Producing method of low-fluorine high-purity tantalic oxide

The technology of tantalum pentoxide and tantalum hydroxide is applied in the field of preparation of tantalum metal oxide, which can solve the problems of high fluorine content, easy sintering in the furnace, uneven temperature in the furnace, etc. good consistency

Inactive Publication Date: 2009-10-28
ZHAOQING DUOLUSN RARE METAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Disadvantages of the traditional calcination method: 1. Due to the fast heating rate, the temperature in the furnace is uneven, and the consistency of the produced products is not very good; 2. The fluorine content is too high; 3. Due to the local temperature is too high, the furnace wire is easy to burn out , the furnace is easy to sinter

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 1. Use the liquid-liquid extraction method to prepare high-purity tantalum liquid from impure tantalum liquid materials. First, put the tantalum liquid into the neutralization sedimentation tank, and pass NH3 gas under stirring to make the solution PH=8-9. Generate Ta(OH) 5 Precipitate, then pass it through a filter press or vacuum filter. Then put the tantalum hydroxide back into the decomposition tank, add hydrofluoric acid and sulfuric acid to dissolve, and perform secondary extraction with organic matter to obtain high-purity tantalum liquid;

[0029] 2. Neutralize the high-purity tantalum liquid with ammonia to pH>9 to generate tantalum hydroxide;

[0030] 3. Then add Ta(OH) 5 Transfer to a vacuum filtration washing tank, wash and filter with pure water until the filtrate contains F<0.02g / L, and transfer to a drying oven to dry after passing the washing;

[0031] 4. Calcining the dried high-purity tantalum hydroxide in sections according to the following steps: ...

Embodiment 2

[0038] 1. Use the liquid-liquid extraction method to prepare high-purity tantalum liquid from impure tantalum liquid materials. First, put the tantalum liquid into the neutralization sedimentation tank, and pass NH3 gas under stirring to make the solution PH=8-9. Generate Ta(OH) 5 Precipitate, then pass it through a filter press or vacuum filter. Then put the tantalum hydroxide back into the decomposition tank, add hydrofluoric acid and sulfuric acid to dissolve, and perform secondary extraction with organic matter to obtain high-purity tantalum liquid;

[0039] 2. Neutralize the high-purity tantalum liquid with ammonia to pH>9 to generate tantalum hydroxide;

[0040] 3. Then add Ta(OH) 5 Transfer to a vacuum filtration washing tank, wash and filter with pure water until the filtrate contains F<0.02g / L, and transfer to a drying oven to dry after passing the washing;

[0041] 4. Calcining the dried high-purity tantalum hydroxide in sections according to the following steps: ...

Embodiment 3

[0048] 1. Use the liquid-liquid extraction method to prepare high-purity tantalum liquid from impure tantalum liquid materials. First, put the tantalum liquid into the neutralization sedimentation tank, and pass NH3 gas under stirring to make the solution PH=8-9. Generate Ta(OH) 5 Precipitate, then pass it through a filter press or vacuum filter. Then put the tantalum hydroxide back into the decomposition tank, add hydrofluoric acid and sulfuric acid to dissolve, and perform secondary extraction with organic matter to obtain high-purity tantalum liquid;

[0049] 2. Neutralize the high-purity tantalum liquid with ammonia to pH>9 to generate tantalum hydroxide;

[0050] 3. Then add Ta(OH) 5 Transfer to a vacuum filtration washing tank, wash and filter with pure water until the filtrate contains F<0.02g / L, and transfer to a drying oven to dry after passing the washing;

[0051] 4. Calcining the dried high-purity tantalum hydroxide in sections according to the following steps: ...

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PUM

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Abstract

The invention provides a preparation method of low-fluorine high-purity tantalic oxide, which comprises the following steps: preparing high-purity tantalic liquid from impure tantalic liquid materials by adopting a liquid-liquid extraction method; neutralizing the high-purity tantalic liquid by purified ammonia to obtain high-purity tantalum hydroxide which is then washed, filtered, dried; sectionally calcining the high-purity tantalum hydroxide according to the following steps: heating to 180-230 DEG C, and carrying out heat preservation for 2-3 hours; heating to 480-530 DEG C, and carrying out heat preservation for 4-6 hours; heating to 620-680 DEG C, and carrying out heat preservation for 2-3 hours; heating to 790-840 DEG C, and carrying out heat preservation for 3-5 hours; reducing temperature to 180-230 DEG C, and then discharging the high-purity tantalum hydroxide from a furnace and screening to obtain the high-purity tantalic oxide. The invention has the advantages that the prepared high-purity tantalic oxide product has good consistency and evenness, low fluorine content, less ignition loss and protection function to a furnace hearth, and the service life of a roasting hearth can be prolonged.

Description

technical field [0001] The invention relates to a preparation method of tantalum metal oxide, in particular to a preparation method of high-purity tantalum pentoxide. Background technique [0002] At present, the traditional high-purity tantalum pentoxide is produced by liquid-liquid extraction and separation of tantalum and niobium. First, the tantalum liquid is poured into the neutralization precipitation tank, and NH3 gas is introduced under stirring to make the solution pH =8-9, generate Ta(OH) 5 Precipitate, then pass it through a filter press or vacuum filter. Then put the tantalum hydroxide back into the decomposition tank, add hydrofluoric acid and sulfuric acid to dissolve, and carry out secondary extraction with organic matter to obtain high-purity tantalum liquid, and the high-purity tantalum liquid is neutralized with purified ammonia water to obtain high-purity tantalum hydroxide. High-purity tantalum hydroxide is calcined, cooled and sieved in a muffle furnac...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G35/00
Inventor 曹七林伍尊中李德阳朱建东
Owner ZHAOQING DUOLUSN RARE METAL
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