CN102747223A - Method for extracting tungsten from tungsten mineral by using soda and adopting high-pressure leaching process - Google Patents
Method for extracting tungsten from tungsten mineral by using soda and adopting high-pressure leaching process Download PDFInfo
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- CN102747223A CN102747223A CN2012102521979A CN201210252197A CN102747223A CN 102747223 A CN102747223 A CN 102747223A CN 2012102521979 A CN2012102521979 A CN 2012102521979A CN 201210252197 A CN201210252197 A CN 201210252197A CN 102747223 A CN102747223 A CN 102747223A
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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
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention discloses a method for extracting tungsten from tungsten mineral by using soda and adopting high-pressure leaching process, comprising the following steps: adding soda and additives into primary tungsten autoclaving slag, carrying out secondary autoclaving at high temperature and pressure; separating the leaching solution from the slag; carrying out primary autoclaving to the tungsten by the leaching solution; separating the primary autoclaving slag from the crude sodium tungstate solution, wherein the primary autoclaving slag is used as the raw material; and mixing the tungstate with the secondary autoclaving leaching solution to prepare slurry. The liquid-solid ratio is controlled to be (3-5):1 in the step of adding the soda and the additives into the primary autoclaving slag and mixing to prepare the slurry, and the soda has the excess coefficient of 2.0-2.5. The liquid-solid ratio is controlled to be (3-5):1 in the step of mixing the tungstate with the secondary autoclaving leaching solution to prepare the slurry. The primary autoclaving temperature and the secondary autoclaving temperature are both 170-240 DEG C, the primary autoclaving pressure and the secondary autoclaving pressure are both 0.9-2.8MPa, and the primary autoclaving time and the secondary autoclaving time are both 2-4 hours. The additives are solid caustic soda and alumina. The method adopts the soda to autoclave the tungsten mineral to extract tungsten at counterflow by using soda at high pressure, so that the leaching rate of the tungsten mineral is more than 99%, the content of WO3 in the tungsten slag is less than 1.0%, the use amount of soda is reduced, and the content of soda in the leaching solution is reduced effectively.
Description
Technical field
The present invention relates to the process for extracting of the tungsten in the tungsten smelting, especially adopt the soda high pressure lixiviation process to extract the method for tungsten in the tungsten minerals.
Background technology
Decomposition leaching method to the multiclass tungsten minerals mainly contains the caustic soda lixiviation process at present, unites the pressure cooking method, fluorochemical decomposition method, acid decomposition, soda high pressure lixiviation process.Wherein the rate of decomposition of caustic soda lixiviation process dialogue tungsten, tungsten ore is not really desirable, and the caustic soda excess coefficient is big, WO in the slag
3Content is higher; The patented technology of in the aforesaid method process, introducing the mechanical activation process had been invented in Li Hong osmanthus afterwards, though rate of decomposition is improved, the caustic soda excess coefficient decreases; But still the tungsten in can not the depth extraction tungsten ore, plant-scale tungsten slag contains WO
3Be generally 1.5～4%.General high grace patent is united and is pressed cooking method to solve the recycling problem of caustic soda preferably, obtains the high de-agglomeration rate but can not stablize when handling white tungsten, tungsten ore, and plant-scale white tungsten slag contains WO
3Be generally 1.5～4%, unite to press and boil the black general tungstenic 1.5～3% of tungsten slag.The fluorochemical decomposition method can only be handled sheelite, and the price amount of increase of fluorochemical is bigger in recent years, and mineral resources is complicated more, and the excess coefficient of fluorochemical increases, and causes production cost to improve again and again.Acid system decomposes big to equipment corrosion, does not re-use basically.Because tungsten resource is in short supply day by day, each tungsten smelting enterprise all in the ability of strengthening handling various mineral resources, often need handle white tungsten simultaneously, tungsten ore, and wolframite, expectation simultaneously obtains high yield.The soda high pressure lixiviation process can address these problems, but the soda pressuring cooking temperature, pressure is high, and the periodical operation thermal waste is serious, and the soda excess coefficient is big, and generally about 4 times, remaining soda also is a difficult problem in the recovery solution.
Summary of the invention
The present invention is directed to above-mentioned deficiency, propose the method that a kind of soda high pressure lixiviation process extracts tungsten in the tungsten minerals, this method adopts two sections adverse currents of soda high pressure to press and boils tungsten minerals extraction tungsten, can make the leaching yield of tungsten ore reach more than 99% WO in the tungsten slag
3Content reduces the soda consumption simultaneously less than 1.0%, effectively reduces the sodiun carbomate inventory in the leach liquor.
Realize that the technical scheme that the object of the invention adopts is:
(1) the once pressure of white tungsten fine ore, wolframite or tungsten ore is boiled slag, with soda and additive carries out tungsten ore and once presses the two-stage autoclave that boils slag under HTHP;
(2) two-stage autoclave being obtained is that the two-stage autoclave slag separates with the two-stage autoclave leach liquor, and said two-stage autoclave leach liquor is the solution of the low high soda concentration of tungsten, and the two-stage autoclave slag is discarded;
(3) utilizing the secondary leach liquor that hangs down the high soda concentration of tungsten that white tungsten fine ore, wolframite or tungsten ore are once pressed boils;
(4) coarse sodium tungstate that step (3) is obtained boils slag with the once pressure of white tungsten fine ore, wolframite or tungsten ore to be separated, and once presses to boil slag and change step (1) over to and make raw material.
Wherein: it is 3～5:1 that the once pressure of the middle white tungsten fine ore of step (1), wolframite or tungsten ore is boiled the liquid-solid ratio that slag is with soda and the additive batch mixing is sized mixing; The soda excess coefficient is 2.0～2.5; 170～240 ℃ of two-stage autoclave temperature, pressure 0.9～2.8MPa, time 2～4 hours.
White tungsten fine ore, wolframite or tungsten ore and two-stage autoclave leach liquor batch mixing are sized mixing in the step (3), and the control liquid-solid ratio is 3～5:1, once press and boil 170～240 ℃ of temperature, pressure 0.9～2.8MPa, time 2～4 hours.
Said additive is solid caustic soda and aluminum oxide.
Boil leaching owing to adopt two sections adverse currents of soda high pressure to press to tungsten ore (white tungsten fine ore, wolframite or tungsten ore); Reduce the excess coefficient of soda; The tungsten slag that promptly obtains with soda pressuring cooking operation carries out two-stage autoclave; Soda solution reaction with newly joining obtains maximum reaction impellent, with the WO in the raw material
3Extract to greatest extent,, leach the stage, contain the leach liquor and the tungsten ore reaction of higher soda concentration, make the WO more than 60% in the tungsten ore at secondary to obtain the rate of decomposition of the highest tungsten
3Get into solution, so the free NaCO in the leach liquor
3Concentration is very low.
The present invention has well solved sheelite, wolframite, tungsten ore soda pressuring cooking process middle soda excess coefficient height, the problem of leach liquor middle soda Separation and Recovery, and can guarantee stable high de-agglomeration rate.
Description of drawings
Fig. 1 is a schema of the present invention.
Embodiment
Embodiment 1 white tungsten fine ore is once pressed the two-stage autoclave that boils slag.Get white tungsten fine ore and once press and boil slag, add 116g soda, excess coefficient 2.1, with the 13g solid caustic soda, 12g aluminum oxide and 1200ml water are sized mixing liquid-solid ratio 4:1; Two-stage autoclave is 4.0 hours under 230 ℃ of temperature, pressure 2.5MPa.The step-down blowing filters afterwards, two-stage autoclave slag sampling analysis, and the slag tungstenic: 0.48%, the discarded stacking; WO in the filtrating
3: 14.47g/l; The leaching yield of tungsten ore: 99.44%.
White tungsten fine ore is once pressed and is boiled.Measure two-stage autoclave filtrating, add the mixing of 250g white tungsten fine ore fine powder and size mixing, control liquid-solid ratio 5:1,230 ℃ of temperature, pressure 2.5MPa leached 4.0 hours down.The step-down blowing filters afterwards, and slag changes the two-stage autoclave batching over to; WO in the filtrating
3: 97.84g/l changes subsequent handling over to.
Embodiment 2 white tungsten ores are once pressed the two-stage autoclave that boils slag.Get tungsten ore and once press and boil slag, add 146g soda, excess coefficient 2.5, with the 13g solid caustic soda, 12g aluminum oxide and 1200ml water are sized mixing liquid-solid ratio 3:1; Two-stage autoclave is 4.0 hours under 180 ℃ of temperature, pressure 0.9MPa.The step-down blowing filters afterwards, two-stage autoclave slag sampling analysis, and the slag tungstenic: 0.36%, the discarded stacking; Filtrating WO
3: 53.30g/l; The leaching yield of tungsten ore: 99.35%.
White tungsten ore is once pressed and is boiled.Measure two-stage autoclave filtrating, add the mixing of 345g tungsten ore fine powder and size mixing, control liquid-solid ratio 3:1,180 ℃ of temperature, pressure 0.9MPa leached 4.0 hours down.The step-down blowing filters afterwards, and slag changes the two-stage autoclave batching over to; Filtrating WO
3: 79.90g/l changes subsequent handling over to.
Embodiment 3 white tungsten ores are once pressed the two-stage autoclave that boils slag.Get white tungsten ore and once press and boil slag, add 147g soda, excess coefficient 2.5, with the 12g solid caustic soda, 6.5g aluminum oxide and 1100ml water are sized mixing liquid-solid ratio 3:1; Two-stage autoclave is 2.0 hours under 230 ℃ of temperature, pressure 2.4MPa.The step-down blowing filters afterwards, two-stage autoclave slag sampling analysis, slag tungstenic: 0.11 %, the discarded stacking; WO in the filtrating
3: 40.41g/l; The leaching yield of tungsten ore: 99.79%.
White tungsten ore is once pressed and is boiled.Measure two-stage autoclave filtrating, add the white tungsten ore fine powder mixing of 345g and size mixing, control liquid-solid ratio 3:1 leached 2.0 hours under 230 ℃ of temperature, pressure 2.4MPa.The step-down blowing filters afterwards, and slag changes the two-stage autoclave batching over to; WO in the filtrating
3: 109.66g/l changes subsequent handling over to.
Embodiment 4 wolframites are once pressed the two-stage autoclave that boils slag.Get wolframite and once press and boil slag, add 135g soda, excess coefficient 2.3, with the 13g solid caustic soda, 12g aluminum oxide and 1200ml water are sized mixing liquid-solid ratio 5:1; Two-stage autoclave is 4.0 hours under 230 ℃ of temperature, pressure 2.5MPa.The step-down blowing filters afterwards, two-stage autoclave slag sampling analysis, slag tungstenic: 0.69 %, the discarded stacking; Filtrating WO
3: 5.32g/l; The leaching yield of tungsten ore: 99.63%.
Wolframite is once pressed and is boiled.Measure two-stage autoclave filtrating, add the mixing of 178g wolframite fine powder and size mixing, control liquid-solid ratio 5:1 leached 4.0 hours under 230 ℃ of temperature, pressure 2.5MPa.The step-down blowing filters afterwards, and slag changes the two-stage autoclave batching over to; Filtrating WO
3: 100.37g/l changes subsequent handling over to.
Embodiment 5 wolframites are once pressed the two-stage autoclave that boils slag.Get wolframite and once press and boil slag, add 146g soda, excess coefficient 2.5, with the 13g solid caustic soda, 12g aluminum oxide and 1200ml water are sized mixing liquid-solid ratio 5:1; Two-stage autoclave is 3.0 hours under 210 ℃ of temperature, pressure 1.8MPa.The step-down blowing filters afterwards, two-stage autoclave slag sampling analysis, slag tungstenic: 0.72 %, the discarded stacking; WO in the filtrating
3: 27.42g/l; The leaching yield of tungsten ore: 99.44%.
Wolframite is once pressed and is boiled.Measure two-stage autoclave filtrating, add the mixing of 178g wolframite fine powder and size mixing, control liquid-solid ratio 5:1 leached 3.0 hours under 210 ℃ of temperature, pressure 1.8MPa.The step-down blowing filters afterwards, and slag changes the two-stage autoclave batching over to; WO in the filtrating
3: 93.82g/l changes subsequent handling over to.
Claims (4)
1. the soda high pressure lixiviation process extracts the method for tungsten in the tungsten minerals, may further comprise the steps successively:
(1) the once pressure of white tungsten fine ore, wolframite or tungsten ore is boiled slag, with soda and additive carries out tungsten ore and once presses the two-stage autoclave that boils slag under HTHP;
(2) two-stage autoclave being obtained is that the two-stage autoclave slag separates with the two-stage autoclave leach liquor, and said two-stage autoclave leach liquor is the solution of the low high soda concentration of tungsten, and the two-stage autoclave slag is discarded;
(3) utilizing the secondary leach liquor that hangs down the high soda concentration of tungsten that white tungsten fine ore, wolframite or tungsten ore are once pressed boils;
(4) coarse sodium tungstate that step (3) is obtained boils slag with the once pressure of white tungsten fine ore, wolframite or tungsten ore to be separated, and once presses to boil slag and change step (1) over to and make raw material.
2. extract the method for tungsten in the tungsten minerals according to the said soda high pressure lixiviation process of claim 1; It is characterized in that: it is 3～5:1 that the once pressure of the middle white tungsten fine ore of step (1), wolframite or tungsten ore is boiled the liquid-solid ratio that slag is with soda and the additive batch mixing is sized mixing; The soda excess coefficient is 2.0～2.5; 170～240 ℃ of two-stage autoclave temperature, pressure 0.9～2.8MPa, time 2～4 hours.
3. extract the method for tungsten in the tungsten minerals according to the said soda high pressure lixiviation process of claim 1; It is characterized in that: white tungsten fine ore, wolframite or tungsten ore and two-stage autoclave leach liquor batch mixing are sized mixing in the step (3); The control liquid-solid ratio is 3～5:1; Once press and boil 170～240 ℃ of temperature, pressure 0.9～2.8MPa, time 2～4 hours.
4. extract the method for tungsten in the tungsten minerals according to the said soda high pressure lixiviation process of claim 1, it is characterized in that: additive is solid caustic soda and aluminum oxide.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103526052A (en) * | 2013-10-23 | 2014-01-22 | 北京矿冶研究总院 | Method for recovering tungsten from tungsten-containing fluorite ore |
| CN105586487A (en) * | 2016-03-14 | 2016-05-18 | 江西稀有金属钨业控股集团有限公司 | Method for treating scheelite and wolframite mixture ore |
| CN106399723A (en) * | 2016-10-17 | 2017-02-15 | 中国恩菲工程技术有限公司 | Processing method of tungsten-containing tin concentrate |
| CN107641724A (en) * | 2017-08-25 | 2018-01-30 | 洛阳栾川钼业集团股份有限公司 | One kind improves WO in scheelite3The method of leaching rate |
| CN108642279A (en) * | 2018-04-13 | 2018-10-12 | 中南大学 | A kind of method that mixture of sulfuric phosphoric acid pressurization adverse current decomposes wolframite |
| CN109182747A (en) * | 2018-10-22 | 2019-01-11 | 赣州海创钨业有限公司 | A kind of tungsten ore smelting impurity removal process |
| CN109850948A (en) * | 2019-03-14 | 2019-06-07 | 东北大学 | It is a kind of to adulterate WO with white tungsten fine ore synthesis Au3The methods and applications of nanometer sheet |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103526052A (en) * | 2013-10-23 | 2014-01-22 | 北京矿冶研究总院 | Method for recovering tungsten from tungsten-containing fluorite ore |
| CN103526052B (en) * | 2013-10-23 | 2014-12-03 | 北京矿冶研究总院 | Method for recovering tungsten from tungsten-containing fluorite ore |
| CN105586487A (en) * | 2016-03-14 | 2016-05-18 | 江西稀有金属钨业控股集团有限公司 | Method for treating scheelite and wolframite mixture ore |
| CN106399723A (en) * | 2016-10-17 | 2017-02-15 | 中国恩菲工程技术有限公司 | Processing method of tungsten-containing tin concentrate |
| CN107641724A (en) * | 2017-08-25 | 2018-01-30 | 洛阳栾川钼业集团股份有限公司 | One kind improves WO in scheelite3The method of leaching rate |
| CN108642279A (en) * | 2018-04-13 | 2018-10-12 | 中南大学 | A kind of method that mixture of sulfuric phosphoric acid pressurization adverse current decomposes wolframite |
| CN108642279B (en) * | 2018-04-13 | 2020-05-26 | 中南大学 | Method for decomposing wolframite by pressurizing and countercurrent sulfur and phosphorus mixed acid |
| CN109182747A (en) * | 2018-10-22 | 2019-01-11 | 赣州海创钨业有限公司 | A kind of tungsten ore smelting impurity removal process |
| CN109850948A (en) * | 2019-03-14 | 2019-06-07 | 东北大学 | It is a kind of to adulterate WO with white tungsten fine ore synthesis Au3The methods and applications of nanometer sheet |
| CN109850948B (en) * | 2019-03-14 | 2021-03-12 | 东北大学 | Au-doped WO synthesized by using scheelite concentrate3Methods and applications of nanoplatelets |
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Effective date of registration: 20170830 Address after: 332000 Jiangxi province Jiujiang Xiushui county Wu Industrial Park Patentee after: Jiangxi Province North Jiangxi Tungsten Industry Co. Ltd. Address before: 423037 non ferrous metal industry zone, Suxian District, Hunan, Chenzhou Patentee before: Chenzhou Diamond Tungsten Products Co., Ltd. |
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