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Method for preparing nano-titanium dioxide with controllable phase composition

A nano-titanium dioxide and butyl titanate technology, applied in the field of chemistry, can solve the problems of difficult particle size control, waste of resources, etc., and achieve the effects of small grain size, controllable grain size, and wide application.

Inactive Publication Date: 2013-05-22
CHANGCHUN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Combining the advantages of the sol-gel method and the microemulsion method to prepare nano-titanium dioxide effectively, this method can well control the particle size of nano-titanium dioxide within a certain range by modifying the test parameters. The preparation of nanoparticles is optimized, which solves the problem that the size of nano-titanium dioxide particles is difficult to control in the preparation of sol-gel method, and the problem of unnecessary waste of resources caused by high-temperature roasting

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  • Method for preparing nano-titanium dioxide with controllable phase composition

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Effect test

Embodiment 1

[0029] as attached figure 1 As shown in the curve a, the preparation method of nano-titanium dioxide with controllable crystal phase composition of the present invention includes the following steps: adding 1.2 g of cetyltrimethylammonium bromide (CTAB) to 100 g of absolute ethanol- Cyclohexane mixture, in which the ratio of absolute ethanol to cyclohexane is 4.2:1, stir until cetyltrimethylammonium bromide (CTAB) is completely dissolved; add 14.3g n-octanol and 3.2g pH to the liquid Nitric acid aqueous solution with pH=6, after stirring evenly, add 6.7g of butyl titanate, stir for 0.5 hours, let stand for 6 days, dry at 100°C to constant weight, and bake at 650°C for 5 hours. The rutile phase in the prepared nano-titanium dioxide is 62.9%, and the anatase phase is 37.1%.

Embodiment 2

[0031] as attached figure 1 As shown in the middle b curve, the preparation method of nano-titanium dioxide with controllable crystal phase composition of the present invention comprises the following steps: adding 1.2 g of cetyltrimethylammonium bromide to 100 g of dehydrated alcohol-cyclohexyl alkane mixture, wherein the mass ratio of absolute ethanol to cyclohexane is 2.1:1, and stirred until cetyltrimethylammonium bromide (CTAB) is completely dissolved. Add 14.3g of n-octanol and 3.2g of nitric acid aqueous solution with pH=6 to the liquid, stir evenly, add 6.7g of butyl titanate, stir for 0.5 hour, and let it stand for 6 days. Dry at 100°C to constant weight. Baking at 650°C for 5 hours. The rutile phase in the prepared nano-titanium dioxide is 80.5%, and the anatase phase is 19.5%.

Embodiment 3

[0033] as attached figure 1 As shown in the curve c in the middle, the preparation method of nano-titanium dioxide with controllable crystal phase composition of the present invention comprises the following steps: adding 1.2 g of cetyltrimethylammonium bromide (CTAB) to 100 g of absolute ethanol -Cyclohexane mixed solution, wherein the absolute ethanol-cyclohexane mass ratio is 1:1, stirred until cetyltrimethylammonium bromide (CTAB) is completely dissolved. Add 14.3g of n-octanol and 3.2g of nitric acid aqueous solution with a pH of 6 to the liquid, stir evenly, add 6.7g of butyl titanate, stir for 0.5 hours, let stand for 6 days, dry at 100°C until constant weight, 650°C Lower roasting for 5 hours. The rutile phase in the prepared nano-titanium dioxide is 100%, and the anatase phase is 0%.

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Abstract

Belonging to the technical field of chemistry, the invention mainly relates to a method for preparing nano-titanium dioxide with controllable phase composition. The method mainly comprises the steps of: using a surfactant and a cosurfactant to disperse water in a mixed solution of absolute ethyl alcohol and cyclohexane; adding butyl titanate into the mixed solution and make it hydrolyzed in the mixed solution; leaving the mixed solution to stand at room temperature and then conducting thermal treatment. The invention adopts a new method to control the crystal phase composition of nano-titanium dioxide, and only by changing the ratio between absolute ethyl alcohol and cyclohexane, the phase composition of nano-titanium can be controlled effectively, thus realizing the purposes of simple preparation method, simple preparation method and accurate control of the crystal phase composition of nano-titanium dioxide.

Description

technical field [0001] The invention relates to the field of chemical technology, and relates to a method for preparing nano titanium dioxide with a controllable phase composition, in particular to a method for preparing nano titanium dioxide with a controllable phase composition. Background technique [0002] The existing preparation methods of nanomaterials are mainly sol-gel method, hydrothermal method and microemulsion method. Generally, when nano-titanium dioxide is prepared by the sol-gel method, the hydrolyzed titanium precursor is often used to obtain nano-titanium dioxide particles. Water is mixed with other organic solvents to control the rate of hydrolysis. However, this method cannot achieve a very ideal effect on the particle size control of nano-titanium dioxide; while the control of nanoparticles by the microemulsion method can be well controlled by the size of the microemulsion. The control of the phase composition of nano-titanium dioxide is usually achiev...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G23/053B82Y40/00
Inventor 张宝昌赵振波王泽青
Owner CHANGCHUN UNIV OF TECH
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