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Method and device for preparing rare earth-doped nano-titanium dioxide photocatalyst by supercritical carbon dioxide method

A nano-titanium dioxide and carbon dioxide technology, applied in metal/metal oxide/metal hydroxide catalysts, physical/chemical process catalysts, chemical instruments and methods, etc., can solve the problem that the photocatalytic performance cannot be better breakthrough, etc. To achieve the desired effect of photocatalytic performance

Inactive Publication Date: 2014-10-01
SHANGHAI NAT ENG RES CENT FORNANOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But looking at their preparation conditions, they all adopt traditional hydrothermal method, sol-gel method or precipitation method, etc., and the reaction environment of liquid solvent has a great influence on the obtained TiO 2 The crystal form, grain size and doping degree of rare earth elements are limited, and the photocatalytic performance cannot be better breakthrough.

Method used

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  • Method and device for preparing rare earth-doped nano-titanium dioxide photocatalyst by supercritical carbon dioxide method
  • Method and device for preparing rare earth-doped nano-titanium dioxide photocatalyst by supercritical carbon dioxide method
  • Method and device for preparing rare earth-doped nano-titanium dioxide photocatalyst by supercritical carbon dioxide method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Example 1, see figure 1

[0023] (1) Take 17ml of tetrabutyl titanate, La(NO 3 ) 3 ·nHO 2 Weigh 0.6498g, dissolve in 150ml of absolute ethanol, stir well until the nitrate hydrate is completely dissolved to obtain a uniform solution, and add it to the reaction kettle A41, stirring at an appropriate speed; heat A41 to 120°C; High-purity CO 2 Pump into A41, the pressure rises to 430bar, close k3;

[0024] (2) Add 6ml of deionized water into the preheating container A31 and raise the temperature to 120°C; 2 Pump into the reactor A31, raise the pressure to 450bar;

[0025] (3) Open k4, the deionized water in A31 will be supercritical CO 2 The fluid is carried into the A41, and the deionized water and the liquid medicine are fully mixed and reacted under the action of stirring. Continue to pump CO into A31 2 To achieve a holding pressure value of 450bar, constant pressure and temperature for 24 hours;

[0026](4) After the reaction is over, collect the material fro...

Embodiment 2

[0027] Embodiment 2: see figure 1 ,

[0028] (1) Take 8ml of tetrabutyl titanate, Y(NO 3 ) 3 ·6HO 2 Weigh 0.0479g, dissolve it in 70ml of absolute ethanol, stir well until the nitrate hydrate is completely dissolved to obtain a uniform solution, and add it to the reaction kettle A41, stirring at an appropriate speed; heat A41 to 140°C; High-purity CO 2 Pump into A41, the pressure rises to 320bar, close k3;

[0029] (2) Add 3ml of deionized water into the preheating container A31 and raise the temperature to 140°C; 2 Pump into the reactor A31, raise the pressure to 350bar;

[0030] (3) Open k4, the deionized water in A31 will be supercritical CO 2 The fluid is carried into the A41, and the deionized water and the liquid medicine are fully mixed and reacted under the action of stirring. Continue to pump CO into A31 2 To achieve a holding pressure value of 350bar, constant pressure and temperature for 16 hours;

[0031] (4) After the reaction is over, collect the materi...

Embodiment 3

[0032] Example 3, see figure 1

[0033] (1) Take tetraisopropyl titanate 15ml, Gd(NO 3 ) 3 ·6HO 2 Weigh 0.0925g, dissolve in 140ml of absolute ethanol together, stir well until the nitrate hydrate is completely dissolved to obtain a uniform solution, and add it to the reaction kettle A41, stirring at an appropriate speed; heat A41 to 140°C; High-purity CO 2 Pump into A41, the pressure rises to 220bar, close k3;

[0034] (2) Add 6ml of deionized water into the preheating container A31 and heat up to 140°C; 2 Pump into the reactor A31, raise the pressure to 250bar;

[0035] (3) Open k4, the deionized water in A31 will be supercritical CO 2 The fluid is carried into the A41, and the deionized water and the liquid medicine are fully mixed and reacted under the action of stirring. Continue to pump CO into A31 2 To achieve a holding pressure value of 250bar, constant pressure and temperature for 8 hours;

[0036] (4) After the reaction is over, collect the material from t...

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Abstract

The invention relates to a method and a device for preparing rare earth doping nano-titania photocatalyst with supercritical carbon dioxide process. The method comprises the following specific steps: adding titanium alkoxide, absolute ethyl alcohol and rare earth element nitrate hydrate in a reaction kettle for stirring and dissolving; pumping high purity CO2 in the reaction kettle at the temperature of 110-150 DEG C under the pressure of 80-500 bar; adding deionized water in a deionized water dissolving kettle and raising the temperature till 110-150 DEG C; then pumping high purity CO2 in the deionized water dissolving kettle under the pressure of 80-500 bar, and causing the pressure difference between the deionized water dissolving kettle and the reaction kettle to be kept at 10-30 bar; flowing supercritical CO2 fluid doped with deionized water in the reaction kettle at the temperature of 110-150 DEG C and under the pressure of 80-500 bar, stirring for 4-24h for reaction; and after the reaction is finished, drying obtained products after being washed, and grinding the products so as to obtain the rare earth doping nano-titania photocatalyst.

Description

technical field [0001] The invention relates to a method and a device for preparing a rare earth-doped nano-titanium dioxide photocatalyst, in particular to a method and a device for preparing a rare-earth-doped nano-titanium dioxide photocatalyst by a supercritical carbon dioxide method. Background technique [0002] In recent years, while enjoying rapid economic growth, we are also facing the largest, most extensive and most serious energy shortage and environmental pollution problems in Chinese history. The treatment and recycling of the accompanying waste and emissions to reduce resource consumption and environmental pollution have attracted more and more attention. The photocatalytic technology developed in recent years using semiconductor metal oxides as catalysts provides us with an ideal method for energy utilization and environmental pollution control, especially it can use inexhaustible and inexhaustible solar energy to process Toxic and harmful substances, improv...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/10C02F1/30
Inventor 陈超赵斌林琳柴瑜超何丹农
Owner SHANGHAI NAT ENG RES CENT FORNANOTECH
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