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Method for preparing high-activity double-effect seed crystals from metatitanic acid

A double-effect seed crystal, metatitanic acid technology, applied in chemical instruments and methods, titanium dioxide, titanium compounds, etc., can solve problems such as inability to perform hydrolysis, and achieve shortened bleaching time, high seed crystal activity, and improved efficiency. Effect

Active Publication Date: 2012-03-28
SICHUAN LOMON TITANIUM IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Patent CN1415548 uses 4-7%SnO 2 doped TiO 2 Cultivate double-effect seed crystals, add them during hydrolysis, and combine K salt and Zn salt with calcination to realize rutile conversion at a lower temperature. The raw material is TiCl 4 , Ti(SO 4 ) 2 , Ti(NO 3)4 , SnCl 2 , needs to be outsourced, easily restricted by upstream companies
[0004] CN1557721 uses metatitanic acid and concentrated sulfuric acid as raw materials to prepare titanium sulfate, and then adds lye to its diluent, pH=6.0~7.5, to obtain orthotitanic acid, add hydrochloric acid after washing, 80~110°C, 30~90min, A calcined seed crystal with a rutile conversion rate of not less than 99% is obtained, which can only be used as a calcined seed crystal and cannot perform hydrolysis

Method used

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  • Method for preparing high-activity double-effect seed crystals from metatitanic acid
  • Method for preparing high-activity double-effect seed crystals from metatitanic acid
  • Method for preparing high-activity double-effect seed crystals from metatitanic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Beat the rinsed metatitanic acid (Fe≤50ppm) into TiO 2 The concentration is 300g / L, take 1000ml and pour it into a 3000ml flask, add 665ml of concentrated sulfuric acid while stirring, boil under normal pressure to make titanium sulfate clear liquid, after the titanium sulfate clear liquid is cooled to 60°C, add distilled water while stirring ( It can also be diluted with desalted water) to 120g / L (using TiO 2 meter), filter. Slowly add the filtrate to 150g / L sodium carbonate solution, control the temperature of the material 2 The solution is dripped into the washing solution without white precipitate). Beat the filter cake to 50g / L (as TiO 2 meter), then press TiO 2 : HCl 0.3 and TiO 2 Concentrated hydrochloric acid and hydrofluoric acid are added at a mass ratio of HF of 0.03, wherein the order of addition of concentrated hydrochloric acid and hydrofluoric acid is not limited. After the mixed acid is added, it is stirred for 30 minutes, and then the temperature of...

Embodiment 2

[0023] Beat the rinsed metatitanic acid (Fe≤50ppm) into TiO 2 The concentration is 350g / L, take 1000ml and pour it into a 3000ml flask, add 776ml of concentrated sulfuric acid while stirring, boil under normal pressure to make a titanium sulfate solution, cool to 30°C, add desalinated water while stirring to dilute to 160g / L (with TiO 2 meter), filter. Slowly add it to 200g / L sodium carbonate solution, control the material temperature 2 The solution is dripped into the washing liquid without white precipitate). Beat the filter cake to 80g / L (as TiO 2 meter), adding concentrated hydrochloric acid and hydrofluoric acid, in which TiO 2 The mass ratio to HCl is 0.45, TiO 2 The mass ratio to HF is 0.03. After stirring for 30 minutes, heat up to 78°C and keep it warm for 6 minutes to obtain a colloidal seed crystal with a slight blue opalescence. Add 1 / 5 times the volume of the colloidal seed crystal in desalted water and quench to - ≤2g / L, beating is 80 g / L (based on TiO 2 co...

Embodiment 3

[0025] Beat the rinsed metatitanic acid (Fe≤50ppm) into TiO 2 The concentration is 450g / L, take 1000ml and pour it into a 3000ml flask, add 998ml of concentrated sulfuric acid while stirring, boil under normal pressure to make a titanium sulfate solution, cool to 45°C, add distilled water to dilute to 200g / L while stirring, filter. Slowly add the filtrate to 175g / L sodium carbonate solution, control the temperature of the material 2 The solution is dripped into the washing liquid without white precipitate). Beat the filter cake to 100g / L, add concentrated hydrochloric acid, in which TiO 2 :HCl=0.6 (mass ratio), TiO 2 : HF=0.04 (mass ratio), after stirring for 30 minutes, heat up to 80°C and hold for 4 minutes to obtain a colloidal seed crystal with a slight blue opalescence, add 1 / 5 times the volume of the colloidal seed crystal in desalted water to quench To - ≤2g / L, beating to 100 g / L (based on TiO 2 count), get crystal seeds.

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Abstract

The invention discloses a method for preparing high-activity double-effect seed crystals from an intermediate product, namely metatitanic acid, of titanium dioxide. The method comprises the following steps of: with metatitanic acid as a raw material, preparing clear titanium sulfate liquid, cooling the clear titanium sulfate liquid, adding a diluent of the clear titanium sulfate liquid to alkaline liquor, controlling pH value to 7.5-9.0, filtering and washing the obtained product, carrying out secondary washing on the washed product, carrying out acid dissolving on hydrofluoric acid and hydrochloric acid for short time under the lower temperature to obtain the high-activity double-effect seed crystals with hydrolyzed seed crystal performance and calcined seed crystal performance. According to the invention, the required titanium source is from the intermediate product produced from the titanium dioxide powder, therefore the method has low cost and production stability; in seed crystals, non-rutile promoted seed crystals and rutile promoted seed crystals are appropriate in proportion and have dual effects of hydrolyzed seed crystals and calcimined seed crystals; when the method is used for titanium dioxide production, calcined seed crystals are unnecessary to be additionally produced, the working procedure of adding the calcined seed crystals in the bleaching process is reduced, the bleaching time is shortened, and the rinsing efficiency is improved at the same time. The seed crystals prepared by using the method disclosed by the invention have high activity, excellent performance and capability of meeting hydrolyzing and calcining requirements just by adding 2 % of seed crystals.

Description

technical field [0001] The invention relates to the technical field of titanium dioxide preparation, in particular to a preparation method with hydrolysis and calcination double-effect seed crystals in the production of titanium dioxide prepared from metatitanic acid. Background technique [0002] In the production of titanium dioxide, the seeds of the hydrolysis method with external seeds need to be prepared separately. There are two types of hydrolysis seeds and calcined seeds. The hydrolysis seeds are added during hydrolysis, and the general size is below 10nm. Calcined seeds are added during bleaching. The general size is 80~120nm. The two have different structures and different roles, so the preparation process is also different. There are rutile-promoted and non-rutile-promoted hydrolyzed seeds, both of which are different and related. The connection is that both are a kind of colloid, which can be used as hydrolysis seed crystals to hydrolyze concentrated titanium s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/053
CPCC01G23/0538C01G23/0532C01G23/0534C01P2006/80
Inventor 林发蓉代堂军蔡平雄邓伯松朱全芳
Owner SICHUAN LOMON TITANIUM IND CO LTD
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