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

A technology of double-effect crystal seed and metatitanic acid, which is applied in the direction of chemical instruments and methods, titanium dioxide, titanium compounds, etc., can solve the problems such as inability to perform hydrolysis, and achieve the effect of shortening bleaching time, low cost, and appropriate ratio

Active Publication Date: 2013-07-31
SICHUAN LOMON TITANIUM IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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, and 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 temperatur...

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 temperature of the material 2 The solution is dripped into the washing solution 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 ...

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 solution 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

Provided is a method for preparing a high-activity dual-functional seed crystal with metatitanic acid, comprising reacting a metatitanic acid having a total iron concentration of = 50 ppm and a concentration of 300 - 400 g / L (expressed as TiO2) with concentrated sulfuric acid at a mass ratio of 1:4 - 1:5, and boiling the mixture to yield a clear solution of titanium sulfate; cooling the clear solution of titanium sulfate to a temperature below 65°C, then diluting same to a concentration of 120 - 200 g / L (expressed as TiO2) and filtering; adding the filtrate into a base solution for neutralization, to a pH of 7.5 - 9.0, so as to obtain a suspension containing ortho-titanic acid; filtering the suspension of ortho-titanic acid and washing until there are no sulfate ions, beating, washing a second time, and beating; adding concentrated hydrochloric acid and hydrofluoric acid into the slurry, raising the temperature for maturing, to obtain a colloid seed crystal with slight blue opalescence, and quenching same to < 50°C. The seed crystal produced by the present method has a proper ratio of non-rutile-promoted and rutile-promoted seed crystals, the dual functions of hydrolysis seed crystal and calcination seed crystal, so that no additional production of calcination seed crystal is needed for the production of titanium white, thereby reducing the procedures for bleaching and calcinating seed crystal, shortening the duration of bleaching and improving the efficiency of rinsing.

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