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Method for preparing single dispersing ball-shape mesoporous titanium dioxide colloid particles whose size and apparance are controllable

A technology of mesoporous titanium dioxide and colloidal particles, which is applied in the treatment of titanium dioxide, titanium oxide/hydroxide, and dyed polymer organic compounds, can solve the problems of difficult control of shape and size, complexity and time-consuming, and poor monodispersity of particles. Easy to popularize and apply, cheap solvent, low energy consumption

Inactive Publication Date: 2007-11-14
TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Preparation of monodisperse spherical mesoporous TiO 2 The method of colloidal particles is mainly based on mesoporous carbon spheres and mesoporous SiO 2 The sphere is used as a template, and titanate is used as a raw material, which is infiltrated into a mesoporous carbon sphere template and hydrolyzed, and then the template is removed. synthesis of mesoporous spheres of metal ofoxi des and phosphates", J.Am.Chem.Soc., 2003, No. 125, pages 4976-4977), the disadvantage of this method is that it is more complicated and time-consuming
In addition, Yunxia Zhang et al. directly prepared mesoporous TiO by introducing surface activity into the alcohol system. 2 Colloidal particles (see the literature "The formation of mesoporous TiO 2 spheres via a facie chemical process”, J.Phys.Chem.B, 2005, 109, pp. 5478-5481), but the monodispersity of the particles obtained by the above method is poor, and the shape and size are not easy to control

Method used

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  • Method for preparing single dispersing ball-shape mesoporous titanium dioxide colloid particles whose size and apparance are controllable

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] (1) absolute ethanol and acetonitrile are mixed uniformly in a volume ratio of 1:2;

[0032] (2) Dissolve tetrabutyl titanate in the mixed solvent obtained in step (1), and stir evenly, wherein the initial concentration of tetrabutyl titanate is 2×10 -3 mole / liter;

[0033] (3) ammoniacal liquor is added in the mixed solvent of step (1) gained, stir, then add a certain amount of commercially available diameter and be the PSMMA ball of 220nm to disperse evenly, wherein the initial concentration of ammonia is 0.1 mol / liter, PSMMA ball The initial concentration of 0.02 g / L;

[0034] (4) At room temperature, the solution prepared in step (3) is added to the reactor, and then the tetrabutyl titanate mixed solvent solution prepared in step (2) is added to the reactor, wherein step (2) and Step (3) The volume ratio of the solution is 1:2, and the reaction is stirred for 12 hours to obtain a milky white or white turbid liquid, which is centrifuged to obtain colloidal particle...

Embodiment 2

[0038] (1) absolute ethanol and acetone are mixed uniformly in a volume ratio of 10:3;

[0039] (2) Dissolve tetrabutyl titanate in the mixed solvent obtained in step (1), and stir evenly, wherein the initial concentration of tetrabutyl titanate is 5×10 -4 mole / liter;

[0040] (3) ammoniacal liquor is added in the mixed solvent of step (1) gained, stir, then add a certain amount of diameter and be the PSMMA ball of 260nm and disperse evenly, wherein the initial concentration of ammonia is 0.06 mol / liter, the initial concentration of PSMMA ball 0.012 g / L;

[0041] (4) Add the solution prepared in step (3) into the reactor at room temperature (25-30°C), and then add the tetrabutyl titanate mixed solvent solution prepared in step (2) into the reactor, Wherein the volume ratio of step (2) to step (3) solution is 3: 2, stirring and reacting for 2 hours, milky white or white turbid liquid is obtained, centrifuged to obtain styrene-methacrylic acid copolymer microsphere surface coa...

Embodiment 3

[0045] (1) absolute ethanol and acetonitrile are mixed uniformly in a volume ratio of 1:13;

[0046] (2) Dissolve tetraisopropyl titanate in the mixed solvent obtained in step (1), and stir evenly, wherein the initial concentration of tetraisopropyl titanate is 2.5×10 -2 mole / liter;

[0047] (3) water is added in the mixed solvent of step (1) gained, stir well, then add the PSMMA ball that a certain amount of self-made diameter is 350nm and disperse evenly, wherein the initial concentration of water is 0.1 mol / liter, the PSMMA ball's The initial concentration is 0.025 g / L;

[0048] (4) At room temperature, add the solution prepared in step (3) into the reactor, and then add the tetraisopropyl titanate mixed solvent solution prepared in step (2) into the reactor, wherein step (2) The volume ratio to the solution in step (3) is 4:1, and the reaction is stirred for 3 hours to obtain a milky white or white turbid liquid, which is centrifuged to obtain colloidal particles of styr...

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Abstract

The invention belongs to the field of preparing material of nanometer and sub-micron of inorganic semiconductor, it is especially relates to the preparation method of colloid granule of TiO2 whose size is between dozens of nanometers and dozens of sub-microns, whose pattern can be controlled, which is monodisperse and has spherical mesoporous. At room temperature, wrap up and cover a layer of TiO2 on surface of polymeric microballoon sphere (PSMMA) and then swell and infiltrate it through the mixed solution of toluene or tetrahydrofuran and ethanol, make colloid granule of TiO2 which is monodisperse and which has spherical mesoporous after getting even complex granule. The preparation method of this invention is simple, the colloid granule of TiO2 has high purity and good dispersibility, diameter of the granule is between 20-2000 nanometer, specific area is between 50-1000m2 / g, the size of the granule distributes narrowly and the warp is smaller than 10%, and the size of granule can be controlled through the covering thickness of TiO2 and size of granule of PSMMA .

Description

technical field [0001] The invention belongs to the field of preparation of inorganic semiconductor nanometer and submicron materials, and in particular relates to a preparation method of monodisperse and spherical mesoporous titanium dioxide colloidal particles whose size and shape are controllable from tens of nanometers to submicrons. Background technique [0002] Titanium dioxide, commonly known as titanium dioxide, is a highly functional and fine inorganic material that has been studied more. High chemical stability, thermal stability, non-toxicity, photoactivity and other unique properties, so it is widely used in chemical industry, electronics, biology, coatings, sensors, dielectric materials, plastics, ink, paper, chemical fiber, rubber, separation, etc. fields, such as: [0003] (1) TiO 2 It is a good photocatalyst, especially when they have mesoporous structure and nanometer size, due to the increase of specific surface area, the bonding state of the surface is d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/047C09C1/36C09C3/10
Inventor 唐芳琼王鹏陈东
Owner TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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