Method for preparing rutile nano titanium dioxide

A nano-titanium dioxide, rutile phase technology, applied in the direction of titanium dioxide, titanium oxide/hydroxide, etc., can solve the problems of small particle size, long sedimentation time, hard agglomeration, etc., to prevent the growth of crystal grains, avoid agglomeration and sticking. The effect of easy industrial production

Inactive Publication Date: 2006-11-08
SUZHOU UNIV
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Problems solved by technology

[0004] At present, there are many methods for preparing nano-titanium dioxide, but most of them are used to produce amorphous or sharp-type titanium dioxide. There are not many high-purity rutile-phase nano-titanium dioxide. The transformation requires high temperature, so it is not easy to produce small particle size rutile phase titanium dioxide
The preparation methods of nano-rutile phase titanium dioxide are generally divided into gas phase method and liquid phase method. The typical gas phase method is the chloride oxidation method, which has high powder purity and small particle size, but requires high technical equipment, high energy consumption and high cost.
The typical liquid-phase method is the sol-gel method. This method generally uses titanium alcohol ester as the raw material, which has high cost and long process flow. Hard agglomeration is easy to occur during the powder post-treatment process, and it is not easy to obtain small particle size. The rutile phase nano-titanium dioxide, and in the sol-gel synthesis process, there are many factors that lead to the transformation of the titanium dioxide crystal form, and the nano-titanium dioxide with multiple crystal forms is often obtained.
The direct precipitation method of inorganic titanium salt hydrolysis is the easiest and most economical method, but due to the slight changes in external conditions (such as concentration, temperature, pH value, etc.) It is carried out at high temperature, so generally only micron-sized rutile phase nano-titanium dioxide powder can be obtained
Although the hydrothermal method can directly generate rutile nano-titanium dioxide, it requires high equipment, complicated operation and high cost
In the Chinese patent "Method for preparing rutile titanium dioxide nanocrystals at room temperature" with the publication number CN1248550A, a method for preparing rutile titanium dioxide nanocrystals with titanium tetrachloride as the main raw material is prepared by inorganic acid hydrolysis and vacuum drying. method, because the method has stricter requirements on the control of process conditions, especially the concentration of titanium tetrachloride has a greater influence on the hydrolysis rate, and the required precipitation time is longer, therefore, the yield is low, which is not conducive to industrial production

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  • Method for preparing rutile nano titanium dioxide
  • Method for preparing rutile nano titanium dioxide
  • Method for preparing rutile nano titanium dioxide

Examples

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Effect test

Embodiment 1

[0023] Add 2g of cyclodextrin to 100ml of ethanol / water mixed solvent containing 0.8g / L lecithin, and fully disperse it under the action of ultrasonic waves; then use concentrated hydrochloric acid to adjust the pH value of the dispersion to 1.1; the concentration is 0.5mol / L of titanium tetrachloride aqueous solution is slowly added to the above dispersion liquid, under the action of ultrasonic waves with a frequency of 30KHz and a power of 250W, drip ammonia water with a concentration of 30%, and react at room temperature for 1.5 hours; after standing for 2 hours, carry out Filtrate, wash, and calcinate the obtained filter cake at 700° C. for 1 hour to obtain milky white powdery rutile nano-titanium dioxide with a particle size of 9.5 nm.

[0024] See attached figure 1 , from the analysis results of the laser particle size analyzer, it can be seen that the rutile phase nano-titanium dioxide powder prepared by the preparation method described in Example 1 has an average part...

Embodiment 2

[0028] Add 2g of modified lignosulfonate to 150ml of ethanol / cyclohexane / water mixed solvent containing EDTA 2.0g / L, fully disperse the carrier under the action of ultrasonic waves, and then adjust the dispersion with concentrated hydrochloric acid The pH value of the solution is 1.5, and the butyl titanate aqueous solution with a concentration of 1.5mol / L is slowly added to the above dispersion liquid, and under the action of ultrasonic waves with a frequency of 30KHz and a power of 300W, ammonia water with a concentration of 30% is added dropwise, and other The steps are the same as in Example 1 to obtain 19.5nm milky white powdery rutile nano-titanium dioxide.

Embodiment 3

[0030] Add 1g of carbon powder and 1g of starch to 150ml of ethanol / cyclohexane / water mixed solvent containing citric acid 2.0g / L, fully disperse it under the action of ultrasonic waves, and then use concentrated nitric acid to adjust the pH value of the dispersion to 1.0 , slowly add titanium tetrachloride aqueous solution with a concentration of 0.5 mol / L to the above dispersion liquid, under the action of ultrasonic waves with a frequency of 30KHz and a power of 250W, add ammonia water with a concentration of 30% dropwise, and react at room temperature for 1.5 hours , let stand for 2 hours, then filter and wash, and calcinate the filter cake at 700°C for 1 hour to obtain 24.5nm milky white powdery rutile nano-titanium dioxide.

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Abstract

The invention relates to a preparation method of rutile phase nano-titanium dioxide powder. The technical scheme adopted is: adding a carrier to a solvent system containing a dispersant, fully dispersing the carrier under the action of ultrasonic waves; adjusting the pH value of the dispersion to 1.0 ~2.0; Slowly add the titanium compound aqueous solution with a solution concentration of 0.5~2.0mol / L to the above dispersion liquid, slowly add lye under the action of ultrasonic waves, and react for 1~3 hours; after standing for 2~3 hours, carry out Filtration and washing treatment, the obtained filter cake is directly calcined at a temperature of 500-900° C. until the carrier is completely removed, and a loose rutile nano-titanium dioxide powder is obtained. Since the reaction is carried out at normal temperature and pressure, the obtained product is powder without grinding, so it has controllable particle size, narrow distribution, high purity, no agglomeration, simple process, short process, low cost, and easy large-scale characteristics of production.

Description

technical field [0001] The invention relates to a preparation method of rutile phase nano-titanium dioxide powder, which belongs to the field of inorganic material preparation. Background technique [0002] Nano-titanium dioxide is a widely used nanomaterial, which has the unique small size effect, quantum size effect, surface effect and macroscopic quantum tunneling effect of nanoparticles (1-100nm). Its extremely strong ultraviolet shielding ability can make it used as an ultraviolet shielding agent in cosmetics and textile fields; its strong photooxidative ability, chemical stability, and non-toxicity make it expected to become an excellent photocatalytic material for purifying air, Deodorization, antifouling, antibacterial; its good optical properties can make paints and paints produce the effect of different color effects, greatly improving the quality of paints and paints; in addition, it can also be used in latex paints to improve the color ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G23/047
Inventor 郑敏
Owner SUZHOU UNIV
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