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Process for preparing rutile-type nano TiO2 by meta titanic acid

A technology of rutile type and metatitanic acid, which is applied in the direction of titanium dioxide, titanium oxide/hydroxide, etc.

Inactive Publication Date: 2005-11-23
JIANGSU UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For example, patent 200510038935.X, which also uses carboxyl or hydroxyl-containing organic compounds as modifiers to prepare ultra-fine rutile nano-titanium dioxide, but uses titanium tetrachloride as raw material. After searching, there is currently no carboxyl or hydroxyl-containing modification. Preparation of Rutile Nano-TiO from Metatitanic Acid 2 reports and patent literature

Method used

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  • Process for preparing rutile-type nano TiO2 by meta titanic acid
  • Process for preparing rutile-type nano TiO2 by meta titanic acid
  • Process for preparing rutile-type nano TiO2 by meta titanic acid

Examples

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example 1

[0022] Weigh 30g of metatitanic acid as shown in R1, add 30ml of distilled water to make a suspension, add 30ml of concentrated sulfuric acid to it, dissolve it in a water bath at 80°C, and then add Na 2 CO 3 Aqueous solution, suction filtration when pH=0.07, Na added dropwise to the filtrate 2 CO 3 aqueous solution until the pH equals 9.26. After adding the lye, while stirring, add 0.7870g of succinic acid. Aging at 15°C for 4h. The precipitate was washed with distilled water until the conductivity of the filtrate was 18 mS / m, and then the filter cake was obtained by suction filtration. Weighed 21.7158 g of the filter cake, and added concentrated hydrochloric acid (HCl, 38%) and distilled water until the total volume was 100 ml and the pH was 0.39. Then aged for 4 hours at room temperature. Put the aged suspension into a polytetrafluoroethylene-lined stainless steel hydrolysis kettle, and react at 100°C for 10 hours to obtain rutile nano-titanium dioxide. After TEM anal...

example 2

[0024] As shown in R2, weigh 30g of metatitanic acid, add 60ml of distilled water to make a suspension, add 35ml of concentrated sulfuric acid to it, dissolve in a water bath at 100°C, and then add Na 2 CO 3 aqueous solution, to pH=-0.07, carry out suction filtration, then add Na to the filtrate dropwise 2 CO 3 aqueous solution until the pH equals 9.14. After adding the lye, while stirring, add 2.3009g of benzoic acid. Aged at 30°C for 1h. Wash the precipitate with distilled water until the conductivity of the filtrate is 15mS / m, then suction filter to obtain a filter cake, weigh 24.4867g of the filter cake, add concentrated hydrochloric acid (HCl, 38%) and distilled water until the total volume is 100ml, and the pH is 0.39. Then aged for 3 hours at room temperature. Put the aged suspension into a polytetrafluoroethylene-lined stainless steel hydrolysis kettle, and react at 120°C for 11 hours to obtain rutile nano-titanium dioxide. After TEM analysis, the particle shape ...

example 3

[0026] As shown in R3, weigh 30g of metatitanic acid, add 90ml of distilled water to make a suspension, add 72ml of concentrated sulfuric acid to it, dissolve in a water bath at 80°C, and then add Na 2 CO 3 aqueous solution, to pH=0.07, carry out suction filtration, then add Na to the filtrate dropwise 2 CO 3 aqueous solution until the pH equals 9.24. After adding the lye, while stirring, add 0.5ml of formic acid. Aging at 60°C for 2h. Wash the precipitate with distilled water until the conductivity of the filtrate is 18mS / m., then suction filter to obtain a filter cake, weigh 18.9906g of the filter cake, add concentrated hydrochloric acid (HCl, 38%) and distilled water until the total volume is 100ml, and the pH is 0.40. Then aged for 2 hours at room temperature. Put the aged suspension into a polytetrafluoroethylene-lined stainless steel hydrolysis kettle, and react at 140°C for 12 hours to obtain rutile nano-titanium dioxide. After TEM analysis, the particle shape of ...

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Abstract

The invention discloses a process for preparing rutile-type nano TiO2 which comprises, preparing metatitanic acid solution by the proportion of water : metatitanic acid = 1-3 : 1, charging concentrated sulfuric acid by the mol ratio of H2SO4 : Ti = 4-10 : 1, heating for dissolution, charging Na2CO3 solution drop by drop, till pH=0, filtering, charging Na2CO3 solution into the filter liquor, till pH is over 7, agitating and charging organic modification agent containing carboxyl or hydroxyl, the mol ratio of OH and metatitanic acid in the organic modification agent is between 1 / 7-1 / 12, ageing 0.5-4h at 10-95 deg. C, washing precipitate with distilled water until the electrical conductivity of the filter liquor is smaller than 20ms / m, filtering to obtain filter cake, charging dense hydrochloric acid and distilled water, making the pH of the solution below 0.8, ageing 1-4 h at room temperature, charging the aged suspending liquid into hydrolysis still, reacting 10-18h at 100-240 deg. C.

Description

technical field [0001] The invention relates to a method for preparing rutile nano-titanium dioxide, in particular to a method for preparing rutile nano-titanium dioxide by using metatitanic acid as a raw material, heating and dissolving with concentrated sulfuric acid, adding organic compounds containing carboxyl or hydroxyl groups, and hydrothermal synthesis. Background technique [0002] Due to its unique properties, nano-titanium dioxide has been widely used, such as white pigments, ultraviolet shielding agents, photocatalysts, photoelectric cell materials, catalysts, etc. There are many methods for synthesizing nano-titanium dioxide, such as liquid phase precipitation calcination method, sol-gel method, alkoxide hydrolysis method, microemulsion method, gas phase method, and hydrothermal synthesis method. These methods usually use titanium alkoxide, titanium tetrachloride and titanium sulfate as starting reactants. Among them, the precipitation after the reaction of the...

Claims

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Application Information

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IPC IPC(8): C01G23/047
Inventor 殷恒波蒋银花姜廷顺谢吉民姚恒平奉辉杨晋安
Owner JIANGSU UNIV
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