CN111994950A - Preparation method of anatase type nano titanium dioxide microspheres - Google Patents

Preparation method of anatase type nano titanium dioxide microspheres Download PDF

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CN111994950A
CN111994950A CN202010963493.4A CN202010963493A CN111994950A CN 111994950 A CN111994950 A CN 111994950A CN 202010963493 A CN202010963493 A CN 202010963493A CN 111994950 A CN111994950 A CN 111994950A
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titanium dioxide
anatase type
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郝世雄
余晓鹏
梁萍
尚建平
王议
邓超仪
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Sichuan University of Science and Engineering
Wuliangye Yibin Co Ltd
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Wuliangye Yibin Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
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    • C01G23/00—Compounds of titanium
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    • C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
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    • B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
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Abstract

The invention discloses a preparation method of anatase type nano titanium dioxide microspheres, which comprises the following steps: dissolving isopropanol in diethylenetriamine, and uniformly mixing to obtain a solution A; dissolving the solution A in isopropyl titanate and uniformly mixing to obtain a solution B; transferring the solution B into a high-pressure reaction kettle with a polytetrafluoroethylene lining, wherein the filling degree of the high-pressure reaction kettle is 80%, then putting the high-pressure reaction kettle into an electronic constant-temperature air-blast drying box at 160-220 ℃ for reaction for 12-24 h, taking out the high-pressure reaction kettle after the reaction is finished, naturally cooling to room temperature, and then centrifuging to obtain a precipitate; and washing, drying, grinding and calcining the precipitate to obtain the anatase type nano titanium dioxide microspheres. According to the preparation method, isopropyl titanate is used as a titanium source, diethylenetriamine is used as a crystal face control agent, the titanium dioxide microspheres with exposed (001) crystal faces are prepared, strong corrosive liquid HF is not used, and the problems of equipment corrosion, environmental pollution and the like are avoided.

Description

Preparation method of anatase type nano titanium dioxide microspheres
Technical Field
The invention belongs to the technical field of photocatalytic materials, and particularly relates to a preparation method of anatase type nano titanium dioxide microspheres.
Background
Titanium dioxide (TiO)2) Because of the advantages of high photocatalytic activity, strong light corrosion resistance, environmental friendliness, relatively low price, no toxicity to human bodies and the like, the TiO-based semiconductor material has become a semiconductor material which is most interesting to people in the field of photocatalytic degradation of pollutants, and researches show that the TiO is2Can degrade various organic pollutants into nontoxic small molecular compounds, water, carbon dioxide and the like by photocatalysis; can also reduce heavy metal ions in the solution into nontoxic metals. TiO 22There are three crystal structures: anatase type, rutile type, and brookite type. Brookite type TiO2Belongs to an orthorhombic system, has low photocatalytic activity, is a metastable state, is rarely researched at present, and surrounds anatase type TiO and rutile type TiO2Has relatively more research on rutile type TiO2The heat resistance, the thermal stability and the chemical stability of the material are all superior to those of anatase TiO2Can be widely applied to the fields of coatings, paints, cosmetics, plastics and the like; when used as a catalytic material, anatase type TiO2The photocatalytic activity is obviously higher than that of rutile TiO2And has wide application prospect in the fields of environmental management, organic synthesis, water photolysis and the like.
In 2008, Yang et al, Nature,2008,453, (29) 638 reported that TiF has a lower hydrolysis rate4Takes hydrofluoric acid (HF) as a morphology control agent as a titanium source, and adopts a hydrothermal method to synthesize micron-sized anatase TiO2And (3) single crystal. In 2009, HanAnatase phase TiO reported by J.AM.CHEM.SOC.2009,131, 3152-3153, etc2Nano single crystal. However, in the above studies, researchers all used HF to obtain TiO2And (3) single crystal. HF is a strongly corrosive liquid, and the direct use of HF is dangerous, and has the problems of equipment corrosion, environmental pollution and the like.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a preparation method of anatase type nano titanium dioxide microspheres, wherein the problems of equipment corrosion, environmental pollution and the like are avoided due to the titanium dioxide microspheres with exposed crystal faces in the preparation method (001).
A preparation method of anatase type nano titanium dioxide microspheres specifically comprises the following steps:
(1) dissolving diethylenetriamine in isopropanol, and uniformly mixing to obtain a solution A, wherein the volume ratio of the isopropanol to the diethylenetriamine in the solution A is 280-1400: 1;
(2) dissolving the solution A obtained in the step (1) in isopropyl titanate, and uniformly mixing to obtain a solution B, wherein the volume ratio of isopropanol to isopropyl titanate in the solution B is 28: 1;
(3) transferring the solution B obtained in the step (2) into a high-pressure reaction kettle with a polytetrafluoroethylene lining, wherein the filling degree of the high-pressure reaction kettle is 80%, then putting the high-pressure reaction kettle into an electronic constant-temperature air-blast drying oven at 160-220 ℃ for reaction for 12-24 h, taking out the high-pressure reaction kettle after the reaction is finished, naturally cooling to room temperature, and then centrifuging to obtain a precipitate;
(4) and (4) washing, drying, grinding and calcining the precipitate obtained in the step (3) to obtain the anatase type nano titanium dioxide microspheres.
Further, the specific steps of the step (1) are as follows: under an ultrasonic field, dripping isopropanol into diethylenetriamine, and after the dripping is finished, carrying out ultrasonic dispersion uniformly to obtain a solution A.
Furthermore, the dropping speed of the isopropanol is 5mL/min to 10 mL/min.
Furthermore, the ultrasonic power is 100W-300W, and the ultrasonic dispersion time is 0.5 h-1 h.
Further, the specific steps of the step (2) are as follows: and (3) under an ultrasonic field, dropwise adding the solution A into isopropyl titanate, and after dropwise adding, performing ultrasonic dispersion uniformly to obtain a solution B.
Furthermore, the dropping speed of the solution A is 5mL/min to 10 mL/min.
Further, the ultrasonic power in the step (2) is 100W-300W, and the ultrasonic dispersion time is 0.5 h-1 h.
Further, in the step (4), the precipitate is washed by absolute ethyl alcohol and deionized water in sequence, and the washing is repeated for a plurality of times until the filtrate is neutral, so as to remove organic matters attached to the surface of the precipitate.
Further, drying was performed at a temperature of 60 ℃ and dried for 12 hours.
Further, the resulting mixture was ground and then calcined at 400 ℃ for 2 hours in a muffle furnace to remove organic substances from the interior of the precipitate and to improve crystallinity.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the invention, isopropyl titanate is used as a titanium source, diethylenetriamine is used as a crystal face control agent, isopropanol is used as an organic solvent to prepare the titanium dioxide microsphere, in the reaction process, the interaction between diethylenetriamine and the (001) crystal face of titanium dioxide is stronger than the interaction between diethylenetriamine and the (101) crystal face, diethylenetriamine is selectively adsorbed on the (001) crystal face, the surface energy of the (001) crystal face is reduced, so that the growth of titanium dioxide along the [001] crystal direction is inhibited, the titanium dioxide with the (001) crystal face exposed is further favorably obtained, and the adsorption energy of the (001) crystal face can be adjusted by regulating and controlling the volume ratio of diethylenetriamine and isopropyl titanate. Meanwhile, diethylenetriamine has strong basicity and can promote isopropyl titanate to be hydrolyzed to generate titanium dioxide.
2. According to the invention, the solution A and the solution B are prepared by ultrasonic dispersion, the isopropanol and the diethylenetriamine can be uniformly mixed at a molecular level by virtue of a micro-jet generated by ultrasonic cavitation effect, and then the mixture is dropwise added into isopropyl titanate placed in an ultrasonic field, so that the whole reaction system can be uniformly mixed at a molecular level, and the titanium dioxide microspheres with good dispersibility can be obtained.
3. Compared with the prior art in which strongly corrosive liquid HF is used for preparing titanium dioxide microspheres, the method effectively avoids the problems of equipment corrosion, environmental pollution and the like.
Drawings
Fig. 1-SEM characterization of nano-titania microspheres prepared in example 1.
Fig. 2-SEM characterization of nano titania microspheres prepared in example 2.
Fig. 3-SEM characterization of the nano-titania microspheres prepared in example 3.
FIG. 4-XRD examination of single crystals of titanium dioxide prepared in examples 1-3;
FIG. 5 is a comparison graph of the effect of different catalysts on photocatalytic degradation of rhodamine B (10mg/L) under irradiation of a xenon lamp.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
Example 1
(1) Pouring 1mL of diethylenetriamine into a beaker, dripping 280mL of isopropanol into the diethylenetriamine at the speed of 10mL/min under an ultrasonic field (the ultrasonic power is 300W), and continuing ultrasonic dispersion for 10min after dripping is finished to obtain a solution A;
(2) pouring 10mL of isopropyl titanate into a beaker, dropwise adding the solution A obtained in the step (1) into the beaker at the speed of 5mL/min under an ultrasonic field (ultrasonic power of 300W), and continuously performing ultrasonic dispersion for 0.5h after dropwise adding to obtain a solution B;
(3) transferring the solution B into a high-pressure reaction kettle with a polytetrafluoroethylene lining, wherein the filling degree of the high-pressure reaction kettle is 80%, then putting the high-pressure reaction kettle into an electronic constant-temperature air blowing drying oven at 180 ℃ for reaction for 24 hours, and then cooling to room temperature;
(4) removing supernatant in the high-pressure reaction kettle, and centrifugally collecting precipitates;
(5) washing the precipitate obtained in the step (4) with absolute ethyl alcohol and deionized water for a plurality of times in sequence until the filtrate is neutral;
(6) drying the precipitate washed in the step (5) at 60 ℃ for 12 h;
(7) and (4) grinding the product obtained in the step (6), and roasting in a 400 ℃ muffle furnace for 2h to obtain the 1# titanium dioxide microspheres.
Example 2
(1) Pouring 0.33mL of diethylenetriamine into a beaker, dripping 280mL of isopropanol into the diethylenetriamine at the speed of 10mL/min under an ultrasonic field (the ultrasonic power is 300W), and continuing ultrasonic dispersion for 10min after finishing dripping to obtain a solution A;
(2) pouring 10mL of isopropyl titanate into a beaker, dropwise adding the solution A obtained in the step (1) into the beaker at the speed of 10mL/min under an ultrasonic field (ultrasonic power of 300W), and continuously performing ultrasonic dispersion for 0.5h after dropwise adding to obtain a solution B;
(3) transferring the solution B into a high-pressure reaction kettle with a polytetrafluoroethylene lining, wherein the filling degree of the high-pressure reaction kettle is 80%, then putting the high-pressure reaction kettle into an electronic constant-temperature air blowing drying oven at 180 ℃ for reaction for 24 hours, and then cooling to room temperature;
(4) removing supernatant in the high-pressure reaction kettle, and centrifugally collecting precipitates;
(5) washing the precipitate obtained in the step (4) with absolute ethyl alcohol and deionized water for a plurality of times in sequence until the filtrate is neutral;
(6) drying the precipitate washed in the step (5) at 60 ℃ for 12 h;
(7) and (4) grinding the product obtained in the step (6), and roasting in a 400 ℃ muffle furnace for 2h to obtain the 2# titanium dioxide microspheres.
Example 3
(1) Pouring 0.33mL of diethylenetriamine into a beaker, dripping 280mL of isopropanol into the diethylenetriamine at the speed of 10mL/min under an ultrasonic field (the ultrasonic power is 300W), and continuing ultrasonic dispersion for 10min after finishing dripping to obtain a solution A;
(2) pouring 10mL of isopropyl titanate into a beaker, placing the beaker on a magnetic stirrer, dropwise adding the solution A obtained in the step (1) into the beaker at the speed of 5mL/min, and continuously stirring the solution A for 0.5h after dropwise adding to obtain a solution B;
(3) transferring the solution B into a high-pressure reaction kettle with a polytetrafluoroethylene lining, wherein the filling degree of the high-pressure reaction kettle is 80%, then putting the high-pressure reaction kettle into an electronic constant-temperature air blowing drying oven at 180 ℃ for reaction for 24 hours, and then cooling to room temperature;
(4) removing supernatant in the high-pressure reaction kettle, and centrifugally collecting precipitates;
(5) washing the precipitate obtained in the step (4) with absolute ethyl alcohol and deionized water for a plurality of times in sequence until the filtrate is neutral;
(6) drying the precipitate washed in the step (5) at 60 ℃ for 12 h;
(7) and (4) grinding the product obtained in the step (6), and roasting in a 400 ℃ muffle furnace for 2h to obtain the 3# titanium dioxide microspheres.
1. SEM representations of the titanium dioxide microspheres prepared in the embodiments 1 to 3 are respectively carried out, and the obtained SEM representations are respectively shown in figures 1, 2 and 3.
As can be seen from FIG. 1, the No. 1 titanium dioxide particles are spherical and have a relatively uniform particle size distribution; as can be seen from FIG. 2, the No.2 titanium dioxide particles are spherical, have a larger particle size than the No. 1 titanium dioxide particles, and have a substantially uniform particle size distribution; as can be seen from fig. 3, the degree of agglomeration of the # 3 titanium dioxide particles was severe. Therefore, the magnetic stirrer can not enable isopropanol, isopropyl titanate and diethylenetriamine to reach the molecular level and be uniformly mixed, so that the agglomeration degree of the prepared titanium dioxide particles is serious; the dispersion is carried out by utilizing ultrasonic waves, and the flow of the micro-jet generated by the ultrasonic cavitation effect can achieve the purpose of uniformly mixing isopropanol, diethylenetriamine and isopropyl titanate at the molecular level, so that the particle size of the prepared titanium dioxide single crystal particles is uniform; however, since the amount of diethylenetriamine added in example 1 is larger than that in example 2, which promotes the reduction of the (001) plane surface energy of titanium dioxide, the # 1 titanium dioxide particles prepared in example 1 are smaller than the # 2 titanium dioxide particles prepared in example 2.
2. XRD tests were carried out on the titanium dioxide single crystals prepared in examples 1 to 3, respectively, using an X-ray diffractometer of the D2PHASER type manufactured by Bruker, Germany.
The test conditions were: a Cu target source (λ ═ 0.154056nm), power 30kV × 10mA, measurement temperature 25 ℃, step size 0.02s, dwell time 0.2s, and scan 2 θ angle range 10 ° to 90 °, fig. 4 was obtained.
As can be seen from FIG. 4, the diffraction peak positions (2. theta.) of titanium dioxides No. 1, No.2 and No. 3 were all identical to those of anatase titanium dioxide of JCPDSNo.21-1272, and no other substances were detected, indicating that the single crystal of titanium dioxide produced by the present method was anatase type and had high purity and no impurities.
3. The photocatalytic performance of the titanium dioxide microspheres prepared in examples 1 to 3 was evaluated by using a phchem iii type photochemical reactor manufactured by beijing neubit technologies ltd. The photocatalytic performance of the samples was evaluated by degrading the rhodamine B solution. The light source is visible light of a 350W xenon lamp. The titanium dioxide microspheres prepared in examples 1-3 are labeled as No. 1, No.2 and No. 3 catalysts, respectively.
50mL of 10mg/L rhodamine B solution is respectively taken to be placed in four parallel photocatalytic containers, 0.05g of 1# catalyst, 0.05g of 2# catalyst and 0.05g of 3# catalyst are respectively added into three of the photocatalytic containers, and the fourth photocatalytic container is not added with the catalyst to be used as a blank sample. And respectively putting the solutions into a reaction dark box, magnetically stirring for 1h to reach adsorption equilibrium, and then carrying out a photocatalytic test under the irradiation of a 350W xenon lamp (XE-JY 500). Samples (5 mL each) were taken every 20min and the reaction was stopped at 100 min. And centrifuging the taken sample solution at 3000rpm for 15min by using a centrifuge, and testing the concentration change of the rhodamine B solution at the wavelength of 552nm by using an ultraviolet-visible spectrophotometer, wherein the effect graph is shown in FIG. 5.
As can be seen from fig. 5, the photocatalytic activities of the catalysts # 1 and # 2 are high, and the photocatalytic activity of the catalyst # 1 is higher than that of the catalyst # 2 because the particles of the catalyst # 1 are small and the specific surface area is large; the 3# catalyst adopts magnetic stirring when the solution A consisting of diethylenetriamine is dripped into isopropyl titanate, so that the solution is not uniformly mixed, and finally the prepared titanium dioxide single crystal particles have serious agglomeration degree, so that the photocatalytic activity is low.
Finally, it should be noted that the above-mentioned examples of the present invention are only examples for illustrating the present invention, and are not intended to limit the embodiments of the present invention. Variations and modifications in other variations will occur to those skilled in the art upon reading the foregoing description. Not all embodiments are exhaustive. All obvious changes and modifications of the present invention are within the scope of the present invention.

Claims (10)

1. A preparation method of anatase type nano titanium dioxide microspheres is characterized by comprising the following steps:
(1) dissolving diethylenetriamine in isopropanol, and uniformly mixing to obtain a solution A, wherein the volume ratio of the isopropanol to the diethylenetriamine in the solution A is 280-1400: 1;
(2) dissolving the solution A obtained in the step (1) in isopropyl titanate, and uniformly mixing to obtain a solution B, wherein the volume ratio of isopropanol to isopropyl titanate in the solution B is 28: 1;
(3) transferring the solution B obtained in the step (2) into a high-pressure reaction kettle with a polytetrafluoroethylene lining, wherein the filling degree of the high-pressure reaction kettle is 80%, then putting the high-pressure reaction kettle into an electronic constant-temperature air-blast drying oven at 160-220 ℃ for reaction for 12-24 h, taking out the high-pressure reaction kettle after the reaction is finished, naturally cooling to room temperature, and then centrifuging to obtain a precipitate;
(4) and (4) washing, drying, grinding and calcining the precipitate obtained in the step (3) to obtain the anatase type nano titanium dioxide microspheres.
2. The preparation method of anatase type nano titanium dioxide micro spheres according to claim 1, wherein the step (1) comprises the following specific steps: under an ultrasonic field, dripping isopropanol into diethylenetriamine, and after the dripping is finished, carrying out ultrasonic dispersion uniformly to obtain a solution A.
3. The preparation method of anatase type nano titanium dioxide micro spheres according to claim 2, wherein the dropping speed of the isopropanol is 5-10 mL/min.
4. The preparation method of the anatase type nano titanium dioxide microspheres according to claim 2 or 3, wherein the ultrasonic power is 100W-300W, and the ultrasonic dispersion time is 0.5 h-1 h.
5. The method for preparing anatase type nano titania microspheres according to claim 1 or 2, wherein the step (2) comprises the following specific steps: and (3) under an ultrasonic field, dropwise adding the solution A into isopropyl titanate, and after dropwise adding, performing ultrasonic dispersion uniformly to obtain a solution B.
6. The preparation method of anatase nano titania microspheres according to claim 5, wherein the dropping speed of the solution A is 5-10 mL/min.
7. The preparation method of anatase type nano titanium dioxide microspheres according to claim 5, wherein the ultrasonic power in the step (2) is 100W-300W, and the ultrasonic dispersion time is 0.5 h-1 h.
8. The method for preparing anatase type nano titania microspheres according to claim 1, wherein in the step (4), the precipitate is washed with absolute ethanol and deionized water sequentially, and the washing is repeated for a plurality of times until the filtrate is neutral, so as to remove organic matters attached to the surface of the precipitate.
9. The method for preparing anatase type nano titania microspheres according to claim 1, wherein the drying is performed at 60 ℃ and for 12 h.
10. The method for preparing anatase type nano titania microspheres according to claim 1, wherein the milled nano titania microspheres are placed in a muffle furnace and calcined at 400 ℃ for 2h to remove organic matter inside the precipitate and improve crystallinity.
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CN114768787A (en) * 2022-05-24 2022-07-22 中国科学院生态环境研究中心 Carbon fiber loaded three-layer titanium dioxide photocatalyst and preparation method and application thereof
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