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Method for preparing rutile type calcination crystal seed

A calcined seed crystal, rutile type technology, applied in the direction of titanium dioxide, titanium oxide/hydroxide, etc., can solve the problems of low rutile conversion rate, high oil absorption of the first product, low activity of rutile type calcined seed crystal, etc. The effect of high redstone rate

Inactive Publication Date: 2004-12-29
攀枝花钢铁有限责任公司钢铁研究院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But use this method to prepare rutile calcined seed crystals with low activity, low rutile conversion rate of the seeds, high oil absorption of the initial product, and because zinc salt or its oxide is often added as an auxiliary accelerator during salt treatment, making anatase TiO 2 It is completely transformed into a rutile structure, and the introduction of zinc increases the average particle size of titanium dioxide particles

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0009] Beat metatitanic acid to 250g / l (as TiO 2 meter), get 400ml and pour it into a 1000ml beaker, add 245ml of vitriol oil while stirring, and boil under normal pressure to make a titanium sulfate clear solution without suspended solids. After cooling to 40°C-45°C, add 540ml of deionized water to dilute while stirring. Take 200ml of this titanium solution and pour it into a 1000ml beaker, slowly add 10% NaOH solution dropwise under stirring to make orthotitanic acid, control the neutralization temperature at 50°C-65°C, when the pH value of the slurry is 7.0-7.5, Stop dripping lye. Then filter and wash with deionized water until the washings are free of SO 4 -2 until (drop 10% barium chloride solution into the washing solution without white precipitation). Then the filter cake was beaten to 100g / l (as TiO 2 meter), adding concentrated hydrochloric acid, in which TiO 2 : HCl=1:0.50 (mass ratio), after 45min of constant temperature stirring reaction at 85 ℃-110 ℃, immedi...

Embodiment 2

[0011] Beat the metatitanic acid to 280g / l, take 357ml and pour it into a 1000ml beaker, add 272ml of concentrated sulfuric acid while stirring, and boil under normal pressure to make a titanium sulfate clear solution without suspended matter. After cooling to 40°C-45°C, add 400ml of deionized water to dilute while stirring. Take 300ml of 15% NaOH solution and pour it into a 1000ml beaker, slowly add the titanium solution dropwise under stirring to make orthotitanic acid, control the neutralization temperature at 50°C-60°C, when the pH value of the slurry is 7.0-7.5 , stop dropping the titanium solution. Then filter and wash with deionized water until the washings are free of SO 4 -2 until. Beat the filter cake to 120g / l, add concentrated hydrochloric acid, in which TiO 2 : HCl = 1: 0.55, at 85°C-110°C constant temperature stirring reaction for 40min, immediately add 100ml of deionized water to quench, and then slowly cool down to room temperature to prepare highly active ...

Embodiment 3

[0013] Beat the metatitanic acid to 320g / l, take 313ml and pour it into a 1000ml beaker, add 255ml of concentrated sulfuric acid while stirring, and boil under normal pressure to make a titanium sulfate clear solution without suspended matter. After cooling to 40°C-45°C, add 450ml of deionized water to dilute while stirring. Take 200ml of this titanium solution and pour it into a 1000ml beaker, slowly add 20% NH 4 The OH solution is made into orthotitanic acid, and the neutralization temperature is controlled at 45°C-65°C. When the pH value of the slurry is 7.0-7.5, stop adding alkali solution dropwise. Then filter and wash with deionized water until the washings are free of SO 4 -2 until. Beat the filter cake to 140g / l, add concentrated hydrochloric acid, in which TiO 2 : HCl=1:0.45, after stirring at 85°C-110°C for 50min at a constant temperature, immediately add 60ml of deionized water to quench, and then slowly cool down to room temperature to obtain high-activity ruti...

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PUM

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Abstract

The rutile type calcining crystal seed preparation process includes the following steps: boiling metatitanic acid and concentrated sulfuric acid for reaction to prepare titanium sulfate solution; cooling, diluting and adding alkali solution to neutralize and obtain titanic acid; filtering, washing, pulping, adding concentration hydrochloric acid and heating to reaction, and rapid cooling to rutile type calcining crystal seed. The rystal seed has high rutile content over 99 %. In the process, the salt treatment has no zinc salt and other auxiliary promoter are used. The crystal seed may be used in obtaining rutile type TiO2 powder with particle size of several nanometer and oil absorption lower than 19 %.

Description

technical field [0001] The invention relates to a preparation method of a highly active rutile calcined seed crystal. Background technique [0002] Rutile calcined seeds are widely used as TiO in the production of rutile pigment titanium dioxide by sulfuric acid process 2 Rutile accelerator, can also be used to produce rutile nano-TiO 2 Functional powder materials. The preparation method of the existing rutile calcined seed crystal is usually to mix metatitanic acid and sodium hydroxide in a certain proportion, then boil for about two hours to generate sodium orthotitanate, and then hydrolyze the sodium orthotitanate to form orthotitanic acid, and then React with a certain amount of hydrochloric acid to obtain rutile calcined seed crystals. But use this method to prepare rutile calcined seed crystals with low activity, low rutile conversion rate of the seeds, high oil absorption of the initial product, and because zinc salt or its oxide is often added as an auxiliary acce...

Claims

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Application Information

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IPC IPC(8): C01G23/053
Inventor 许述林王兰武
Owner 攀枝花钢铁有限责任公司钢铁研究院