CN102586598A - Method for decomposing tantalum-niobium compound - Google Patents
Method for decomposing tantalum-niobium compound Download PDFInfo
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- CN102586598A CN102586598A CN2012100786655A CN201210078665A CN102586598A CN 102586598 A CN102586598 A CN 102586598A CN 2012100786655 A CN2012100786655 A CN 2012100786655A CN 201210078665 A CN201210078665 A CN 201210078665A CN 102586598 A CN102586598 A CN 102586598A
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- niobium compound
- tantalum
- tantalum niobium
- reaction
- acid
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
The invention relates to a method for decomposing a tantalum-niobium compound. The method comprises the following steps of: adding the tantalum-niobium compound into a mixture of high-boiling-point acid and fluoride, heating to 95 to 200 DEG C, reacting for 1 to 2 hours under full agitation, and dissolving a reaction product in water to obtain a tantalum-niobium solution after the reaction. The fluoride and the high-boiling-point acid (concentrated sulfuric acid or strong phosphoric acid) are used for reacting, and the reaction temperature can be raised to 90 to 200 DEG C, so that the tantalum-niobium compound is further decomposed in a melt at high temperature; and therefore, the decomposition rate is improved and reaches over 95 percent. Meanwhile, the whole reaction system works under the condition of low moisture, and the reaction temperature is increased, so that the further decomposition of the tantalum-niobium compound is facilitated.
Description
Technical field
The present invention relates to metallurgical technology field, particularly relate to a kind of decomposition method of tantalum niobium compound.
Background technology
Present tantalum niobium extracts, purification process mainly is to adopt wet method hydrofluoric acid-sulfuric acid-MIBK system system, is about to tantalum niobium concentrate stone or/and tantalum niobium compound and 55% above hydrofluoric acid and strong sulfuric acid response decompose aqueous phase with the tantalum niobium.In this technology, owing to reasons such as temperature, the rate of decomposition of tantalum niobium compound can only reach 92%～95%.Can not decompose in this way for tantalum oxide or niobium oxides, utilize this method to handle tantalum oxide and niobium oxides, rate of decomposition is lower than 5%.
Actual based on producing, in substance reaction processes such as tantalum niobium raw material and hydrofluoric acid, the fluorine ion that improve reaction temperature, improves in the reactant can improve resolution ratio.But top temperature can only reach about 90 ℃-95 ℃ in present tantalum niobium production process, after temperature is too high, can reach the boiling point of water, evaporates with a large amount of steam or hydrogen fluoride gas, and environmental influence is bigger.
Chinese patent CN 1159424 A have introduced and have utilized K
2CO
3The method of decomposing oxidation tantalum, but this method cycle is longer, and cost is higher.
Summary of the invention
The object of the invention just is to overcome the defective of above-mentioned prior art, a kind of tantalum niobium concentrate stone of effective raising tantalum niobium compound rate of decomposition is provided and contains the decomposition method of the compound of tantalum niobium.
For realizing that the technical scheme that the present invention taked is:
A kind of decomposition method of tantalum niobium compound; It is characterized in that: at first the tantalum niobium compound is joined in the mixture of high boiling point acid and fluorochemical; Be heated to 95 ℃～200 ℃ then; Fully stirring reaction 1-2 hour, reaction back water solubilizing reaction thing obtained tantalum niobium solution, and the mass ratio of above-mentioned tantalum niobium compound and high boiling point acid and fluorochemical is: 1:1.5-10:1.5-10;
Above-mentioned high boiling point acid is the vitriol oil or the 80% above SPA more than 90%, is preferably concentration and is 98% sulfuric acid and 85% phosphoric acid;
Above-mentioned fluorochemical is one or more in Neutral ammonium fluoride, matt salt, Potassium monofluoride, Sodium Fluoride, ALUMNIUM FLUORIDE, potassium hydrogen fluoride, sodium bifluoride and the potassium silicofluoride;
Above-mentioned Heating temperature is 110 ℃～180 ℃.
The present invention adopts fluorochemical and high boiling point acid (vitriol oil or SPA) reaction; Temperature of reaction is brought up between 95-200 ℃; The tantalum niobium compound can further react with fluorion under the high temperature; Impel in the tantalum niobium compound melts at high temperature and further decompose, thereby improve rate of decomposition.Because whole reaction system is operation under the low moisture situation, can make the boiling point of reaction simultaneously, increase the concentration of ion and tantalum niobium element reaction, help the raising of tantalum niobium rate of decomposition more above water.
Embodiment
Embodiment 1
With 1 kilogram of Ta
2O
5Be dissolved in 2 kilograms 98% sulfuric acid, be heated to 110 ℃, add 2 kilograms of Sodium Fluorides then; Reactant is stirred, utilize the hydrogen fluoride gas of emitting in the cooling water circulation absorption reaction, reaction back water solubilizing reaction thing; Obtain containing the solution of the solution 10L of tantalum niobium, wherein contained Ta
2O
5Content is 98.7g/L, Ta
2O
5Rate of decomposition is 98.7%.
Embodiment 2
With 1 kilogram of Nb
2O
5Be dissolved in 10 kilograms 98% sulfuric acid, be heated to 120 ℃, add 4 kilograms of ALUMNIUM FLUORIDEs then; Reactant is stirred, utilize the hydrogen fluoride gas of emitting in the cooling water circulation absorption reaction, reaction back water solubilizing reaction thing; Obtain containing the solution of the solution 10L of tantalum niobium, wherein contained Nb
2O
5Content is 98.7g/L, Ta
2O
5Rate of decomposition is 98.7%.
Embodiment 3
With 0.5 kilogram of Nb
2O
5With 0.5 kilogram of Ta
2O
5Mixture be dissolved in 3 kilograms the SPA, be heated to 110 ℃, add 1 kilogram of Potassium monofluoride then; Reactant is stirred, utilize the hydrogen fluoride gas of emitting in the cooling water circulation absorption reaction, reaction back water solubilizing reaction thing; Obtain containing the solution of the solution 10L of tantalum niobium, wherein contained Nb
2O
5Content is 49.6g/L, Ta
2O
5Content is 49.5g/L, Nb
2O
5Rate of decomposition is 99.2%, Ta
2O
5Rate of decomposition is 99%.
Embodiment 4
With 1 kilogram of Nb
2O
5Be dissolved in 6 kilograms the SPA, be heated to 180 ℃, add 3 kilograms of Sodium Fluorides then; Reactant is stirred, utilize the hydrogen fluoride gas of emitting in the cooling water circulation absorption reaction, reaction back water solubilizing reaction thing; Obtain containing the solution of the solution 20L of niobium, wherein contained Nb
2O
5Content is 49.4g/L, Nb
2O
5Rate of decomposition is 98.8%.
Embodiment 5
With 1 kilogram of ore content is tantalum oxide 25.4%, and niobium oxides 10.1%, mixture are dissolved in 1.5 kilograms the vitriol oil; Be heated to 170 ℃, add 1.5 kilograms of potassium silicofluorides then, reactant is stirred; Utilize the hydrogen fluoride gas of emitting in the cooling water circulation absorption reaction; Reaction back water solubilizing reaction thing has obtained containing the solution of the solution 5L of tantalum niobium, wherein contains Nb
2O
5Content is 18.9g/L, Ta
2O
5Content is 47.6g/L, Nb
2O
5Rate of decomposition is 95.2%, Ta
2O
5Rate of decomposition is 94.5%.
Embodiment 6
With 1 kilogram of content is tantalum oxide 99%, is dissolved in 10 kilograms the vitriol oil, is heated to 120 ℃; Add 10 kilograms of ALUMNIUM FLUORIDEs then, reactant is stirred, utilize the hydrogen fluoride gas of emitting in the cooling water circulation absorption reaction; Reacted about 60 minutes; Reaction back water solubilizing reaction thing has obtained containing the solution of the solution 15L of tantalum niobium, wherein contains Ta
2O
5Content is 65g/L, Ta
2O
5Rate of decomposition is 97.5%.
Claims (5)
1. the decomposition method of a tantalum niobium compound; It is characterized in that: at first the tantalum niobium compound is joined in the mixture of high boiling point acid and fluorochemical; Be heated to 95 ℃～200 ℃ then; Fully stirring reaction 1-2 hour, reaction back water solubilizing reaction thing obtained tantalum niobium solution, and the mass ratio of above-mentioned tantalum niobium compound and high boiling point acid and fluorochemical is: 1:1.5-10:1.5-10.
2. according to the decomposition method of the described tantalum niobium compound of claim 1, it is characterized in that above-mentioned high boiling point acid is the vitriol oil or the 80% above SPA more than 90%.
3. according to the decomposition method of the described tantalum niobium compound of claim 1, it is characterized in that above-mentioned high boiling point acid concentration is 98% sulfuric acid and 85% phosphoric acid.
4. according to the decomposition method of the described tantalum niobium compound of claim 1, it is characterized in that above-mentioned fluorochemical is one or more in Neutral ammonium fluoride, matt salt, Potassium monofluoride, Sodium Fluoride, ALUMNIUM FLUORIDE, potassium hydrogen fluoride, sodium bifluoride and the potassium silicofluoride.
5. according to the decomposition method of the described tantalum niobium compound of claim 1, it is characterized in that above-mentioned Heating temperature is 110 ℃～180 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012100786655A CN102586598A (en) | 2012-03-23 | 2012-03-23 | Method for decomposing tantalum-niobium compound |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012100786655A CN102586598A (en) | 2012-03-23 | 2012-03-23 | Method for decomposing tantalum-niobium compound |
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|---|---|
| CN102586598A true CN102586598A (en) | 2012-07-18 |
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| CN2012100786655A Pending CN102586598A (en) | 2012-03-23 | 2012-03-23 | Method for decomposing tantalum-niobium compound |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110964928A (en) * | 2019-12-20 | 2020-04-07 | 西安瑞鑫科金属材料有限责任公司 | Method for dissolving tantalum from tantalum-containing material |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1076731A (en) * | 1992-03-06 | 1993-09-29 | H.C施塔克公司 | The method of isolating tantalum and niobium |
| CN1420185A (en) * | 1996-03-26 | 2003-05-28 | 卡伯特公司 | Obtaining product by solubilizing metal component from Ta-Nb metal ore contg. insoluble fluoride |
| CN101215635A (en) * | 2007-01-05 | 2008-07-09 | 中国科学院过程工程研究所 | Method for separating tantalum and niobium from potassium metatantalate and potassium metaniobate mixture |
-
2012
- 2012-03-23 CN CN2012100786655A patent/CN102586598A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1076731A (en) * | 1992-03-06 | 1993-09-29 | H.C施塔克公司 | The method of isolating tantalum and niobium |
| CN1420185A (en) * | 1996-03-26 | 2003-05-28 | 卡伯特公司 | Obtaining product by solubilizing metal component from Ta-Nb metal ore contg. insoluble fluoride |
| US20030170158A1 (en) * | 1996-03-26 | 2003-09-11 | Hard Robert A. | Method for solubilizing metal values |
| CN101215635A (en) * | 2007-01-05 | 2008-07-09 | 中国科学院过程工程研究所 | Method for separating tantalum and niobium from potassium metatantalate and potassium metaniobate mixture |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110964928A (en) * | 2019-12-20 | 2020-04-07 | 西安瑞鑫科金属材料有限责任公司 | Method for dissolving tantalum from tantalum-containing material |
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Application publication date: 20120718 |