Method for preparing titanic oxide nano powder with visual light catalytic activity
A catalytic activity, titanium dioxide technology, applied in the direction of titanium dioxide, chemical instruments and methods, titanium oxide/hydroxide, etc., can solve the problems of inability to control the relative content of anatase and rutile nano-TiO2, use restrictions, etc., and achieve the change of visible light. Absorption Threshold, Change Absorption Rate, Easily Controlled Effects
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[0025] 1 nm TiO 2 preparation (see figure 1 )
[0026] In the fume hood, measure 20-50ml of TiCl with a dry clean measuring cylinder 4 , slowly pour it into a clean beaker filled with ice cubes, while stirring constantly, be careful not to let the TiCl 4 The liquid drips onto the beaker wall, otherwise the TiCl 4 When the liquid meets the water vapor on the beaker wall, a yellow precipitate will form on the beaker wall, affecting the TiCl 4 The purity of the aqueous solution. After the ice cubes are completely dissolved, a clear, colorless and transparent TiCl 4 Aqueous solution, the solution concentration is 1.5-3.0M.
[0027] In the prepared TiCl 4 Added to the aqueous solution (NH 4 ) 2 SO 4 Crystals, added (NH 4 ) 2 SO 4 The amount of crystals makes SO 4 2- / Ti 4+ The ion concentration ratio is 10-20. Stir fully to ensure the uniformity of the solution. After mixing evenly, move the mixed solution into a constant temperature water bath for constant temperat...
Embodiment 1
[0034] Prepare TiCl as above 4 , the TiCl 4 After hydrolyzing and aging at about 95°C, add ammonia water to adjust the pH value of the mixture to 6.1, and obtain nano-TiO after suction filtration, washing and drying 2 Powder, through XRD analysis (see figure 2 ), it was found that the 2θ of the characteristic diffraction peak of the (101) crystal plane is about 25.3°, which belongs to the anatase structure, and the spectral line broadening is obvious, indicating that its crystallinity is not good. TEM observation finds that its particle diameter is 6-10nm (see image 3 ). The O / Ti atomic ratio was determined to be 2.0 by XPS. UV-Vis Diffuse Reflectance Spectroscopy (DRS) analysis shows that its light absorption threshold is less than 400nm, which is only limited to the ultraviolet region.
[0035] The anatase nano-TiO 2 Calcined at 400°C for 1h under vacuum conditions, with a heating rate of 35°C / h. Its crystal structure is tested by XRD, and it is found that it is sti...
Embodiment 2
[0038] The difference from Example 1 is that the vacuum calcination temperature is 1000°C, the heating rate is 50°C / h, and the time is 0.5h. Its crystal structure was tested by XRD, and it was found that it had all transformed into rutile ( Figure 5 ). The O / Ti atomic ratio was determined to be 1.9390 by XPS. UV-Vis Diffuse Reflectance Spectroscopy (DRS) analysis showed that the light absorption threshold of the sample was red-shifted to 600nm after calcination. Add calcined nano-TiO 2 The degradation rate of the methyl orange solution was 40.055% after visible light irradiation for 3 hours.
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