CN103160684A - Method for extracting tantalum and niobium through low alkali decomposition of tantalum-niobium ore - Google Patents
Method for extracting tantalum and niobium through low alkali decomposition of tantalum-niobium ore Download PDFInfo
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- CN103160684A CN103160684A CN2011104211826A CN201110421182A CN103160684A CN 103160684 A CN103160684 A CN 103160684A CN 2011104211826 A CN2011104211826 A CN 2011104211826A CN 201110421182 A CN201110421182 A CN 201110421182A CN 103160684 A CN103160684 A CN 103160684A
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Abstract
The invention relates to a method for extracting tantalum and niobium through low alkali decomposition of a tantalum-niobium ore. According to the method, a small amount of sodium hydroxide is used as a melting agent for roasting decomposition of the tantalum-niobium ore to allow tantalum and niobium to be converted into sodium metatantalate and sodium metaniobate; and then, under the condition of addition of a conversion agent, tantalum and niobium in a roasting product are extracted with diluted hydrofluoric acid at a low temperature so as to obtain ore pulp containing fluotantalic acid and fluoniobic acid. The method provided by the invention has the advantages of simple process flow, small consumption of alkali, low cost and capacity of realizing nearly 100% of a tantalum-niobium ore decomposition rate.
Description
Technical field
The present invention relates to a kind of tantalum niobium concentrate decomposition method, specifically relate to a kind of method that adopts low alkali number to decompose tantalum niobium concentrate extraction tantalum and niobium.
Background technology
Tantalum, niobium belong to rare refractory metal, obtain using more and more widely in each side such as the industry such as electronics, iron and steel, space travel, computing technique and medical science.At present, the method for processing tantalum niobium concentrate both at home and abroad mainly comprises hydrofluoric acid decomposition method and alkali fusion.The hydrofluoric acid decomposition method is the method for industrial main application at present.In the hydrofluoric acid decomposition method, adopt the mixing acid of high dense hydrofluoric acid or high dense hydrofluoric acid-sulfuric acid to decompose the tantalum niobium concentrate thing, in this process, 6～7% hydrofluoric acid vapors away with the form of waste gas, causes serious topsoil, and highly toxic hydrofluoric acid can damage people's health; In the liquid waste disposal process, one ton of tantalum niobium concentrate of every processing can produce the fluorine-containing waste residue of 10～15 tons, causes very serious environmental pollution.In addition, although China's tantalum niobium aboundresources, most tantalum niobium concentrate bed reserves are little, the low and complicated components of ore grade.If adopt existing hydrofluoric acid method to process, the rate of decomposition of tantalum niobium concentrate is only 85% left and right, causes the great wasting of resources.
Traditional alkali fusion adopt potash or soda under the high temperature of 800-900 ℃ with the tantalum niobium concentrate frit reaction, and then extract tantalum and niobium from molten reaction products.The method is controlled at the frit reaction condition in the scope that makes tantalum and niobium generate tantalum niobium normal salt, needs higher alkali ore deposit ratio, and alkali consumption is excessive, is 6～8 times of theoretical amount, and alkali can not efficient recovery, and cost is higher.In order to satisfy the growing tantalum niobium market requirement, need badly at present and develop a kind of novel process low-grade, complicated components tantalum niobium raw material that is applicable to process.
For low-grade, difficult tantalum niobium concentrate, Chinese patent CN1605639A and CN101191161A successively disclose terms of settlement.Chinese patent CN1605639A discloses a kind of tantalum niobium concentrate cleaning transforming method, and the method adopts high density KOH solution to substitute the hydrofluoric acid treatment tantalum niobium concentrate, obtained and decomposed preferably effect, but the method reaction conditions is comparatively harsh, to having relatively high expectations of equipment.Perfect as to the method, patent CN10119116A discloses a kind of mechanical activation reinforcement, and purpose is that tantalum niobium concentrate is carried out pre-treatment, destroys mineral lattice, makes the difficult Mineral Transformation of decomposing for easily decomposing mineral, thereby reduces temperature of reaction and alkaline concentration.But this method has increased the mechanical activation pretreatment procedure, causes operation loaded down with trivial details.
Summary of the invention
The present invention is directed to existing hydrofluoric acid technique fluoride pollution serious, be unsuitable for processing low grade ore, difficult tantalum niobium concentrate and traditional alkali fusion decomposition temperature is high, alkali consumption is large, cost the is high problem of decomposing, proposed the low alkali of tantalum niobium concentrate that a kind of technical process is simple, the tantalum niobium concentrate rate of decomposition is high and economic and decomposed the method for extracting tantalum and niobium.The condition that the method is decomposed tantalum niobium concentrate alkali is controlled at the scope that generates the inclined to one side salt of tantalum niobium, thereby the alkali consumption is down near theoretical amount, greatly reduces alkaline consumption, provides cost savings.
The objective of the invention is to realize by the following technical solutions:
1) sodium hydroxide and tantalum niobium concentrate are mixed after, put into retort furnace, decompose 10～60min under the condition of 550～700 ℃.
Described sodium hydroxide concentration is 1.0～1.5 times of theoretical amount.
The initial particle size of described tantalum niobium concentrate is 58～150 μ m.
2) after product to be decomposed is down to normal temperature, quantitatively adds agent transition and leach degradation production 1.5～5.0h with hydrofluoric acid, generate the ore pulp of diffluent fluorine niobic acid and fluorotantalic acid.
Described initial hydrofluoric acid concentration is 3.00～6.06mol/L.
Described transition, temperature was 50～80 ℃.
Described transition liquid-solid ratio (m: v) be 5: 1～10: 1.
Described roasting condition be stirring-type (half industry or industrial rank) or without stirring-type (laboratory rank).
Described agent transition is silicofluoric acid, quartz, silica gel or other silicon-containing compound.
Described time transition is 1.5～5.0h.
Description of drawings
Accompanying drawing 1 is that the low alkali of tantalum niobium concentrate provided by the invention decomposes the process flow sheet that extracts tantalum and niobium.
Embodiment
Embodiment 1:
After sodium hydroxide and tantalum niobium concentrate are mixed, put into retort furnace, in mixture, alkali ore deposit mass ratio is 1: 1, the initial particle size of tantalum niobium concentrate is 58～75 μ m, decompose 30min under 650 ℃, react complete after, obtain containing sodium metatantalate and sodium columbate and a small amount of sodium tantalate and the degradation production of sodium columbate partially, after product to be decomposed is cooled to normal temperature, adding 5ml 0.6mol/L silicofluoric acid is also that 4.00mol/L hydrofluoric acid is at 60 ℃ with initial concentration, liquid-solid ratio (m: v) be under the condition of 10: 1 transition leach 2h, obtain ore pulp after leaching.
Analyze through ICP-AES, in tantalum niobium concentrate, the rate of decomposition of tantalum, niobium is respectively 99.2% and 99.5%.
Embodiment 2:
After sodium hydroxide and tantalum niobium concentrate are mixed, put into retort furnace, in mixture, alkali ore deposit mass ratio is 12: 1, the initial particle size of tantalum niobium concentrate is 75～106 μ m, decompose 50min under 600 ℃, react complete after, obtain containing sodium metatantalate and sodium columbate and a small amount of sodium tantalate and the degradation production of sodium columbate partially, after product to be decomposed is cooled to normal temperature, adding 0.5g quartzy is also that 5.06mol/L hydrofluoric acid is at 70 ℃ with initial concentration, liquid-solid ratio (m: v) be under the condition of 8: 1 transition leach 3h, obtain ore pulp after leaching.
Analyze through ICP-AES, in tantalum niobium concentrate, the rate of decomposition of tantalum, niobium is respectively 99.1% and 99.3%.
Embodiment 3:
After sodium hydroxide and tantalum niobium concentrate are mixed, put into retort furnace, in mixture, alkali ore deposit mass ratio is 1.5: 1, the initial particle size of tantalum niobium concentrate is 58～75 μ m, decompose 60min under 550 ℃, react complete after, obtain containing sodium metatantalate and sodium columbate and a small amount of sodium tantalate and the degradation production of sodium columbate partially, after product to be decomposed is cooled to normal temperature, adding 0.8g silica gel is also that 5.39mol/L hydrofluoric acid is at 80 ℃ with initial concentration, liquid-solid ratio (m: v) be under the condition of 7: 1 transition leach 2h, obtain ore pulp after leaching.
Analyze through ICP-AES, in tantalum niobium concentrate, the leaching yield of tantalum, niobium is respectively 99.1% and 99.5%.
Embodiment 4:
After sodium hydroxide and tantalum niobium concentrate are mixed, put into retort furnace, in mixture, alkali ore deposit mass ratio is 1.3: 1, the initial particle size of tantalum niobium concentrate is 75～106 μ m, decompose 10min under 700 ℃, react complete after, obtain containing sodium metatantalate and inclined to one side sodium columbate and a small amount of sodium tantalate and sodium columbate, after product to be decomposed is cooled to normal temperature, adding 5ml 0.6mol/L silicofluoric acid is also that 6.06mol/L hydrofluoric acid is at 80 ℃ with initial concentration, liquid-solid ratio be under the condition of 5: 1 transition leach 1.5h, obtain ore pulp after leaching.
Analyze through ICP-AES, in tantalum niobium concentrate, the leaching yield of tantalum, niobium is respectively 99% and 99.2%.
Claims (10)
1. one kind low alkali decomposes the method that tantalum niobium concentrate extracts tantalum and niobium, comprises the steps:
A) sodium hydroxide and tantalum niobium concentrate are mixed after, put into retort furnace and carry out roasting;
B) product of roasting after being cooled to normal temperature, adding agent transition and leaches product of roasting with diluted hydrofluoric acid, obtains fluorine-containing niobic acid
Ore pulp with fluorotantalic acid.
2. method according to claim 1, is characterized in that described sodium hydroxide concentration is 1.0～1.5 times of theoretical amount.
3. method according to claim 1, is characterized in that described maturing temperature is 550～700 ℃, and roasting time is 10～60min.
4. method according to claim 1, is characterized in that described initial tantalum niobium concentrate thing particle diameter is 58～150 μ m.
5. method according to claim 1, it is characterized in that described roasting condition be stirring-type or without stirring-type.
6. method according to claim 1, is characterized in that described agent transition is silicofluoric acid, quartz, silica gel or other silicon-containing compound.
7. method according to claim 1, is characterized in that described initial hydrofluoric acid concentration is 3.00～6.06mol/L.
8. method according to claim 1 is characterized in that described transition, temperature was 50～80 ℃.
9. method according to claim 1, is characterized in that described time transition is 1.5～5.0h.
10. method according to claim 1 is characterized in that described transition of liquid-solid ratio (m: v) 5: 1～10: 1.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103572045A (en) * | 2012-07-23 | 2014-02-12 | 中国科学院过程工程研究所 | Alkali-acid combined technology for processing low-grade niobium-tantalum ore |
| 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 |
| CN113151669A (en) * | 2021-04-28 | 2021-07-23 | 郑州大学 | Method for decomposing low-grade tantalum-niobium resource and extracting tantalum-niobium by alkaline process |
| CN113151695A (en) * | 2021-04-28 | 2021-07-23 | 郑州大学 | Method for decomposing low-grade tantalum-niobium resource and extracting tantalum-niobium by acid method |
| CN113186399A (en) * | 2021-03-12 | 2021-07-30 | 北京工业大学 | Method for extracting tantalum and niobium |
| CN113234920A (en) * | 2021-04-30 | 2021-08-10 | 长沙矿冶研究院有限责任公司 | Method for converting niobium minerals in niobium rough concentrate into sodium niobium minerals and producing niobium concentrate |
| CN113388745A (en) * | 2021-06-15 | 2021-09-14 | 中国科学院过程工程研究所 | Method for extracting valuable components from niobium-iron rutile without fluorine |
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| US3058825A (en) * | 1958-09-22 | 1962-10-16 | Paul B Cardon | Process for recovering columbium and tantalum from ores and ore concentrates containing same |
| CN1605639A (en) * | 2003-10-08 | 2005-04-13 | 中国科学院过程工程研究所 | Process for clean conversion of tantalum niobium ore |
| CN101191161A (en) * | 2006-11-22 | 2008-06-04 | 中国科学院过程工程研究所 | Mechanical activating strengthening alkali decomposition cleaning transforming method for hard-decomposition tantalum niobium concentrate |
| 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 |
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2011
- 2011-12-15 CN CN2011104211826A patent/CN103160684A/en active Pending
Patent Citations (4)
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| US3058825A (en) * | 1958-09-22 | 1962-10-16 | Paul B Cardon | Process for recovering columbium and tantalum from ores and ore concentrates containing same |
| CN1605639A (en) * | 2003-10-08 | 2005-04-13 | 中国科学院过程工程研究所 | Process for clean conversion of tantalum niobium ore |
| CN101191161A (en) * | 2006-11-22 | 2008-06-04 | 中国科学院过程工程研究所 | Mechanical activating strengthening alkali decomposition cleaning transforming method for hard-decomposition tantalum niobium concentrate |
| 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 |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103572045A (en) * | 2012-07-23 | 2014-02-12 | 中国科学院过程工程研究所 | Alkali-acid combined technology for processing low-grade niobium-tantalum ore |
| 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 |
| CN113186399A (en) * | 2021-03-12 | 2021-07-30 | 北京工业大学 | Method for extracting tantalum and niobium |
| CN113186399B (en) * | 2021-03-12 | 2022-11-18 | 北京工业大学 | Method for extracting tantalum and niobium |
| CN113151669A (en) * | 2021-04-28 | 2021-07-23 | 郑州大学 | Method for decomposing low-grade tantalum-niobium resource and extracting tantalum-niobium by alkaline process |
| CN113151695A (en) * | 2021-04-28 | 2021-07-23 | 郑州大学 | Method for decomposing low-grade tantalum-niobium resource and extracting tantalum-niobium by acid method |
| CN113151669B (en) * | 2021-04-28 | 2022-07-29 | 郑州大学 | Method for decomposing low-grade tantalum-niobium resource and extracting tantalum-niobium by alkaline process |
| CN113151695B (en) * | 2021-04-28 | 2022-08-09 | 郑州大学 | Method for decomposing low-grade tantalum-niobium resource and extracting tantalum-niobium by acid method |
| CN113234920A (en) * | 2021-04-30 | 2021-08-10 | 长沙矿冶研究院有限责任公司 | Method for converting niobium minerals in niobium rough concentrate into sodium niobium minerals and producing niobium concentrate |
| CN113388745A (en) * | 2021-06-15 | 2021-09-14 | 中国科学院过程工程研究所 | Method for extracting valuable components from niobium-iron rutile without fluorine |
| CN113388745B (en) * | 2021-06-15 | 2022-09-02 | 中国科学院过程工程研究所 | Method for extracting valuable components from niobium-iron rutile without fluorine |
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Application publication date: 20130619 |