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Method for preparation of TiO2 by steam hot solution evaporation

A technology of hot solution and steam, applied in chemical instruments and methods, chemical/physical processes, titanium oxide/hydroxide, etc., can solve problems such as unfavorable photocatalytic degradation performance, explosion hazard, and difficult control of hydrolysis process, etc. Effect of photocatalytic performance, improvement of photoresponse range, and promotion of exposed growth

Inactive Publication Date: 2019-08-23
ANHUI UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But there are also some deficiencies. Firstly, the conventional hydrothermal reaction prepares TiO 2 In the process, water is used as a solvent, and the hydrolysis reaction rate is fast, so the hydrolysis process is difficult to control, and the prepared sample has large particles and small specific surface area, which is not good for photocatalytic degradation performance. In order to solve this problem, a dispersant is usually added to the reaction solution , will face the problem of being difficult to clean
Secondly, when preparing samples by the conventional hydrothermal method, the reaction temperature is usually below 220°C due to the limitation of the reaction kettle itself, because the polytetrafluoroethylene lining in the reaction kettle will be seriously deformed at 230°C, resulting in poor sealing and easy explosion hazard
However, the lower reaction temperature will lead to a low degree of crystallization of the sample, and subsequent heat treatment is required for further crystallization.

Method used

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  • Method for preparation of TiO2 by steam hot solution evaporation
  • Method for preparation of TiO2 by steam hot solution evaporation
  • Method for preparation of TiO2 by steam hot solution evaporation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) Take 4 mL of isopropyl titanate (TIP), drop it into 96 mL of ethanol, and stir it magnetically for 30 minutes.

[0026] (2) Transfer the solution in step (1) to a 120mL quartz high foot.

[0027] (3) Weigh 200mL of ethanol into a 1000mL high-temperature and high-pressure reactor, and put the quartz cup in (2) into the high-temperature and high-pressure reactor. Carry out following condition reaction respectively subsequently:

[0028] The reaction was carried out at 240° C. for 5 hours. After the solution is cooled, there will be a small amount of liquid precipitate in the quartz cup, and the product obtained by centrifugation will be washed with absolute ethanol for 4-5 times, then the supernatant will be poured off, and the resulting precipitate will be placed in a vacuum drying oven at 60 °C for 12 hours to obtain TiO 2 Nanoparticles①;

[0029] The reaction was carried out at 250° C. for 5 hours. After the solution is cooled, the product in the cup is a dry ...

Embodiment 2

[0032] (1) Test TiO with X-ray polycrystal diffractometer (XRD; Smartlab9KW) 2 For the X-ray diffraction pattern of nanoparticles, see figure 2 . Depend on figure 2 Medium TiO 2 The position and relative intensity of the nanoparticle diffraction peaks are compared with the standard PDF card No.21-1272, which shows that the TiO we prepared 2 The crystal structure of nanoparticles is tetragonal anatase phase.

[0033] (2) Characterization of TiO prepared at 240°C by transmission electron microscope (JEOLJEM-2100) 2 The transmission electron microscope (TEM) picture of the nanoparticle (i.e. particle ①), see image 3 (a); Characterization of TiO at 250°C 2 Transmission electron micrograph (TEM) of nanoparticles (i.e. particles ②), see image 3 (b); Characterization of 250°C TiO 2 High-resolution transmission electron micrographs (HRTEM) of nanoparticles, see Fig. 3(c) and (d)

[0034] Depend on image 3(a) and image 3 (b) It can be seen that the prepared TiO 2 Nano...

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Abstract

The invention discloses a method for preparation of TiO2 by steam hot solution evaporation. The method includes: dripping a titanium salt into an organic solvent, performing magnetic stirring and mixing, transferring the mixture into a standing quartz cup, then adding an organic solvent into a Hadtelloy alloy reaction kettle, and putting the standing quartz cup into the reaction kettle, carrying out steam hydrothermal reaction for 5h, then introducing cooling water to a condenser pipe in the reaction kettle to rapidly lower the temperature inside the kettle, after cooling to room temperature,taking out the product from the cup, when the product in the cup is in a solid state, performing levigating to obtain a TiO2 photocatalyst, and when the product in the cup is in a liquid state, conducting solid-liquid separation, then adding ethanol and performing washing, and then conducting drying in a vacuum oven to obtain the TiO2 photocatalyst. The TiO2 photocatalyst obtained by the method provided by the invention has the characteristics of excellent catalytic performance and simple and safe preparation process, and has good application prospects in the field of photocatalysis.

Description

technical field [0001] The present invention relates to the preparation of TiO by steam thermal solution evaporation 2 The method belongs to the field of photocatalyst technology. Background technique [0002] TiO 2 It has broad application prospects in the field of photocatalytic degradation, TiO prepared by conventional methods 2 The (101) crystal plane is usually exposed in the crystal, and the disadvantages of the (101) plane are low carrier mobility and few reactive sites. [0003] The researchers found that TiO 2 The (001) face has a high density of active unsaturated Ti atoms, which has a higher photocatalytic activity than the (101) face. Therefore, the exposed TiO on the (001) plane 2 It has great application potential in the field of photocatalysis. In order to expose the (001) plane during crystal growth, it is usually necessary to add F-ions such as strong corrosive hydrofluoric acid, or strong oxidizing agents such as H 2 o 2 , Adding these substances wi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/053B01J21/06
CPCC01G23/0536C01G23/053B01J21/063C01P2002/72C01P2004/04C01P2002/84C01P2002/82B01J35/39Y02P20/54
Inventor 马永青刘畅孙筱雨钱旎娴
Owner ANHUI UNIVERSITY
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