CN103896335A - Preparation method of nano-porous titanium dioxide with high specific surface - Google Patents
Preparation method of nano-porous titanium dioxide with high specific surface Download PDFInfo
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- CN103896335A CN103896335A CN201310696697.6A CN201310696697A CN103896335A CN 103896335 A CN103896335 A CN 103896335A CN 201310696697 A CN201310696697 A CN 201310696697A CN 103896335 A CN103896335 A CN 103896335A
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Abstract
The invention provides a preparation method of nano-porous titanium dioxide with a high specific surface. The preparation method comprises the following steps of: a, providing metatitanic acid slurry, wherein the concentration of TiO2 in the metatitanic acid slurry is 80-100 g/L; b, slowly adding ammonium bicarbonate in the state of stirring the metatitanic acid slurry to adjust the pH value of the slurry to be 6.0-6.5, continuously stirring, and slowly adding ammonium hydroxide to adjust the pH value of the slurry to be 6.5-8.0; c, continuously stirring the slurry obtained in step (b) for 1-3 hours, then dehydrating till the solid content of the material is controlled to be more than 50%; d, calcining the material at 250-400 DEG C and dehydrating constitution water; and e, cooling and grinding the calcined material to obtain a nano-porous titanium dioxide finished product with the high specific surface.
Description
Technical field
The present invention relates to a kind of preparation method of high-ratio surface nano porous titanium dioxide.
Background technology
Titanium dioxide is a kind of widely used wide bandgap semiconductor materials, because of its good stability, harmless, and there is wet sensitive, pressure-sensitive, air-sensitive performance and be widely used in the fields such as sensor, electronic material, material of paint and other industrial chemicals, and show wide application prospect in the field such as solar cell, environmental improvement.
The specific surface area of the nano titanium dioxide powder that employing liquid phase high-temperature calcination and hydrolysis method prepare is at present less, has limited it in industrial application.
Summary of the invention
In sum, be necessary to provide a kind of preparation method of high-ratio surface nano porous titanium dioxide, adopt the method can prepare the titanium dioxide of high-specific surface area.
A preparation method for high-ratio surface nano porous titanium dioxide, it comprises the following steps: a. provides a metatitanic acid slurry, TiO in this metatitanic acid slurry
2concentration is 80g/L ~ 100g/L; B. under the state that stirs metatitanic acid slurry, slowly add bicarbonate of ammonia, the pH value of slurry is adjusted to 6.0 ~ 6.5, continue stirring and slowly add ammoniacal liquor that the pH value of slurry is adjusted to 6.5 ~ 8.0; C. the slurry obtaining by step (b) is carried out to processed to solid content is controlled at more than 50%; D. continue material to calcine and slough water of constitution at 250 ℃ ~ 400 ℃; E. by calcining after material cooling, pulverize after obtain high-ratio surface nano porous titanium dioxide finished product.
In the preparation method of high-ratio surface nano porous titanium dioxide provided by the invention, adopting skewness acid is raw material, adds bicarbonate of ammonia and ammoniacal liquor to regulate pH value to have high-specific surface area through the nano titanium oxide dewatering and calcining process prepares.Production technique is simple, and production cost is low, is conducive to suitability for industrialized production.
Accompanying drawing explanation
The titanium dioxide high-resolution-ration transmission electric-lens photo that Fig. 1 provides for the embodiment of the present invention 1.
The titanium dioxide high-resolution-ration transmission electric-lens photo that Fig. 2 provides for the embodiment of the present invention 1.
Embodiment
Below in conjunction with specific embodiment, technical scheme of the present invention is further explained in detail.
The preparation method of high-ratio surface nano porous titanium dioxide provided by the invention, with skewness acid be raw material, add bicarbonate of ammonia and ammoniacal liquor to regulate pH value through dewatering and calcining process is prepared nano titanium oxide.
Concrete preparation method, it comprises the following steps:
Step (1), provides a metatitanic acid slurry, TiO in this metatitanic acid slurry
2concentration is 80g/L ~ 100g/L;
Step (2) slowly adds bicarbonate of ammonia in by 15 minutes under the state that stirs metatitanic acid slurry, and the pH value of slurry is adjusted to 6.0 ~ 6.5;
Step (3), continues stirring and slowly added ammoniacal liquor that the pH value of slurry is adjusted to 6.5 ~ 8.0 in 15 minutes;
Step (4), the slurry that will obtain by step (3) continues to stir after 1 ~ 3 hour, and puts it at 90 ℃ ~ 110 ℃, dries 1 hour ~ 3 hours in thermostatic drying chamber, sloughs planar water; Processed is to being controlled at more than 50% the solid content in material, and preferably 50% ~ 65%;
Step (5), pours the material obtaining by step (4) in clean porcelain dish into, then enters in retort furnace and calcines, and calcining temperature is 250 ℃ ~ 400 ℃, and calcination time is 4 hours ~ 5 hours, sloughs water of constitution;
Step (6), by calcining after material cooling, pulverize after obtain high-ratio surface nano porous titanium dioxide finished product.
The metatitanic acid slurry providing in described step is hydrolyzed into titanyl sulfate by titanium sulfate and is further hydrolyzed and obtains.Reaction equation is as follows:
Ti(SO
4)
2?+?H
2O?=?TiOSO
4?+?H
2SO
4
TiOSO
4?+?2H
2O?=?H
2TiO
3?+?H
2SO
4
The titanium dioxide main ingredient and the component concentration that obtain afterwards by described step (6) are: 85% ~ 90% titanium dioxide, 1.0% ~ 1.5% sulfate radical.The specific surface area of titanium dioxide can reach 250 m
2more than/g.
The mechanism of technical solution of the present invention is: by the titanium dioxide process of the synthetic high-ratio surface of certain density metatitanic acid control, the principal element that affects specific surface size has additive, sintering temperature, sintering time, pH etc.The principles of chemistry of control ratio surface-area based on: although bicarbonate of ammonia is weak acid and weak base salt, bicarbonate radical is than the violent (K of ammonium root hydrolysis
h1> K
h2), therefore it is weakly alkaline.
HCO
3 -+?H
2O?=?H
2CO
3?+?OH
-?K
h1?=?K
W/K
a1(H
2CO
3)?=?10
-14?/4.2×10
-7
NH
4 +?+?H
2O?=?NH
3H
2O?+?H
+?K
h2?=?K
W/K
b(NH
3H
2O)?=10
-14?/1.8×10
-5
Bicarbonate of ammonia is below 10 ℃ time, and stable chemical nature, does not decompose substantially; 10-20 ℃ time, decompose not remarkable; When more than 30 ℃, decompose in a large number, produce ammonia, carbonic acid gas and water.Heating up to dewater at metatitanic acid forms in the process of particle, utilizes ammonium bicarbonate soln to decompose and produces a large amount of gas, forms poriferous titanium dioxide.Ammoniacal liquor can with metatitanic acid slurry in a small amount of sulfate radical effect generate monoammonium sulfate, its effect is to guarantee that the pH of the product after slurry high-temperature calcination is being less than 7.
Embodiment 1
In the present embodiment, main raw material is metatitanic acid.
To there is certain density metatitanic acid slurry pure water dilution and obtain TiO
2concentration is the metatitanic acid slurry of 90g/L, gets and puts in right amount beaker, slowly adds bicarbonate of ammonia that material pH value is adjusted to 6.0 ~ 6.5 under whipped state, continues to stir slowly to add ammoniacal liquor that material pH value is adjusted to 6.5 ~ 7.0; Continue to stir after 2 hours and carry out processed, solid content is controlled at more than 50%, and the material that above-mentioned reaction is obtained is poured in clean porcelain dish, and put it in the thermostatic drying chamber of 105 ℃ and dry 2 hours, then enter in retort furnace and calcine, calcining temperature is 300 ℃, and calcination time is 4h.Calcination product is pulverized by pulverizer after cooling, and smashing fineness 325 order screen overflows are less than 0.03%, obtain the nano titanium oxide finished product of high-specific surface area, refer to the transmission electron microscope photo of Fig. 1 and 2.
Embodiment 2
In the present embodiment, main raw material is metatitanic acid.
To there is certain density metatitanic acid slurry pure water dilution and obtain TiO
2concentration is the metatitanic acid slurry of 96g/L, gets and puts in right amount beaker, slowly adds bicarbonate of ammonia that material pH value is adjusted to 6.0 ~ 6.5 under whipped state, continues to stir slowly to add ammoniacal liquor that material pH value is adjusted to 7.0; Continue to stir after 1 hour and carry out processed, solid content is controlled at 50% ~ 55%, and the material that above-mentioned reaction is obtained is poured in clean porcelain dish, and put it in the thermostatic drying chamber of 100 ℃ and dry 3 hours, then enter in stove and calcine, calcining temperature is 350 ℃, and calcination time is 4h.Calcination product is pulverized by pulverizer after cooling, and smashing fineness 325 order screen overflows are less than 0.03%, obtain the nano titanium oxide finished product for the high-specific surface area of catalysis.
Embodiment 3
In the present embodiment, main raw material is metatitanic acid.
To there is certain density metatitanic acid slurry pure water dilution and obtain TiO
2concentration is the metatitanic acid slurry of 94g/L, gets and puts in right amount beaker, slowly adds bicarbonate of ammonia that material pH value is adjusted to 6.0 ~ 6.5 under whipped state, continues to stir slowly to add ammoniacal liquor that material pH value is adjusted to 7.2; Continue to stir after 2 hours and carry out processed, solid content is controlled at 55% ~ 60%, and the material that above-mentioned reaction is obtained is poured in clean porcelain dish, and put it in the thermostatic drying chamber of 105 ℃ and dry 3 hours, then enter in retort furnace and calcine, calcining temperature is 300 ℃, and calcination time is 5h.Calcination product is pulverized by pulverizer after cooling, and smashing fineness 325 order screen overflows are less than 0.03%, obtain the nano titanium oxide finished product for the high-specific surface area of catalysis.
Embodiment 4
In the present embodiment, main raw material is metatitanic acid.
To there is certain density metatitanic acid slurry pure water dilution and obtain TiO
2concentration is the metatitanic acid slurry of 98g/L, gets and puts in right amount beaker, slowly adds bicarbonate of ammonia that material pH value is adjusted to 6.0 ~ 6.5 under whipped state, continues to stir slowly to add ammoniacal liquor that material pH value is adjusted to 7.0; Continue to stir after 3 hours and carry out processed, solid content is controlled at 60% ~ 62%, and the material that above-mentioned reaction is obtained is poured in clean porcelain dish, and put it in the thermostatic drying chamber of 105 ℃ and dry 3 hours, then enter in retort furnace and calcine, calcining temperature is 320 ℃, and calcination time is 4h.Calcination product is pulverized by pulverizer after cooling, and smashing fineness 325 order screen overflows are less than 0.03%, obtain the nano titanium oxide finished product for the high-specific surface area of catalysis.
Embodiment 5
In the present embodiment, main raw material is metatitanic acid.
To there is certain density metatitanic acid slurry pure water dilution and obtain TiO
2concentration is the metatitanic acid slurry of 100g/L, gets and puts in right amount beaker, slowly adds bicarbonate of ammonia that material pH value is adjusted to 6.0 ~ 6.5 under whipped state, continues to stir slowly to add ammoniacal liquor that material pH value is adjusted to 6.8; Continue to stir after 2.5 hours and carry out processed, solid content is controlled at 62% ~ 65%, the material that above-mentioned reaction is obtained is poured in clean porcelain dish, and put it in the thermostatic drying chamber of 90 ℃ and dry 3 hours, then enter in retort furnace and calcine, calcining temperature is 300 ℃, and calcination time is 5h.Calcination product is pulverized by pulverizer after cooling, and smashing fineness 325 order screen overflows are less than 0.03%, obtain the nano titanium oxide finished product for the high-specific surface area of catalysis.
Embodiment 6
In the present embodiment, main raw material is metatitanic acid.
To there is certain density metatitanic acid slurry pure water dilution and obtain TiO
2concentration is the metatitanic acid slurry of 92g/L, gets and puts in right amount beaker, slowly adds bicarbonate of ammonia that material pH value is adjusted to 6.0 ~ 6.5 under whipped state, continues to stir slowly to add ammoniacal liquor that material pH value is adjusted to 6.8; Continue to stir after 3 hours and carry out processed, solid content is controlled at 50% ~ 55%, and the material that above-mentioned reaction is obtained is poured in clean porcelain dish, and put it in the thermostatic drying chamber of 105 ℃ and dry 3 hours, then enter in retort furnace and calcine, calcining temperature is 280 ℃, and calcination time is 5h.Calcination product is pulverized by pulverizer after cooling, and smashing fineness 325 order screen overflows are less than 0.03%, obtain the nano titanium oxide finished product for the high-specific surface area of catalysis.
Embodiment 7
In the present embodiment, main raw material is metatitanic acid.
To there is certain density metatitanic acid slurry pure water dilution and obtain TiO
2concentration is the metatitanic acid slurry of 90g/L, gets and puts in right amount beaker, slowly adds bicarbonate of ammonia that material pH value is adjusted to 6.0 ~ 6.5 under whipped state, continues to stir slowly to add ammoniacal liquor that material pH value is adjusted to 7.0; Continue to stir after 2.5 hours and carry out processed, solid content is controlled at 50% ~ 60%, the material that above-mentioned reaction is obtained is poured in clean porcelain dish, and put it in the thermostatic drying chamber of 100 ℃ and dry 2.5 hours, then enter in retort furnace and calcine, calcining temperature is 400 ℃, and calcination time is 4h.Calcination product is pulverized by pulverizer after cooling, and smashing fineness 325 order screen overflows are less than 0.03%, obtain the nano titanium oxide finished product for the high-specific surface area of catalysis.
Comparative example 1
In the present embodiment, main raw material is metatitanic acid.
To there is certain density metatitanic acid slurry pure water dilution and obtain TiO
2concentration is the metatitanic acid slurry of 89g/L, gets and puts in right amount beaker, slowly adds bicarbonate of ammonia that material pH value is adjusted to 6.0 ~ 7.0 under whipped state, continues to stir slowly to add ammoniacal liquor that material pH value is adjusted to 8.0; Continue to stir after 1 hour and carry out processed, solid content is controlled at more than 50%, and the material that above-mentioned reaction is obtained is poured in clean porcelain dish, and put it in the thermostatic drying chamber of 90 ℃ and dry 3 hours, then enter in retort furnace and calcine, calcining temperature is 500 ℃, and calcination time is 2h.Calcination product is pulverized by pulverizer after cooling, obtains the nano titanium oxide finished product for the high-specific surface area of catalysis.
Comparative example 2
In the present embodiment, main raw material is metatitanic acid.
To there is certain density metatitanic acid slurry pure water dilution and obtain TiO
2concentration is the metatitanic acid slurry of 88g/L, gets and puts in right amount beaker, slowly adds bicarbonate of ammonia that material pH value is adjusted to 6.0 ~ 6.5 under whipped state, continues to stir slowly to add ammoniacal liquor that material pH value is adjusted to 8.5; Continue to stir after 1.5 hours and carry out processed, solid content is controlled at 50% ~ 60%, and the material that above-mentioned reaction is obtained is poured in clean porcelain dish, and put it in the thermostatic drying chamber of 100 ℃ and dry 1.5 hours, then enter in stove and calcine, calcining temperature is 500 ℃, and calcination time is 2h.Calcination product is pulverized by pulverizer after cooling, obtains the nano titanium oxide finished product for the high-specific surface area of catalysis.
Comparative example 3
In the present embodiment, main raw material is metatitanic acid.
To there is certain density metatitanic acid slurry pure water dilution and obtain TiO
2concentration is the metatitanic acid slurry of 86g/L, gets and puts in right amount beaker, slowly adds bicarbonate of ammonia that material pH value is adjusted to 6.0 ~ 6.5 under whipped state, continues to stir slowly to add ammoniacal liquor that material pH value is adjusted to 8.3; Continue to stir after 3 hours and carry out processed, solid content is controlled at 60% ~ 65%, the material that above-mentioned reaction is obtained is poured in clean porcelain dish, and put it in the thermostatic drying chamber of 105 ℃ and dry 1 hour, then enter in retort furnace and first at 400 ℃, calcine 2 hours, at 500 ℃, calcine 1 hour afterwards.Calcination product is pulverized by pulverizer after cooling, obtains the nano titanium oxide finished product for the high-specific surface area of catalysis.
The titanium dioxide results of performance analysis that the present invention prepares is as shown in table 1 below.
Listed parameter in table 1 is the parameter of the titanium dioxide for preparing under the preparation condition by each embodiment and comparative example.For example, TiO in table
2(%) refer to actual TiO in the titanium dioxide preparing
2quality percentage composition, SO
4 2-(%) refer to the quality percentage composition of sulfate radical residual in the titanium dioxide preparing, so-called pH value refers to the pH value of the titanium dioxide finished product preparing.
More low specific surface area is just higher for calcining temperature as can be seen from Table 1, and for example in comparative example 1～3, calcining temperature has all reached 500 ℃, and therefore, its specific surface area is lower only has 89m
2/ g ~ 94m
2/ g, and in each embodiment of the present invention, calcining temperature is all controlled at 250 ℃ ~ 400 ℃, therefore, the specific surface area of the titania nanoparticles preparing can reach 250 m
2more than/g.Also, calcination time is longer, and the aperture of particle can be more and more less, causes specific surface area to diminish.Conventionally specific surface area is larger, and bulk density is less.In addition, utilize as can be seen from Table 1 the granular size of the titanium dioxide granule that the method for effecting a permanent cure of the present invention prepares more all between 20nm ~ 60nm.
The preparation method's of high-ratio surface nano porous titanium dioxide of the present invention principle is in first coming with bicarbonate of ammonia and metatitanic acid, and carry out washing precipitation metatitanic acid with bicarbonate of ammonia, the sulfate radical being adsorbed in titanium dioxide space can be washed away, reduce the content of sulphur.It is more that bicarbonate of ammonia decomposes the gas producing than ammoniacal liquor, thereby can guarantee to produce a large amount of pores during calcining, and then increase the specific surface area of titanium dioxide.On the other hand, then use the final pH value of ammoniacal liquor regulator solution, ammoniacal liquor can with metatitanic acid slurries in a small amount of sulfate radical effect generate monoammonium sulfate, its effect is to guarantee that the pH of product is less than 7 after slurry high-temperature calcination.If singly add bicarbonate of ammonia, after calcining, the finished product pH value can be greater than 7.
In addition, those skilled in the art also can do other and change in spirit of the present invention, and these variations of doing according to spirit of the present invention certainly, all should be included in the present invention's scope required for protection.
Claims (5)
1. a preparation method for high-ratio surface nano porous titanium dioxide, comprises the following steps:
A. provide a metatitanic acid slurry, TiO in this metatitanic acid slurry
2concentration is 80g/L ~ 100g/L;
B. under the state that stirs metatitanic acid slurry, slowly add bicarbonate of ammonia, the pH value of slurry is adjusted to 6.0 ~ 6.5, form the first slurry;
C. under the state that stirs the first slurry, slowly add ammoniacal liquor, the pH value of slurry is adjusted to 6.5 ~ 8.0, form one second slurry;
D. the second slurry being carried out to processed is controlled at more than 50% solid content;
E. the second slurry after processed is calcined and sloughed water of constitution at 250 ℃ ~ 400 ℃;
F. by cooling material after calcining, obtain high-ratio surface nano porous titanium dioxide finished product after pulverizing.
2. the preparation method of high-ratio surface nano porous titanium dioxide as claimed in claim 1, is characterized in that, the specific surface area of the titanium dioxide preparing can reach 250 m
2more than/g.
3. the preparation method of high-ratio surface nano porous titanium dioxide as claimed in claim 1, is characterized in that, in described steps d, described the second slurry, at 90 ℃ ~ 110 ℃, is dried 1 hour ~ 3 hours in thermostatic drying chamber, sloughs planar water.
4. the preparation method of high-ratio surface nano porous titanium dioxide as claimed in claim 1, is characterized in that, in described step e, calcination time is 4 hours ~ 5 hours.
5. the preparation method of high-ratio surface nano porous titanium dioxide as claimed in claim 1, is characterized in that, in described steps d, the solid content in material is controlled at 55% ~ 65%.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104475071A (en) * | 2014-11-21 | 2015-04-01 | 广西美之峰科技有限责任公司 | Preparation method of nano titanium dioxide serving as flue gas denitrification catalyst |
| CN105712398A (en) * | 2016-05-10 | 2016-06-29 | 湖北天瓷电子材料有限公司 | Method for preparing adjustable-particle-size adjustable-specific-area titanium dioxide by direct heating |
| CN105776329A (en) * | 2016-05-10 | 2016-07-20 | 湖北天瓷电子材料有限公司 | Method for preparing flocculent titanium dioxide with large specific surface area |
| CN108516584A (en) * | 2018-07-09 | 2018-09-11 | 江苏中研创星材料科技有限公司 | A kind of preparation method of high-purity super large specific surface poriferous titanium dioxide |
| CN110075903A (en) * | 2019-05-30 | 2019-08-02 | 河北麦森钛白粉有限公司 | A kind of preparation method of C, N coblended nano TiO 2 |
| CN110902716A (en) * | 2019-12-26 | 2020-03-24 | 南京钛白化工有限责任公司 | Preparation method of high specific surface area metatitanic acid |
| CN111362302A (en) * | 2020-03-18 | 2020-07-03 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing nano titanium dioxide |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104475071A (en) * | 2014-11-21 | 2015-04-01 | 广西美之峰科技有限责任公司 | Preparation method of nano titanium dioxide serving as flue gas denitrification catalyst |
| CN105712398A (en) * | 2016-05-10 | 2016-06-29 | 湖北天瓷电子材料有限公司 | Method for preparing adjustable-particle-size adjustable-specific-area titanium dioxide by direct heating |
| CN105776329A (en) * | 2016-05-10 | 2016-07-20 | 湖北天瓷电子材料有限公司 | Method for preparing flocculent titanium dioxide with large specific surface area |
| CN108516584A (en) * | 2018-07-09 | 2018-09-11 | 江苏中研创星材料科技有限公司 | A kind of preparation method of high-purity super large specific surface poriferous titanium dioxide |
| CN108516584B (en) * | 2018-07-09 | 2020-05-08 | 江苏中研创星材料科技有限公司 | Preparation method of high-purity super-large specific surface porous titanium dioxide |
| CN110075903A (en) * | 2019-05-30 | 2019-08-02 | 河北麦森钛白粉有限公司 | A kind of preparation method of C, N coblended nano TiO 2 |
| CN110075903B (en) * | 2019-05-30 | 2022-03-22 | 河北麦森钛白粉有限公司 | Preparation method of C, N co-doped nano titanium dioxide |
| CN110902716A (en) * | 2019-12-26 | 2020-03-24 | 南京钛白化工有限责任公司 | Preparation method of high specific surface area metatitanic acid |
| CN111362302A (en) * | 2020-03-18 | 2020-07-03 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing nano titanium dioxide |
| CN111362302B (en) * | 2020-03-18 | 2022-07-26 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing nano titanium dioxide |
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|---|---|
| CN103896335B (en) | 2016-03-30 |
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