CN107099661A - A kind of method that niobium is extracted from pyrochlore - Google Patents
A kind of method that niobium is extracted from pyrochlore Download PDFInfo
- Publication number
- CN107099661A CN107099661A CN201710419110.5A CN201710419110A CN107099661A CN 107099661 A CN107099661 A CN 107099661A CN 201710419110 A CN201710419110 A CN 201710419110A CN 107099661 A CN107099661 A CN 107099661A
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- CN
- China
- Prior art keywords
- niobium
- pyrochlore
- extracted
- tantalum
- leaching
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/10—Hydrochloric acid, other halogenated acids or salts thereof
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/20—Obtaining niobium, tantalum or vanadium
- C22B34/24—Obtaining niobium or tantalum
-
- 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
Abstract
The invention belongs to tantalum niobium concentrate material technology field, a kind of method that niobium is extracted from pyrochlore is disclosed, the method that niobium is extracted from pyrochlore comprises the following steps：Pyrochlore is ground；Pyrochlore is added to the in the mixed solvent of hydrochloric acid and villiaumite；By compound 1.5~3h of pressure leaching, the ore pulp after leaching obtains the filtrate containing tantalum and niobium after filtering.It is seriously polluted that the present invention solves existing hydrofluoric acid process environments, the problem of seriously constraining the sustainable development of China tantalum niobium metallurgical industry；There is provided a kind of green metallurgical new technology for developing tantalum niobium resources sustainable development, environmental pollution is alleviated；The leaching rate of niobium reaches more than 95%.
Description
Technical field
The invention belongs to tantalum niobium concentrate material technology field, more particularly to a kind of method that niobium is extracted from pyrochlore.
Background technology
Tantalum, niobium belong to rare precious metal.Tantalum has that hardness is big, dielectric constant is big, resistivity is high, the excellent spy such as corrosion-resistant
Property, mainly for the production of capacitor (account for tantalum aggregate consumption more than 60%).Niobium is then classic steel microalloy element, by with
The niobium for making steel alloy additive accounts for more than the 90% of niobium aggregate consumption.In recent years, developing rapidly with electronics and information industry
With the sustainable growth of high added value steel products demand, China tantalum niobium industry is promoted rapidly to develop, so as to be tantalum niobium hydrometallurgy
Development create excellent opportunity.At present, domestic and international Tan Ni enterprises decompose tantalum niobium concentrate stone using highly concentrated hydrofluoric acid.It is per ton
Tantalum niobium concentrate stone about consumes 4 tons of hydrofluoric acid, and 6-8 tons are reached if more low-grade tantalum niobium concentrate stone acid consumption is decomposed.Because hydrofluoric acid is easy
In volatilization, acid hemolysis process, about 10% hydrofluoric acid is volatilized in the form of waste gas containing fluoride, the generation pair of substantial amounts of fluorine-containing waste residue and waste gas
Ecological environment causes severe contamination.In recent years, for the Heavy environmental pollution caused by hydrofluoric acid technique, Bayer Bitterfeld GmbH group
Subsidiary strictly controls medium consumption by improving the inside hydrofluoric acid medium circulation approach of tantalum niobium hydrometallurgical processes, comes
The consumption of the chemical raw materials such as HF is reduced, and using Free HF in vacuum evaporation Recycling of waste liquid material.China's Zhuzhou hard alloy
The method that Group Co., Ltd is eluted afterwards using first condensing reclaims HF, the rate of recovery about 70%.It is cold that Han Jianshe etc. proposes graphite
Solidifying to absorb HF techniques, the HF rate of recovery is up to 50%-80%, and recovering effect is preferable.Existing hydrofluoric acid process environments are seriously polluted,
The sustainable development of China tantalum niobium metallurgical industry has seriously been constrained.
In summary, the problem of prior art is present be：Existing hydrofluoric acid technique uses 60-70% hydrofluoric acid conduct
Decomposition media, decomposition temperature is up to 80-90 DEG C, and hydrofluoric acid is volatile, and working environment is not only resulted in badly, and causes whole
Ecological environmental pollution is serious, and the sustainable development of China tantalum niobium metallurgical industry is seriously constrained.
The content of the invention
The problem of existing for prior art, the invention provides a kind of method that niobium is extracted from pyrochlore.
The present invention is achieved in that a kind of method that niobium is extracted from pyrochlore, described that niobium is extracted from pyrochlore
Method comprises the following steps：
Step one, pyrochlore is ground；
Step 2, pyrochlore is added the in the mixed solvent of hydrochloric acid and villiaumite；
Step 3, by compound 1.5~3h of pressure leaching, the ore pulp after leaching is obtained containing tantalum and niobium after filtering
Filtrate.
Further, pyrochlore is milled to -0.074mm in the step one.
Further, pyrochlore in mass ratio in the step 2：Villiaumite=1:0.8~2.4 carries out dispensing；Concentrated sulfuric acid concentration
Adjust to 8.5~12.5mol/；Liquid-solid ratio is controlled 4:1~8:1.
Further, in the step 3 by compound pressure be 1.5MPa~2.5MPa, temperature be 150 DEG C~200 DEG C
Under conditions of 1.5~3h of pressure leaching, speed of agitator be 400~600r/min.
Further, sulfate is the one or more in ammonium fluoride, potassium fluoride and sodium fluoride in the step 2.
Advantages of the present invention and good effect are：Compared with existing hydrofluoric acid technique, work as pyrochlore：Ammonium fluoride is with 1:0.8
When carrying out dispensing, fluorine mass concentration is reduced to 0.08% from 60-70%, greatly reduces the Funing tablet of pyrochlore decomposing solution；
Even if pyrochlore：Ammonium fluoride proportioning reaches 1:2.4, Funing tablet is also no more than 1.5% in decomposing solution, and the present invention solves existing
Hydrofluoric acid technique fluoride pollution it is serious the problem of there is provided it is a kind of develop tantalum niobium resources sustainable development the new skill of green metallurgical
Art, alleviates environmental pollution；The leaching rate of niobium reaches more than 95%.
Brief description of the drawings
Fig. 1 is the method flow diagram provided in an embodiment of the present invention that niobium is extracted from pyrochlore.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
The application principle of the present invention is explained in detail below in conjunction with the accompanying drawings.
As shown in figure 1, the method provided in an embodiment of the present invention that niobium is extracted from pyrochlore comprises the following steps：
S101：Pyrochlore is milled to -0.074mm；
S102：Pyrochlore in S101 is added to the in the mixed solvent of hydrochloric acid and villiaumite, in mass ratio pyrochlore：Villiaumite=
1:0.8~2.4 carries out dispensing；Concentrated sulfuric acid concentration is adjusted to 8.5~12.5mol/；Liquid-solid ratio is controlled 4:1~8:1；
S103：By compound in S102 pressure be 1.5MPa~2.5MPa, temperature be 150 DEG C~200 DEG C under conditions of
1.5~3h of pressure leaching, speed of agitator is 400~600r/min, and the ore pulp after leaching is obtained containing tantalum and niobium after filtering
Filtrate.
Sulfate in the step S102 is the one or more in ammonium fluoride, potassium fluoride and sodium fluoride.
The application principle of the present invention is further described with reference to specific embodiment.
Embodiment 1
20g pyrochlores are milled to -0.074mm, the in the mixed solvent of hydrochloric acid and ammonium fluoride is then added, wherein hydrochloric acid is dense
Spend for 10mol/L, ammonium fluoride is 30g, and liquid-solid ratio is 6:1；Dispensing is transferred in autoclave and carries out Leach reaction, pressure is
1.5MPa, temperature is 180 DEG C, and the reaction time is 2h.Ore pulp after leaching obtains the solution containing niobium after filtering.Through analysis,
The leaching rate of niobium respectively reaches 96.89%.
Embodiment 2
20g pyrochlores are milled to -0.074mm, the in the mixed solvent of hydrochloric acid and ammonium fluoride is then added, wherein hydrochloric acid is dense
Spend for 8.5mol/L, ammonium fluoride is 40g, and liquid-solid ratio is 5:1；Dispensing is transferred in autoclave and carries out Leach reaction, pressure is
2.0MPa, temperature is 200 DEG C, and the reaction time is 2.5h.Ore pulp after leaching obtains the solution containing niobium after filtering.Through dividing
Analysis, the leaching rate of niobium respectively reaches 95.66%.
Embodiment 3
20g pyrochlores are milled to -0.074mm, the in the mixed solvent of hydrochloric acid and potassium fluoride is then added, wherein hydrochloric acid is dense
Spend for 12.5mol/L, ammonium fluoride is 36g, and liquid-solid ratio is 7:1；Dispensing is transferred in autoclave and carries out Leach reaction, pressure is
2MPa, temperature is 180 DEG C, and the reaction time is 2.5h.Ore pulp after leaching obtains the solution containing niobium after filtering.Through analysis,
The leaching rate of niobium respectively reaches 95.62%.
Embodiment 4
20g pyrochlores are milled to -0.074mm, the in the mixed solvent of hydrochloric acid and ammonium fluoride is then added, wherein hydrochloric acid is dense
Spend for 12.5mol/L, sodium fluoride is 40g, and liquid-solid ratio is 6:1；Dispensing is transferred in autoclave and carries out Leach reaction, pressure is
1.5MPa, temperature is 200 DEG C, and the reaction time is 2.5h.Ore pulp after leaching obtains the solution containing niobium after filtering.Through dividing
Analysis, the leaching rate of niobium respectively reaches 96.16%.
Pressure leaching ore pulp of the present invention is after filtering, pickling, and the leaching rate of niobium reaches more than 95%；
The present invention solves the problem of existing hydrofluoric acid process environments are seriously polluted, and technological process is simple.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
Any modifications, equivalent substitutions and improvements made within refreshing and principle etc., should be included in the scope of the protection.
Claims (5)
1. it is a kind of from pyrochlore extract niobium method, it is characterised in that it is described from pyrochlore extract niobium method include with
Lower step：
Step one, pyrochlore is ground；
Step 2, pyrochlore is added the in the mixed solvent of hydrochloric acid and villiaumite；
Step 3, by compound 1.5~3h of pressure leaching, the ore pulp after leaching obtains the filter containing tantalum and niobium after filtering
Liquid.
2. the method for niobium is extracted from pyrochlore as claimed in claim 1, it is characterised in that by pyrochlore in the step one
It is milled to -0.074mm.
3. the method for niobium is extracted from pyrochlore as claimed in claim 1, it is characterised in that in the step 2 in mass ratio
Pyrochlore：Villiaumite=1:0.8~2.4 carries out dispensing；Concentrated sulfuric acid concentration is adjusted to 8.5~12.5mol/；Liquid-solid ratio is controlled 4:1
~8:1.
4. the method for niobium is extracted from pyrochlore as claimed in claim 1, it is characterised in that by compound in the step 3
It is 1.5MPa~2.5MPa in pressure, temperature is 1.5~3h of pressure leaching under conditions of 150 DEG C~200 DEG C, and speed of agitator is
400~600r/min.
5. the method for niobium is extracted from pyrochlore as claimed in claim 1, it is characterised in that sulfate is in the step 2
One or more in ammonium fluoride, potassium fluoride and sodium fluoride.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710419110.5A CN107099661A (en) | 2017-06-06 | 2017-06-06 | A kind of method that niobium is extracted from pyrochlore |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710419110.5A CN107099661A (en) | 2017-06-06 | 2017-06-06 | A kind of method that niobium is extracted from pyrochlore |
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| CN107099661A true CN107099661A (en) | 2017-08-29 |
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| CN201710419110.5A Pending CN107099661A (en) | 2017-06-06 | 2017-06-06 | A kind of method that niobium is extracted from pyrochlore |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109280314A (en) * | 2018-08-09 | 2019-01-29 | 苗霞明 | A kind of environmental protection flame retardant polyurethane plastics |
| CN111719055A (en) * | 2020-07-15 | 2020-09-29 | 江西拓泓新材料有限公司 | Method for decomposing and leaching tantalum and niobium from sodium-reduced tantalum-niobium metal waste |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB960433A (en) * | 1960-10-17 | 1964-06-10 | Nat Res Dev | Treatment of pyrochlore |
| US3947542A (en) * | 1972-12-08 | 1976-03-30 | Societe Francaise D'electrometallurgie | Process for treatment of pyrochlore concentrates |
| EP0041459A1 (en) * | 1980-06-02 | 1981-12-09 | Gouvernement Du Quebec | Process for the lixiviation of a niobium and/or tantalum ore containing calcium as main impurity |
| US20040213716A1 (en) * | 2003-04-24 | 2004-10-28 | Osram Sylvania Inc. | Tantalum Concentrates Dissolution and Purification Method |
| CN102753710A (en) * | 2009-09-11 | 2012-10-24 | 南非核能源有限公司 | Treatment of minerals |
| RU2013130384A (en) * | 2013-07-02 | 2015-01-10 | Открытое акционерное общество "Ангарский электролизный химический комбинат" | METHOD FOR PRODUCING NIOBIUM AND TANTALUM OXIDES FROM ORE CONCENTRATES |
-
2017
- 2017-06-06 CN CN201710419110.5A patent/CN107099661A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB960433A (en) * | 1960-10-17 | 1964-06-10 | Nat Res Dev | Treatment of pyrochlore |
| US3947542A (en) * | 1972-12-08 | 1976-03-30 | Societe Francaise D'electrometallurgie | Process for treatment of pyrochlore concentrates |
| EP0041459A1 (en) * | 1980-06-02 | 1981-12-09 | Gouvernement Du Quebec | Process for the lixiviation of a niobium and/or tantalum ore containing calcium as main impurity |
| US20040213716A1 (en) * | 2003-04-24 | 2004-10-28 | Osram Sylvania Inc. | Tantalum Concentrates Dissolution and Purification Method |
| CN102753710A (en) * | 2009-09-11 | 2012-10-24 | 南非核能源有限公司 | Treatment of minerals |
| RU2013130384A (en) * | 2013-07-02 | 2015-01-10 | Открытое акционерное общество "Ангарский электролизный химический комбинат" | METHOD FOR PRODUCING NIOBIUM AND TANTALUM OXIDES FROM ORE CONCENTRATES |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109280314A (en) * | 2018-08-09 | 2019-01-29 | 苗霞明 | A kind of environmental protection flame retardant polyurethane plastics |
| CN111719055A (en) * | 2020-07-15 | 2020-09-29 | 江西拓泓新材料有限公司 | Method for decomposing and leaching tantalum and niobium from sodium-reduced tantalum-niobium metal waste |
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Application publication date: 20170829 |
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