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Process for preparing nanometer titanium dioxide

A nano-titanium dioxide and nano-technology, applied in the direction of titanium dioxide, titanium oxide/hydroxide, etc., can solve the problems of difficult particle size control, high production cost, complex process, etc., and achieve low cost, simple preparation method, and easy-to-obtain raw materials Effect

Inactive Publication Date: 2008-01-09
SHANGHAI NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The technical problem to be solved in the present invention is to provide a preparation method of nano-titanium dioxide to overcome the defects of complex process, high production cost and difficult control of particle size in the prior art

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] The preparation technology of present embodiment nano-titanium dioxide comprises the following steps:

[0020] 1) Prepare 2.5mol / L of TiCl 4 aqueous solution;

[0021] 2) Preparation of TiCl 4 Mixed solution of aqueous solution and concentrated hydrochloric acid, in which TiCl 4 The volume ratio of aqueous solution to concentrated hydrochloric acid is 3.8:1;

[0022] 3) Add 10% aqueous ammonia solution dropwise to the above 100ml mixed solution in an ice-water bath, stir while adding dropwise, and stop adding the aqueous ammonia solution when the pH of the reaction system is 6-9;

[0023] 4) Aging for half an hour, filter the precipitate, and wash the chloride ions in the precipitate with deionized water until AgNO is added dropwise to the washed aqueous solution. 3 Until the solution has no white precipitate, the precursor is obtained;

[0024] 5) Add 3 to 5 grams of citric acid to the precursor;

[0025] 6) Calcined at 450°C for 3 hours to obtain anatase nano-Ti...

Embodiment 2

[0027] The preparation technology of present embodiment nano-titanium dioxide comprises the following steps:

[0028] 1) Prepare 5mol / L TiCl 4 aqueous solution;

[0029] 2) Preparation of TiCl 4 Mixed solution of aqueous solution and concentrated hydrochloric acid, in which TiCl 4 The volume ratio of aqueous solution to concentrated hydrochloric acid is 4:3;

[0030] 3) Add 15% aqueous ammonia solution dropwise to the above 100ml mixed solution in an ice-water bath, stir while adding dropwise, and stop adding the aqueous ammonia solution when the pH of the reaction system is 6-9;

[0031] 4) Aging for half an hour, filter the precipitate, and wash the chloride ions in the precipitate with deionized water until AgNO is added dropwise to the washed aqueous solution. 3 Until the solution has no white precipitate, the precursor is obtained;

[0032] 5) Add 3 to 5 grams of citric acid to the precursor;

[0033] 6) Calcined at 650°C for 1 hour to obtain anatase nano-TiO 2 , w...

Embodiment 3

[0035] The preparation technology of present embodiment nano-titanium dioxide comprises the following steps:

[0036] 1) Prepare 8mol / L TiCl 4 aqueous solution;

[0037] 2) Preparation of TiCl 4 Mixed solution of aqueous solution and concentrated hydrochloric acid, in which TiCl 4 The volume ratio of aqueous solution to concentrated hydrochloric acid is 5:2;

[0038] 3) Add 12% aqueous ammonia solution dropwise to the above 100ml mixed solution in an ice-water bath, stir while adding dropwise, and stop adding the aqueous ammonia solution when the pH of the reaction system is 6-9;

[0039] 4) Aging for half an hour, filter the precipitate, and wash the chloride ions in the precipitate with deionized water until AgNO is added dropwise to the washed aqueous solution. 3 Until the solution has no white precipitate, the precursor is obtained;

[0040] 5) Add 7.5-9.5 grams of citric acid to the precursor;

[0041] 6) Calcined at 500°C for 2 hours to obtain anatase nano-TiO 2 ,...

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Abstract

This invention relates to a method for preparing nanometer titanium dioxide. The procedures are: preparation of solution of titanium tetrachloride; preparation of mixed solution of above mentioned solution with concentrated hydrochloric acid; preparation of predecessor; adding organic acid into said predecessor; obtaining the inventive nanometer titanium dioxide after calcinations. In this invention, due to the control of H+ content in titanium-containing solution, and the strict control of pH value between 6-9 in the reaction system of predecessor preparation, so the average size of the produced nanometer titanium dioxide is controlled between 20-60mn. This invention has advantages of: simple preparation method, raw materials being available, low cost and with commercialized foreground.

Description

technical field [0001] The invention relates to a preparation method of nano titanium dioxide, which belongs to the technical field of nano material preparation. Background technique [0002] At present, the preparation methods of nano-titanium dioxide can be classified into two categories: physical methods and chemical methods. The physical method is also called pulverization method. This kind of method has high requirements for pulverization equipment, and it is generally difficult to reach the real nanometer level. The industrial preparation of nano-TiO 2 Generally, chemical methods are used, which are divided into gas phase method and liquid phase method. Although the gas phase method is suitable for large-scale production, there are problems such as serious corrosion, large investment, complex equipment and process, for example, CN1245144 and CN1810653 all disclose the preparation of nano-titanium dioxide by the gas phase method. The liquid-phase method adopts the mod...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/053
Inventor 彭子飞孙佳玉
Owner SHANGHAI NORMAL UNIVERSITY
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