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Preparation method of crystal phase controllable titanium dioxide nanometer crystal

A titanium dioxide and nanocrystalline technology, applied in the direction of titanium dioxide, titanium oxide/hydroxide, etc., can solve the problems that the ratio of anatase and rutile cannot be continuously modulated, difficult to promote industrially, and the preparation cost is high, and it is easy to achieve process parameters. Control, easy industrial promotion, short production cycle effect

Inactive Publication Date: 2004-03-03
FUDAN UNIV
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Problems solved by technology

It has been reported in the literature that different types of titanium esters were used as precursors to prepare nano-titanium dioxide with anatase phase and rutile phase ratios of 0:100, 50:50, and 70:30 (R.R.Bacsa, J.Kiwi, Appl.Catal .B: Environmental, 1998; 16: 19), but the preparation cost of this method is high, the cycle is long, and the ratio of anatase and rutile phase cannot be adjusted continuously, so it is difficult to promote industrially

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  • Preparation method of crystal phase controllable titanium dioxide nanometer crystal
  • Preparation method of crystal phase controllable titanium dioxide nanometer crystal
  • Preparation method of crystal phase controllable titanium dioxide nanometer crystal

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example 10

[0025] The XRD patterns of samples 1-9 were measured on a Rigaku D / MAX-IIA diffractometer, and the peaks at 25.2, 38.7 and 48.0° belonged to the diffraction of anatase (101), (004) and (200) crystal planes, respectively , and the peaks at 27.4, 36.1, 41.2, and 54.3° are assigned to the diffraction of rutile (110), (101), (111) and (211) crystal planes, respectively. The proportion of anatase phase and rutile phase in titanium dioxide using the phase quantification formula x A =(1+1.26I R / I A ) -1 Calculate (C.C. Wang, J.Y. Ying, Chem. Mater, 1999; 11:3113), where x A is the proportion of anatase phase, I A and I R are the intensities of the diffraction peaks attributed to anatase and rutile, respectively, and the results are shown in Table 1. Examples 11~12

example 11～12

[0026] Dissolve 0.1 mol of butyl titanate in 1.5 mol of absolute ethanol, add dropwise a mixture of 1 mol of ethanol and 5 mol of water, stir at room temperature for 3 hours, then filter with suction and dry at room temperature to obtain amorphous titanium dioxide powder. Add a certain amount of hydrochloric acid (20mL / g titanium dioxide powder) to the amorphous titanium dioxide powder, the concentration is 0.2, 0.3mol / L respectively, stir at room temperature for 1 hour, 180 ℃ hydrothermal crystallization for 24 hours, after suction filtration, Titanium dioxide samples were obtained by washing and drying, which were respectively recorded as samples 11 and 12, and the proportion of the anatase phase was determined by the method of Example 10. Examples 13-14

example 13～14

[0027] Dissolve 40ml of titanium tetrachloride in 100mL of 0.6N hydrochloric acid, and then add dropwise 1:1 ammonia water until the pH value is 9-10. Aging at room temperature for 12 hours, suction filtration, washing with distilled water until there is no chloride ion, drying and grinding to obtain amorphous titanium dioxide powder. Add a certain amount of hydrochloric acid (10mL / g titanium dioxide powder) to the amorphous titanium dioxide powder, the concentration is 0.3mol / L, stir at room temperature for 1 hour, 150°C hydrothermal crystallization for 24 and 48 hours respectively, after suction filtration, Titanium dioxide samples were obtained by washing and drying, respectively recorded as samples 13 and 14, and the proportion of the anatase phase was determined by the method of Example 10. Examples 15-18

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Abstract

A process for preparing the crystal phase controllable TiO2 nanocrystals includes such steps as hydrolyzing the Ti-cotnained compound in the aqueous solution of alcohol to obtain amorphous TiO2 powder, adding inorganic acid, hydrothermal treating, filtering, washing and drying. Its resultant TiO2 nanocrystal has the continuously regulatable ratio of anatase phase to rutile phase.

Description

technical field [0001] The invention is a method for preparing nano-titanium dioxide whose phase ratio of anatase and rutile is continuously adjustable. By using the method, titanium dioxide nanocrystals of mixed crystal phases can be obtained without high-temperature roasting, and the ratio of the two crystal phases can be continuously adjusted by controlling the preparation conditions. Background technique [0002] Due to its good photoelectric properties, chemical stability, wear resistance, and non-toxicity to organisms, nano-titanium dioxide has been widely used in gas sensors, pressure sensitive elements, solar cells, nonlinear optical materials, and environmental purification materials, etc. preparation. There are mainly three crystal forms of titanium dioxide in nature: brookite, anatase and rutile, and the artificially synthesized ones are mainly the latter two. Recent research results show that the photocatalytic activity of titanium dioxide containing anatase an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/047C01G23/053
Inventor 乐英红吴春莹邓兴毅高滋
Owner FUDAN UNIV
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