO2 bulk material |
| CN105948805A (en) * | 2016-05-05 | 2016-09-21 | 陕西科技大学 | Preparation method of titanium dioxide porous material |
| CN115159993A (en) * | 2022-05-06 | 2022-10-11 | 云南纳诺电子新材料有限公司 | Preparation method of titanium dioxide for MLCC |
| CN116986626A (en) * | 2023-06-16 | 2023-11-03 | 核工业理化工程研究院 | Post-treatment method for germanium tetrafluoride to germanium dioxide reaction |
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Open date: 20081008 |