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Method for preparing titanium dioxide nanoparticles

A nanoparticle, titanium dioxide technology, applied in titanium dioxide, titanium oxide/hydroxide, nanotechnology and other directions, to achieve the effect of simple and easy process, reduced production cost and low reaction temperature

Active Publication Date: 2014-06-04
吉林省润臻分离技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition, there are few reports in the literature on the preparation of anatase phase titanium dioxide nanoparticles below 5 nm and rutile phase titanium dioxide nanoparticles below 10 nm.

Method used

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  • Method for preparing titanium dioxide nanoparticles
  • Method for preparing titanium dioxide nanoparticles
  • Method for preparing titanium dioxide nanoparticles

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] The total amount is 180ml, and the volume ratio of cyclohexane:ethanol=1:0.5 is mixed as a solvent, and 36ml of tetrabutyl titanate is added to the mixed solvent. After stirring evenly, add 8ml of concentrated hydrochloric acid (36-38%) according to the ratio of tetrabutyl titanate:concentrated hydrochloric acid=1:0.22 by volume. Reflux for 10 hours after heating up to boiling. The reflux reaction product (light yellow transparent liquid) was added dropwise with 3 times the volume of ethanol under the condition of stirring, the stirring was stopped, and it settled overnight. The resulting product was washed, centrifuged and dried.

[0033] Figure 1~3 The X-ray diffraction spectrum, transmission electron microscope pictures and high resolution transmission electron microscope pictures of the prepared titanium dioxide nanoparticles are given respectively. The obtained product is monodisperse anatase phase titanium dioxide nanoparticles with a particle diameter of less...

Embodiment 2

[0035] The total amount is 180ml, and the volume ratio of cyclohexane:ethanol=1:5 is mixed as a solvent, and 36ml of tetrabutyl titanate is added to the mixed solvent. After stirring evenly, add 8ml of concentrated hydrochloric acid (36-38%) according to the ratio of tetrabutyl titanate:concentrated hydrochloric acid=1:0.22 by volume. Reflux for 10 hours after heating up to boiling. The reflux reaction product (light yellow transparent liquid) was added dropwise with 3 times the volume of ethanol under the condition of stirring, the stirring was stopped, and it settled overnight. The resulting product was washed, centrifuged and dried.

[0036] Compared with Example 1, the volume ratio of the reaction solvent cyclohexane:ethanol was changed to 1:5, and the obtained product was titanium dioxide nanoparticles in anatase phase with no obvious change in morphology. Figure 4 X-ray diffraction pattern for the product. When the volume ratio of the reaction solvent hexamethylene: ...

Embodiment 3

[0038] The total amount is 180ml, and the volume ratio of cyclohexane:ethanol=1:0.5 is mixed as a solvent, and 36ml of tetrabutyl titanate is added to the mixed solvent. After stirring evenly, add 9 ml of concentrated hydrochloric acid (36-38%) according to the ratio of tetrabutyl titanate:concentrated hydrochloric acid=1:0.25 by volume. Reflux for 10 hours after heating up to boiling. The reflux reaction product (light yellow transparent liquid) was added dropwise with 3 times the volume of ethanol under the condition of stirring, the stirring was stopped, and it settled overnight. The resulting product was washed, centrifuged and dried.

[0039]Compared with Example 1, the reactant volume ratio of tetrabutyl titanate:concentrated hydrochloric acid was changed to 1:0.25, and the obtained product was titanium dioxide nanoparticles in anatase phase with no obvious change in morphology. Figure 5 X-ray diffraction pattern for the product. When reactant volume ratio tetrabutyl...

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Abstract

The invention provides a method for preparing titanium dioxide nanoparticles and belongs to the technical field of inorganic material preparation processes. The method provided by the invention comprises the following steps: adding tetrabutyl titanate and concentrated hydrochloric acid to a mixed solvent of cyclohexane and ethanol, and reacting under a reflux condition to obtain monodispersed anatase-phase titanium dioxide nanoparticles. The product can be gradually transformed into rutile phase from the anatase phase by increasing the dosage of the concentrated hydrochloric acid, and as a result, the pure rutile phase can be obtained at last. The method is simple, convenient and easy to implement, and can be used for avoiding complex steps of adding a surfactant, high-temperature firing and the like of the prior art, and the obtained anatase-phase titanium dioxide nanoparticles are monodispersed and have a particle size less than 5nm; the obtained rutile-phase titanium dioxide nanoparticles have the particle size less than 10nm; the phase of the titanium dioxide nanoparticles is controlled by changing the dosage of the reactant in the same synthetic system, which is advantageous for industrial production.

Description

technical field [0001] The invention provides a method for preparing titanium dioxide nanoparticles, which belongs to the technical field of inorganic material preparation technology. Background technique [0002] The industrial production of titanium dioxide originated in the early 20th century, and it was used as a pigment in sunscreens, paints, ointments, toothpaste and other products. In 1972, Fujishima et al. first discovered the phenomenon that titanium dioxide electrodes can catalyze the decomposition of water and generate hydrogen under the irradiation of ultraviolet lamps (Nature, 1972, 238, 37-38). Since then, titanium dioxide nanomaterials have received extensive attention, and with in-depth research, it has shown broad application prospects in the fields of luminescent materials, solar cells, electronic devices, and dielectric materials (Advanced Materials, 2005, 17, 1991 -1995; Nano Letter, 2006, 6, 215-218; Nanotechnology, 2004, 15, 1277-1283). [0003] The k...

Claims

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Application Information

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IPC IPC(8): C01G23/053B82Y30/00
Inventor 庞广生刘旭焦世惠
Owner 吉林省润臻分离技术有限公司
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