CN110342573B - Preparation method of cubic titanium oxide - Google Patents
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- CN110342573B CN110342573B CN201910646250.5A CN201910646250A CN110342573B CN 110342573 B CN110342573 B CN 110342573B CN 201910646250 A CN201910646250 A CN 201910646250A CN 110342573 B CN110342573 B CN 110342573B
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Abstract
The invention discloses a preparation method of cubic titanium oxide, which comprises the following steps: (1) dissolving trisodium citrate dihydrate in ethylene glycol to obtain a solution A; (2) adding a titanium trichloride hydrochloric acid solution into ethylene glycol, and mixing to obtain a solution B; (3) adding anhydrous sodium acetate and deionized water into the solution A obtained in the step (1), and dissolving to obtain a solution C; (4) adding the solution B prepared in the step (2) into the solution C prepared in the step (3), and mixing under the stirring action to obtain a solution D; (5) and (3) placing the solution D in a closed high-pressure reaction kettle, discharging air of the high-pressure reaction kettle under normal pressure by using nitrogen, and heating for reaction to obtain cubic titanium oxide. The cubic titanium oxide prepared by the invention is a composite phase of anatase and brookite, has controllable particle size and good dispersibility, is widely applied in the fields of chemical industry, environment, electronics, semiconductors and the like, and is particularly suitable for the field of air purification materials.
Description
Technical Field
The invention relates to the field of titanium oxide preparation, in particular to a preparation method of cubic titanium oxide.
Background
Titanium dioxide (TiO)2) Is one of the most important metal oxides in industrial applications, as it can be used in a range of different fields, from paper making to pharmaceuticals, cosmetics, photocatalysts, photovoltaic cells, sensors, inks, coatings, coverings (coverings) and plastics, even including the photocatalysis of organic pollutants. In particular, certain types of TiO2Particularly suitable for use in photovoltaic cells, especially dye-sensitized solar cells (DSSCs), and in photoelectrolysis cells and tandem cells for the conversion between solar energy and hydrogen products.
TiO2Have a variety of crystalline shapes. Most common TiO2The crystalline phases anatase, rutile and brookite exhibit different chemical/physical properties such as stability field, refractive index, and chemical reactivity and behavior to electromagnetic radiation exposure. TiO, as reported by X.Chen and S.S.Mao in J.Nanosci.Nanotechnol, 6(4), 906-2The use and properties of (a) depend mainly on its crystalline phase, morphology and particle size. The phase composition, crystal shape and particle size have a large influence on the chemical, physical, mechanical, electronic, magnetic and optical properties of the final product.
Anatase phase TiO2Has the advantages of excellent optical and electrical properties, good chemical stability, low cost, safety, no toxicity, no secondary pollution and the like, is favored, is not only used for degrading, deodorizing, sterilizing and sterilizing organic pollutants in gas phase and aqueous solution, but also is applied to the field of photoelectric conversion.
At present, anatase phase TiO2The synthesis method of (A) is various, and TiO is prepared2The main method comprises the following steps:
a) hydrothermal synthesis method; b) a solvothermal synthesis method; c) sol-gel synthesis. Although the research on the preparation of titanium dioxide has made great progress, the preparation method has disadvantages. At present, the synthesized titanium dioxide is mainly synthesized by a solvothermal method or a sol-gel synthesis method. The particles prepared by the method have uneven particle size, the titanium dioxide particles with even particle size are difficult to prepare, and the prepared titanium dioxide particles are easy to agglomerate and have poor dispersibility.
Disclosure of Invention
The invention aims to provide a preparation method of cubic titanium oxide, and the titanium oxide prepared by the method is a composite phase of anatase and brookite, and has controllable particle size and good dispersibility.
A method for preparing cubic titanium dioxide comprises the following steps:
(1) dissolving trisodium citrate dihydrate in ethylene glycol to obtain a solution A;
(2) adding a titanium trichloride hydrochloric acid solution into ethylene glycol, and mixing to obtain a solution B;
(3) adding anhydrous sodium acetate and deionized water into the solution A obtained in the step (1), and dissolving to obtain a solution C;
(4) adding the solution B prepared in the step (2) into the solution C prepared in the step (3), and mixing under the stirring action to obtain a solution D;
(5) and heating the solution D, and reacting to obtain cubic titanium oxide.
The preparation principle of the invention is as follows: the titanium trichloride hydrochloric acid solution is firstly hydrolyzed into titanium suboxide containing trivalent titanium in a closed high-temperature environment, then the titanium suboxide reacts with sodium acetate and water to generate anatase and brookite composite titanium dioxide, and the crystal form of the titanium dioxide can be adjusted by controlling the proportion of the titanium trichloride hydrochloric acid, anhydrous sodium acetate and deionized water; according to the invention, the ethylene glycol solution B of the titanium trichloride hydrochloric acid solution is mixed with the solution C to obtain a purple black clear solution, instead of directly adding the titanium trichloride hydrochloric acid solution into the solution C, so that the titanium trichloride hydrochloric acid solution can uniformly react with sodium acetate and water to obtain titanium dioxide particles with good appearance and uniform particle size.
The trisodium citrate dihydrate is used as a dispersion stabilizer to improve the dispersibility of reaction products, and the concentration of the trisodium citrate dihydrate in the solution A is 5 g/L-40 g/L. In the step (1), the trisodium citrate dihydrate is heated at the temperature of 50-120 ℃ and dissolved in ethylene glycol.
In the step (2), the titanium trichloride hydrochloric acid solution is a titanium trichloride hydrochloric acid solution with a mass fraction of 15%. The concentration of the titanium trichloride hydrochloric acid solution in the solution B is 25 g/L-125 g/L.
In the step (3), the mass ratio of the added anhydrous sodium acetate to the deionized water is 1: 0.1 to 3.
In the step (4), in the solution D, the mass ratio of the titanium trichloride hydrochloric acid solution to the anhydrous sodium acetate is 1: 0.3 to 10.
Preferably, in the step (4), the mass ratio of the titanium trichloride hydrochloric acid solution to the anhydrous sodium acetate in the solution D is 1: 1 to 5.
In the invention, the titanium trichloride hydrochloric acid solution mainly influences the nucleation and crystal form of the particles, and titanium dioxide with different crystal forms and particle sizes can be obtained by adding anhydrous sodium acetate and the titanium trichloride hydrochloric acid solution with different mass ratios. As the proportion of the titanium trichloride hydrochloric acid solution is increased, the particle size basically tends to be gradually reduced, and the content of the brookite is increased.
In the step (5), the reaction temperature is 140-220 ℃ and the reaction time is 2-30 h. In the invention, the reaction rate and the nuclear growth are influenced by the temperature, and the reaction is sufficient under the condition, so that particles with good appearance and uniform particle size can be obtained.
Preferably, in the step (5), the reaction temperature is 180 ℃ and the reaction time is 10 h.
In the step (5), the cubic titanium oxide is titanium dioxide compounded by anatase and brookite, and the diameter of the cubic titanium oxide is 1-4 μm.
Preferably, in the step (3), the mass ratio of the anhydrous sodium acetate to the deionized water is 1: 0.1 to 3; in the step (4), the mass ratio of the titanium trichloride hydrochloric acid solution to the anhydrous sodium acetate in the solution D is 1: 1-2; in the step (5), the reaction temperature is 180 ℃ and the reaction time is 10 hours; and preparing the anatase and brookite compounded cubic titanium oxide, wherein the diameter of the cubic titanium oxide is 1-4 mu m.
In the present invention, cubic titanium oxide is also called cubic titanium dioxide, titanium dioxide or titanium oxide.
The preparation method disclosed by the invention is simple to operate, only simple dissolving, mixing and heating operations are needed, the whole operation process is directly carried out in the air, and the operation is simple; and the anatase and brookite compounded titanium dioxide is obtained, has uniform particle size and good morphology, can be applied to the fields of chemical industry, environment, electronics, semiconductors and the like, and is particularly suitable for the field of air purification materials.
Compared with the prior art, the method has the advantages of short reaction time, low cost and simple process, and can prepare anatase and brookite compounded cubic titanium oxide particles with small particle size, good dispersity, uniform particle size and controllable size. Due to good uniform and controllable appearance and size, the nano-particle has wide application in the fields of chemical industry, environment, electronics, semiconductors and the like, and is small in particle size, and particularly suitable for the field of air purification materials.
Drawings
FIG. 1 is a Scanning Electron Microscope (SEM) photograph of cubic titanium oxide prepared in example 1;
FIG. 2 is a polycrystalline X-ray diffractometer plot of cubic titanium oxide prepared in example 1;
fig. 3 is a Scanning Electron Microscope (SEM) photograph of the cubic titanium oxide prepared in example 2.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be further described in detail with reference to the accompanying drawings and examples. It should be understood that the detailed description and specific examples, while indicating the scope of the invention, are intended for purposes of illustration only and are not intended to limit the scope of the invention.
Example 1
6g trisodium citrate dihydrate was dissolved in 400ml ethylene glycol at ambient temperature and pressure and stirred to give a clear solution, denoted as solution A. Simultaneously, 16g of titanium trichloride hydrochloric acid solution was mixed with 150ml of ethylene glycol to obtain a purple transparent solution, which was marked as solution B. Mixing the components in a mass ratio of 1: 0.7 g of anhydrous sodium acetate (30g) and deionized water (21g) were added to solution A and stirred until completely dissolved to give solution C. And adding the solution B into the solution C, and stirring to fully mix to obtain a purple black solution D. The purple black solution D was placed in a high-temperature high-pressure reaction vessel having a volume of 1L, and the air in the reaction vessel was purged with nitrogen gas at a temperature of 180 ℃ and reacted at that temperature for 20 hours. And separating the obtained mixed solution after the reaction is finished. And washing the obtained grey white solid with deionized water for several times to obtain the product cubic titanium oxide particles.
The cubic titanium oxide particles obtained were observed by a scanning electron microscope, and as a result, as can be seen from FIG. 1, the diameter of the product was 4 μm. The cubic titanium oxide was measured by a polycrystalline X-ray diffractometer, and the result is shown in fig. 2 (the abscissa is an angle 2 θ, and the ordinate is intensity), and the crystal form of the titanium oxide is a mixture of anatase and brookite.
Example 2
6g trisodium citrate dihydrate was dissolved in 400ml ethylene glycol at ambient temperature and pressure and stirred to give a clear solution, denoted as solution A. Simultaneously, 30g of titanium trichloride hydrochloric acid solution was mixed with 150ml of ethylene glycol to obtain a purple transparent solution, which was marked as solution B. Mixing the components in a mass ratio of 1: 0.5 g of anhydrous sodium acetate (30g) and deionized water (15g) were added to solution A and stirred until completely dissolved to give solution C. And adding the solution B into the solution C, and stirring to fully mix to obtain a purple black solution D. The purple black solution D was placed in a high-temperature high-pressure reaction vessel having a volume of 1L, and the air in the reaction vessel was purged with nitrogen gas at a temperature of 180 ℃ and reacted at that temperature for 20 hours. And separating the obtained mixed solution after the reaction is finished. And washing the obtained grey white solid with deionized water for several times to obtain the product cubic titanium oxide particles.
When the cubic titanium oxide particles were observed by a scanning electron microscope, as shown in FIG. 3, the diameter of the product was 3 μm as seen in FIG. 3.
Example 3
6g trisodium citrate dihydrate was dissolved in 400ml ethylene glycol at ambient temperature and pressure and stirred to give a clear solution, denoted as solution A. Simultaneously, 30g of titanium trichloride hydrochloric acid solution was mixed with 150ml of ethylene glycol to obtain a purple transparent solution, which was marked as solution B. Mixing the components in a mass ratio of 1: 0.3g of anhydrous sodium acetate (30g) and deionized water (9g) were added to solution A and stirred until completely dissolved to give solution C. And adding the solution B into the solution C, and stirring to fully mix to obtain a purple black solution D. The purple black solution D was placed in a high-temperature high-pressure reaction vessel having a volume of 1L, and the air in the reaction vessel was purged with nitrogen gas at a temperature of 180 ℃ and reacted at that temperature for 20 hours. And separating the obtained mixed solution after the reaction is finished. And washing the obtained grey white solid with deionized water for several times to obtain the product cubic titanium oxide particles.
The cubic titanium oxide particles were observed by a scanning electron microscope, and the diameter of the product was 2 μm.
Example 4
6g trisodium citrate dihydrate was dissolved in 400ml ethylene glycol at ambient temperature and pressure and stirred to give a clear solution, denoted as solution A. Simultaneously, 6g of titanium trichloride hydrochloric acid solution was mixed with 150ml of ethylene glycol to obtain a purple transparent solution, which was denoted as solution B. Mixing the components in a mass ratio of 1: 0.1 g of anhydrous sodium acetate (3g) and deionized water (0.3g) were added to solution A and stirred until completely dissolved to give solution C. And adding the solution B into the solution C, and stirring to fully mix to obtain a purple black solution D. The purple black solution D was placed in a high-temperature high-pressure reaction vessel having a volume of 1L, and the air in the reaction vessel was purged with nitrogen gas at a temperature of 180 ℃ and reacted at that temperature for 20 hours. And separating the obtained mixed solution after the reaction is finished. And washing the obtained grey white solid with deionized water for several times to obtain the product cubic titanium oxide particles.
The cubic titanium oxide particles were observed by a scanning electron microscope, and the diameter of the product was 3 μm.
Example 5
6g trisodium citrate dihydrate was dissolved in 400ml ethylene glycol at ambient temperature and pressure and stirred to give a clear solution, denoted as solution A. Simultaneously, 15g of titanium trichloride hydrochloric acid solution was mixed with 150ml of ethylene glycol to obtain a purple transparent solution, which was denoted as solution B. Mixing the components in a mass ratio of 1: 3 (30g) of anhydrous sodium acetate and deionized water (90g) were added to solution A and stirred until completely dissolved to give solution C. And adding the solution B into the solution C, and stirring to fully mix to obtain a purple black solution D. The purple black solution D was placed in a high-temperature high-pressure reaction vessel having a volume of 1L, and the air in the reaction vessel was purged with nitrogen gas at a temperature of 180 ℃ and reacted at that temperature for 20 hours. And separating the obtained mixed solution after the reaction is finished. And washing the obtained grey white solid with deionized water for several times to obtain the product cubic titanium oxide particles.
The cubic titanium oxide particles were observed by a scanning electron microscope to obtain a product having a diameter of 1.5. mu.m.
Example 6
6g trisodium citrate dihydrate was dissolved in 400ml ethylene glycol at ambient temperature and pressure and stirred to give a clear solution, denoted as solution A. Simultaneously, 16g of titanium trichloride hydrochloric acid solution was mixed with 150ml of ethylene glycol to obtain a purple transparent solution, which was marked as solution B. Mixing the components in a mass ratio of 1: 0.7 g of anhydrous sodium acetate (30g) and deionized water (21g) were added to solution A and stirred until completely dissolved to give solution C. And adding the solution B into the solution C, and stirring to fully mix to obtain a purple black solution D. The purple black solution D was placed in a high-temperature high-pressure reaction vessel having a volume of 1L, and the air in the reaction vessel was purged with nitrogen gas at a set temperature of 200 ℃ and reacted for 5 hours at that temperature. And separating the obtained mixed solution after the reaction is finished. And washing the obtained grey white solid with deionized water for several times to obtain the product cubic titanium oxide particles.
The cubic titanium oxide particles were observed by a scanning electron microscope, and the diameter of the product was 1 μm.
Comparative example 1
6g trisodium citrate dihydrate was dissolved in 400ml ethylene glycol at ambient temperature and pressure and stirred to give a clear solution, denoted as solution A. 16g of titanium trichloride hydrochloric acid solution was taken and recorded as solution B. Mixing the components in a mass ratio of 1: 0.7 g of anhydrous sodium acetate (30g) and deionized water (21g) were added to solution A and stirred until completely dissolved to give solution C. And adding the solution B into the solution C, and stirring to fully mix to obtain a purple black solution D. The purple black solution D was placed in a high-temperature high-pressure reaction vessel having a volume of 1L, and the air in the reaction vessel was purged with nitrogen gas at a set temperature of 200 ℃ and reacted for 5 hours at that temperature. And separating the obtained mixed solution after the reaction is finished. And washing the obtained grey white solid with deionized water for several times to obtain the product cubic titanium oxide particles.
The cubic titanium oxide particles obtained in the comparative example were not regular cubes and were not uneven in particle diameter, as compared with examples 1 to 6.
The above-mentioned embodiments are intended to illustrate the technical solutions and advantages of the present invention, and it should be understood that the above-mentioned embodiments are only the most preferred embodiments of the present invention, and are not intended to limit the present invention, and any modifications, additions, equivalents, etc. made within the scope of the principles of the present invention should be included in the scope of the present invention.
Claims (5)
1. A method for preparing cubic titanium dioxide, which is characterized by comprising the following steps:
(1) dissolving trisodium citrate dihydrate in ethylene glycol to obtain a solution A;
(2) adding a titanium trichloride hydrochloric acid solution into ethylene glycol, and mixing to obtain a solution B;
(3) adding anhydrous sodium acetate and deionized water into the solution A obtained in the step (1), and dissolving to obtain a solution C;
(4) adding the solution B prepared in the step (2) into the solution C prepared in the step (3), and mixing under the stirring action to obtain a solution D;
(5) heating the solution D, and reacting to obtain cubic titanium oxide;
in the step (4), the mass ratio of the titanium trichloride hydrochloric acid solution to the anhydrous sodium acetate in the solution D is 1: 0.3 to 10;
in the step (5), the reaction temperature is 140-220 ℃ and the reaction time is 2-30 h;
in the step (5), the cubic titanium oxide is titanium dioxide compounded by anatase and brookite, and the diameter of the cubic titanium oxide is 1-4 μm.
2. The method for preparing cubic titanium dioxide as claimed in claim 1, wherein in the step (1), the concentration of trisodium citrate dihydrate in the solution A is 5g/L to 40 g/L.
3. The method for producing cubic titanium dioxide as claimed in claim 1, wherein in the step (3), anhydrous sodium acetate and deionized water are added in a mass ratio of 1: 0.1 to 3.
4. The method for producing cubic titanium dioxide as claimed in claim 1, wherein in the step (4), the mass ratio of the titanium trichloride hydrochloric acid solution to the anhydrous sodium acetate in the solution D is 1: 1 to 5.
5. The method for producing cubic titanium dioxide as claimed in claim 1, wherein in the step (3), anhydrous sodium acetate and deionized water are added in a mass ratio of 1: 0.1 to 3; in the step (4), the mass ratio of the titanium trichloride hydrochloric acid solution to the anhydrous sodium acetate in the solution D is 1: 1-2; in the step (5), the reaction temperature is 180 ℃ and the reaction time is 10 hours.
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