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Method for quickly preparing rutile phase nano titanium dioxide

A technology of nano-titanium dioxide and rutile phase, applied in the direction of titanium dioxide, titanium oxide/hydroxide, nanotechnology, etc., can solve the problems of inconvenient large-scale production by microwave radiation method, long hydrolysis reaction time, poor production environment, etc., and achieve easy large-scale production Large-scale industrial production, low cost, and energy-saving effects

Active Publication Date: 2010-04-28
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

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Problems solved by technology

The disadvantage of this method is that the hydrolysis reaction time is longer under strong acid, the hydrochloric acid vapor generated by hydrolysis will cause corrosion to the equipment, and the production environment is poor
Cao Rong et al [Chinese patent, application number is 2007101161058.4] can rapidly synthesize rutile phase nano-titanium dioxide through microwave radiation, but this method requires a large amount of anhydrous organic alcohol and anhydrous organic acid, and the microwave radiation method is not convenient for large-scale production

Method used

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  • Method for quickly preparing rutile phase nano titanium dioxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Weigh a certain amount of sodium hydroxide and titanium tetrachloride, add deionized water respectively to prepare 1.4mol / L sodium hydroxide aqueous solution and 2mol / L titanium tetrachloride aqueous solution, and measure 1.4mol / L hydrogen Put 400mL of sodium oxide solution in a 1000mL three-necked flask, heat up to 80°C, and while stirring, add 126mL of 2mol / L titanium tetrachloride aqueous solution dropwise, after the titanium tetrachloride aqueous solution is added dropwise, continue at 80°C Heat preservation reaction 25min, obtain rutile phase nano-titanium dioxide suspension, with the sodium hydroxide solution of 1.4mol / L, the pH value of rutile phase nano-titanium dioxide suspension is adjusted to pH=8, filter, wash repeatedly until there is no chloride ion (1% in the filtrate). Silver nitrate test), the obtained filter cake is dried and pulverized, and the content of rutile in the obtained nano-titanium dioxide powder is 100%.

Embodiment 2

[0019] Weigh a certain amount of sodium hydroxide and titanium tetrachloride, add deionized water respectively to prepare 6mol / L sodium hydroxide aqueous solution and 3.6mol / L titanium tetrachloride aqueous solution, measure 6mol / L hydroxide Put 300mL of sodium solution in a 1000mL three-necked flask, heat up to 90°C, and while stirring, add 400mL of 3.6mol / L titanium tetrachloride aqueous solution dropwise, after the titanium tetrachloride aqueous solution is added dropwise, continue to keep warm at 90°C Reaction 10min, obtain rutile phase nano-titanium dioxide suspension, add solid sodium carbonate to adjust the pH value of rutile phase nano-titanium dioxide suspension to pH=6, filter, repeatedly wash to no chloride ion (1% silver nitrate test) in the filtrate, will The obtained filter cake is dried and pulverized, and the content of rutile in the obtained nano titanium dioxide powder is 100%.

Embodiment 3

[0021] Weigh a certain amount of sodium hydroxide and titanium tetrachloride, add deionized water respectively to prepare 2mol / L sodium hydroxide aqueous solution and 2.5mol / L titanium tetrachloride aqueous solution, measure 2mol / L hydroxide Put 300mL of sodium solution in a 1000mL three-necked flask, heat up to 100°C, and while stirring, add 300mL of 2.5mol / L titanium tetrachloride aqueous solution dropwise, after the titanium tetrachloride aqueous solution is added dropwise, continue to keep warm at 100°C Reaction 20min, obtain rutile phase nano-titanium dioxide suspension, add solid ammonium carbonate and adjust the pH value of rutile phase nano-titanium dioxide suspension to pH=6.5, filter, repeatedly wash to no chloride ion (1% silver nitrate test) in the filtrate, will The obtained filter cake is dried and pulverized, and the content of rutile in the obtained nano titanium dioxide powder is 100%.

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Abstract

The invention discloses a method for quickly preparing rutile phase nano titanium dioxide, comprising: first, preparing 1.4-6.0mol / L of sodium hydroxide water solution and 1-3.6mol / L of titanium tetrachloride water solution; heating the sodium hydroxide water solution to be 80-100 DEG C, and adding the titanium tetrachloride water solution into the sodium hydroxide water solution while stirring; after the titanium tetrachloride water solution is completely added, continuously carrying out heat preservation reaction for 10-25min, and obtaining rutile phase nano titanium dioxide suspending liquid; and finally, using alkali to adjust the pH of the suspending liquid to be 6-8, filtering and washing to remove foreign ions, drying and grinding the obtained filter cake, and obtaining the rutile phase nano titanium dioxide powder. The method can be used for quickly synthesizing the nano titanium dioxide with the rutile content of 100% under the mild condition, avoids the steps of high temperature calcination adopted by the traditional method, saves the energy, and has the characteristics of short process flow, low cost, convenient operation and easy realization of large-scale industrialized production.

Description

technical field [0001] The invention relates to a method for rapidly preparing rutile-phase nano-titanium dioxide, which belongs to the fields of nanometer materials and inorganic chemical industry. Background technique [0002] 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. Usually, the preparation of rutile phase nano-titanium dioxide adopts the liquid phase method, which is to prepare the titanium dioxide precursor with an amorphous structure first, and then convert it into an anatase structure by heat treatment at 300-500 °C, and finally undergo a high temperature above 600 °C. After calcining and phase transformation, nano-titanium dioxide with rutile structure can be obtained. The high-temperature calcination proce...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/053B82B3/00
Inventor 吴凤芹姚超成庆堂徐斌海徐新前魏科年
Owner 江苏河海纳米科技股份有限公司
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