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Preparation method of mixed crystal type nanometer titanium dioxide

A nano-titanium dioxide, mixed crystal technology, applied in the direction of titanium dioxide, nanostructure manufacturing, titanium oxide/hydroxide, etc., to achieve the effects of less pollution, low cost and short process flow

Active Publication Date: 2011-06-22
江苏河海纳米科技股份有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The high-temperature calcination process will cause the rapid growth, agglomeration, and even sintering of nano-titanium dioxide particles. As a result, the photocatalytic and photoelectric conversion efficiency of nano-titanium dioxide will be greatly reduced.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Weigh 100 grams of metatitanic acid (solid content is 32%) through repeated washing to remove sulfate radicals, add 60 g of deionized water to make a metatitanic acid slurry with a mass percentage content of 20%, and transfer the slurry to a container In a 2000mL three-necked flask with a condenser. While stirring, 320 g of an aqueous solution of titanium tetrachloride with a mass percent content of 10% was added to the metatitanic acid slurry. Open the cooling water valve and feed the cooling water into the condenser. The temperature of the reaction solution in the three-necked flask was raised to 80°C. After reaching the reaction temperature, the stirring was continued and the heat preservation reaction was continued for 600 minutes. At the same time, the condenser recondensed the water evaporated from the three-necked flask and recovered it into the reaction system. After the reaction finished, the pH value of the system was adjusted to pH=6 with 2.0mol / L sodium hyd...

Embodiment 2

[0020] Weigh 100 grams of metatitanic acid (solid content is 32%) through repeated washing to remove sulfate radicals, add 220 g of deionized water to make a metatitanic acid slurry with a mass percentage content of 10%, and transfer the slurry to a container In a 5000mL three-necked flask with a condenser. While stirring, 640 g of a 50% by mass titanium tetrachloride aqueous solution was added to the metatitanic acid slurry. Open the cooling water valve and feed the cooling water into the condenser. The temperature of the reaction solution in the three-necked flask was raised to 100°C. After reaching the reaction temperature, the stirring was continued and the reaction was heated and kept for 60 minutes. At the same time, the condenser recondensed the water evaporated from the three-necked flask and recovered it into the reaction system. After the reaction finishes, adjust the pH value of the system to pH=8 with 2mol / L potassium hydroxide aqueous solution, filter, and repeat...

Embodiment 3

[0022] Weigh 100 grams of metatitanic acid (solid content is 32%) through repeated washing to remove sulfate radicals, add 100 g of deionized water to form a metatitanic acid slurry with a mass percentage of 16%, and transfer the slurry to a container In a 3000mL three-necked flask with a condenser. While stirring, 640 g of an aqueous titanium tetrachloride solution with a mass percent content of 25% was added to the metatitanic acid slurry. Open the cooling water valve and feed the cooling water into the condenser. The temperature of the reaction solution in the three-necked flask was raised to 90°C. After reaching the reaction temperature, the stirring was continued and the heat preservation reaction was continued for 300 minutes. At the same time, the condenser recondensed the water evaporated from the three-necked flask and recovered it into the reaction system. After the reaction finishes, adjust the pH value of the system to pH=6.5 with 2mol / L ammonia solution, filter, ...

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Abstract

The invention discloses a preparation method of a mixed crystal type nanometer titanium dioxide. The method comprises the following steps of adding the deionized water in the metatitanic acid which is washed repeatedly for removing the sulfate radical therein to prepare a metatitanic acid slurry of which the mass percent is 10 to 12, adding titanium tetrachloride aqueous solution of which the mass percent is10 to 50 in the metatitanic acid slurry in the stirring process so as to obtain a precursor suspension, heating the precursor suspension to be 80 to 100 DEG C, preserving the temperature, reacting 60 to 600 minutes to finally obtain the mixed crystal type nanometer titanium dioxide suspension, regulating the pH of the mixed crystal type nanometer titanium dioxide suspension to be 6 to 8 with alkali, filtering, repeatedly washing and removing the impurity ions, drying and crushing the obtained filter cake to prepare the mixed crystal type nanometer titanium dioxide powder. The preparation method of the invention prepares the mixed crystal type nanometer titanium dioxide in a mild condition, which avoids the calcining step at high temperature, saves energy. The metatitanic acid and titanium tetrachloride are cheap and easily obtainable, the processes are short, and the operations are convenient, thereby being applicable to the large-scale industrialized production.

Description

technical field [0001] The invention relates to a preparation method of mixed crystal nano-titanium dioxide, which belongs to the field of nanometer materials and inorganic chemical industry. Background technique [0002] Titanium dioxide has three crystal forms: anatase, rutile, and brookite. The former two are tetragonal, and the latter is orthorhombic. Among them, anatase and rutile are the most useful and researched two types of crystals. type. Rutile phase nano titanium dioxide has the advantages of stable properties, high refractive index and relatively low photocatalytic activity, thus becoming an ideal inorganic ultraviolet shielding agent, widely used in sunscreen cosmetics, chemical fibers, plastics, rubber and coatings and other fields. Due to its strong photocatalysis and photoelectric conversion efficiency, anatase phase nano-dioxide is used in the fields of pollutant degradation, antibacterial and sterilization, cyanobacteria treatment, self-cleaning glass an...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G23/053B82B3/00
Inventor 姚超徐斌海成庆堂吴凤芹徐新前马江权王茂华
Owner 江苏河海纳米科技股份有限公司
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