CN1730686A - Method of combined dissolve to multiple tungsten to deeply extracting tungsten - Google Patents
Method of combined dissolve to multiple tungsten to deeply extracting tungsten Download PDFInfo
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- CN1730686A CN1730686A CNA2005100320119A CN200510032011A CN1730686A CN 1730686 A CN1730686 A CN 1730686A CN A2005100320119 A CNA2005100320119 A CN A2005100320119A CN 200510032011 A CN200510032011 A CN 200510032011A CN 1730686 A CN1730686 A CN 1730686A
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Abstract
The invention discloses a method of combined dissolve to multiple tungsten to deeply extracting tungsten, which comprises pressurized boiling slag from white wolfram, charging alkali liquid into black wolfram boiled slag, carrying out high-basic secondary pressurized boiling to the wolfram slag, separating the secondary boiled slag with low wolfram high alkali solution, abandoning and depositing the secondary boiled slag, pressurized boiling the white wolfram refined ore and wolfram medium ore with low wolfram high alkali solution.
Description
Technical field
The present invention relates to a kind of method of decomposing deeply extracting tungsten that the multiclass tungsten minerals is united.
Background technology
Decomposition leaching method to the multiclass tungsten minerals mainly contains soda high pressure lixiviation process, caustic soda lixiviation process, acid decomposition, unites the pressure cooking method at present, but which kind of method no matter, the tungstenic amount is all higher in its tungsten slag, and white tungsten slag contains WO in the cooking method such as pressing in current with the most use uniting
3Be generally about 4%, how the black general tungstenic about 3% of tungsten slag under tungsten resource situation in short supply day by day, improves that the extraction yield of tungsten is the problem that the tungsten smelting industry urgently waits solution in the tungsten ore.
Summary of the invention
The object of the present invention is to provide a kind of can effectively improve tungsten extraction yield in the tungsten ore the multiclass tungsten minerals is united the method for decomposing deeply extracting tungsten.
The present invention unites the method for decomposing deeply extracting tungsten to the multiclass tungsten minerals, carries out as follows:
A, will carry out once pressing the white tungsten that boils to press boiling slag, tungsten ore to press boiling slag, black tungsten to press boiling slag to add liquid caustic soda carrying out two-stage autoclave, obtain two-stage autoclave slag and the high alkaline solution of low tungsten;
B, the two-stage autoclave slag that step a is obtained separate with the high alkaline solution of low tungsten, and the two-stage autoclave slag is discarded, and the low high alkaline solution of tungsten is used for pressing and boils white tungsten fine ore and tungsten ore, obtain the pressure that tungstenic contains alkaline solution and white tungsten fine ore and tungsten ore and boil slag;
C, the tungstenic that step b is obtained contain alkaline solution and boil slag with the pressure of white tungsten fine ore and tungsten ore and separate, and described pressure is boiled slag and changed the two-stage autoclave batching that step a uses over to; Described tungstenic contains alkaline solution and is used for pressing and boils wolframite, obtains black tungsten and presses and boil slag and low alkali sodium tungstate solution;
D, the black tungsten that step c is obtained are pressed and are boiled slag and separate with low alkali sodium tungstate solution, and black tungsten is pressed and boiled slag and change the two-stage autoclave batching that step a uses over to, and low alkali sodium tungstate solution shifts to be smelted subsequent handling and handle;
Essence of the present invention be with existing unite to press desire depleted tungsten slag in the cooking method and add alkali and carry out two-stage autoclave, tungsten in the depth extraction tungsten ore, the high alkali lye of low tungsten that will obtain then is used for pressure and boils white tungsten fine ore and tungsten ore, press the process integration boil wolframite at last, tungstenic solution alkali concn is reduced successively and tungstenic concentration successively according to increase.The contriver passes through repetition test, to two-stage autoclave slag sampling analysis, the result who draws be two-stage autoclave slag tungstenic only between 0.7%-1%, the effect of deeply extracting tungsten is fine, the present invention has not only made full use of tungsten resource, has meanwhile also solved the recycling problem of caustic soda.
Embodiment
The present invention unites the concrete technology that the method for decomposing deeply extracting tungsten takes to the multiclass tungsten minerals:
1, will once press sheelite after boiling, tungsten ore to press to boil slag and wolframite to press to boil slag to mix with alkali lye and size mixing, controlling liquid-solid ratio is 2～4: 1, and alkali concn is 200～350g/l.At 150～200 ℃, two-stage autoclave is 0.5～1.5 hour under 0.4～0.8MPa, after decomposing materials filters, and washing, gained secondary slag is discarded to be stacked.Low tungsten alkaline solution forwards white tungsten fine ore, the high-alkali pressurization leaching process of tungsten ore to.
2, white tungsten fine ore, tungsten ore are dry grinded and are crossed 325 mesh sieves more than 95%, press tungsten concentrate tungstenic amount and add low tungsten alkaline solution and caustic soda, the alkali consumption is 3-5 a times of theoretical amount, alkali concn is 400～550g/l, regulating liquid-solid ratio is 1.5～2.0: 1, confected materials is added pressure boil still, 190～200 ℃ of temperature, pressure 0.8～1.0MPa leached 1.0～1.5 hours down, decomposing materials, behind dilute filtration, washing, the high-alkali tungstenic solution of gained changes black tungsten pressure over to and boils the batching stage, and slag changes the two-stage autoclave batching over to.
3, wolframite is dry grinded and is crossed 325 mesh sieves more than 90%, add high-alkali tungstenic solution and caustic soda by wolframite tungstenic amount, the alkali consumption is 1.4～2.0 times of theoretical amount, the water glass that adds wolframite weight 2%, the microcosmic salt that adds the required theoretical amount 80～100% of wolframite calcium content, the nitre that adds wolframite weight 2%, regulating liquid-solid ratio is 2～4: 1, at 190～200 ℃, 1.0～1.2MPa leached 1.0～1.5 hours down, decomposing materials, behind the dilute filtration, washing, the low alkali tungstenic solution of gained changes the smelting subsequent handling over to, and slag changes the two-stage autoclave batching over to.
Below provided four embodiments of contriver on probation:
Embodiment carries out during 1 operation as follows:
1, two-stage autoclave is got white tungsten, chats, black tungsten mixing tungsten slag 500g, tungsten pulp water branch: 40%, and WO
3: 4.51%.The liquid caustic soda and the 100ml water that add 750ml, 400g/l are sized mixing, and two-stage autoclave is 1.0 hours under 160～170 ℃ of temperature, pressure 0.5～0.6MPa.The step-down blowing filters afterwards, two-stage autoclave slag sampling analysis, and the slag tungstenic: 0.97%, the discarded stacking; Filtrate basicity 260g/l, WO
3: 9.2g/l.
2, white tungsten is pressed to boil and is measured 1000ml two-stage autoclave filtrate, adds white tungsten fine powder of 500g and sheet alkali 160g mixing and sizes mixing, and 190～200 ℃ of temperature, pressure 0.8～1.0MPa leached 1.0 hours down.The step-down blowing filters afterwards, presses and boils slag sampling analysis, slag tungstenic: 4.42%, and slag changes the two-stage autoclave batching over to; Filtrate basicity 188g/l, WO
3: 210g/l.
3, black tungsten is pressed to boil and is measured the high-alkali high tungsten liquid of 1000ml, adds black tungsten fine powder of 500g and sheet alkali 30g, and adding nitre 10g, additives such as water glass 10ml, microcosmic salt 50g mix sizes mixing, and 190～200 ℃ of temperature, pressure 1.0～1.2MPa leached 1.5 hours down.The step-down blowing filters afterwards, presses and boils slag sampling analysis, slag tungstenic: 3.77%, and slag changes the two-stage autoclave batching over to; Filtrate basicity 25.6g/l, WO
3: 185.0g/l changes subsequent handling over to.
Embodiment carries out during 2 operations as follows:
1, two-stage autoclave is got white tungsten, chats, black tungsten mixing tungsten slag 500g, tungsten pulp water branch: 48%, and WO
3: 4.11%.The liquid caustic soda and the 50ml water that add 800ml, 400g/l are sized mixing, and two-stage autoclave is 1.5 hours under 180 ℃ of temperature, pressure 0.50～0.55MPa.The step-down blowing filters afterwards, two-stage autoclave slag sampling analysis, and the slag tungstenic: 0.78%, the discarded stacking; Filtrate basicity 280g/l, WO
3: 8.4g/l.
2, white tungsten, tungsten ore are pressed to boil and are measured 1000ml secondary filtrate, add the white tungsten of 500g, tungsten ore fine powder and sheet alkali 105g mixing and size mixing, and 190～200 ℃ of temperature, pressure 0.8～1.0MPa leached 1.0 hours down.The step-down blowing filters afterwards, presses and boils slag sampling analysis, slag tungstenic: 5.22%, and slag changes the two-stage autoclave batching over to; Filtrate basicity 180g/l, WO
3: 180g/l.
3, black tungsten is pressed to boil and is measured the high-alkali high tungsten liquid of 1000ml, adds black tungsten fine powder of 500g and sheet alkali 30g, and adding nitre 10g, additives such as water glass 10ml, microcosmic salt 50g mix sizes mixing, and 190～200 ℃ of temperature, pressure 1.0～1.2MPa leached 1.5 hours down.The step-down blowing filters afterwards, presses and boils slag sampling analysis, slag tungstenic: 3.26%, and slag changes the two-stage autoclave batching over to; Filtrate basicity 28.0g/l, WO
3: 176.0g/l changes subsequent handling over to.
Embodiment carries out during 3 operations as follows:
1, two-stage autoclave is got white tungsten, chats, black tungsten mixing tungsten slag 500g, tungsten pulp water branch: 50%, and WO
3: 4.51%.The liquid caustic soda that adds 800ml, 400g/l is sized mixing, and two-stage autoclave is 0.5 hour under 180 ℃ of temperature, pressure 0.4～0.5MPa.The step-down blowing filters afterwards, two-stage autoclave slag sampling analysis, and the slag tungstenic: 1.01%, the discarded stacking; Filtrate basicity 285g/l, WO
3: 8.80g/l.
2, tungsten ore is pressed to boil and is measured 1000ml secondary filtrate, adds 500g tungsten ore fine powder and sheet alkali 65g mixing and sizes mixing, and 190～200 ℃ of temperature, pressure 0.8～1.0MPa leached 1.5 hours down.The step-down blowing filters afterwards, presses and boils slag sampling analysis, slag tungstenic: 6.84%, and slag changes the two-stage autoclave batching over to; Filtrate basicity 210.0g/l, WO
3: 165.0g/l.
3, black tungsten is pressed to boil and is measured the high-alkali high tungsten liquid of 1000ml, adds the black tungsten fine powder of 500g, and adding nitre 10g, additives such as water glass 10ml, microcosmic salt 50g mix sizes mixing, and 190～200 ℃ of temperature, pressure 1.0～1.2MPa leached 1.0 hours down.The step-down blowing filters afterwards, presses and boils slag sampling analysis, slag tungstenic: 2.47%, and slag changes the two-stage autoclave batching over to; Filtrate basicity 22.0g/l, WO
3: 188.0g/l changes subsequent handling over to.
Embodiment carries out during 4 operations as follows:
1, two-stage autoclave is got white tungsten, chats, black tungsten mixing tungsten slag 500g, tungsten pulp water branch: 50%, and WO
3: 5.52%.The liquid caustic soda that adds 1000ml, 400g/l is sized mixing, and two-stage autoclave is 1.5 hours under 190 ℃ of temperature, pressure 0.4～0.5MPa.The step-down blowing filters afterwards, two-stage autoclave slag sampling analysis, and the slag tungstenic: 0.76%, the discarded stacking; Filtrate basicity 302g/l, WO
3: 11.0g/l.
2, white tungsten, tungsten ore are pressed to boil and are measured 1000ml secondary filtrate, add the white tungsten of 500g, tungsten ore fine powder and sheet alkali 170g mixing and size mixing, and 190～200 ℃ of temperature, pressure 0.8～1.0MPa leached 1.5 hours down.The step-down blowing filters afterwards, presses and boils slag sampling analysis, slag tungstenic: 4.22%, and slag changes the two-stage autoclave batching over to; Filtrate basicity 206g/l, WO
3: 193g/l.
3, black tungsten is pressed to boil and is measured the high-alkali high tungsten liquid of 1000ml, adds the black tungsten fine powder of 500g, and adding nitre 10g, additives such as water glass 10ml, microcosmic salt 50g mix sizes mixing, and 190～200 ℃ of temperature, pressure 1.0～1.2MPa leached 1.5 hours down.The step-down blowing filters afterwards, presses and boils slag sampling analysis, slag tungstenic: 3.34%, and slag changes the two-stage autoclave batching over to; Filtrate basicity 26.8g/l, WO
3: 190.0g/l changes subsequent handling over to.
Claims (2)
1, a kind of the multiclass tungsten minerals is united the method for decomposing deeply extracting tungsten, it is characterized in that carrying out as follows:
A, will carry out once pressing the white tungsten that boils to press boiling slag, tungsten ore to press boiling slag, black tungsten to press boiling slag to add liquid caustic soda carrying out two-stage autoclave, obtain two-stage autoclave slag and the high alkaline solution of low tungsten;
B, the two-stage autoclave slag that step a is obtained separate with the high alkaline solution of low tungsten, and the two-stage autoclave slag is discarded, and the low high alkaline solution of tungsten is used for pressing and boils white tungsten fine ore and tungsten ore, obtain the pressure that tungstenic contains alkaline solution and white tungsten fine ore and tungsten ore and boil slag;
C, the tungstenic that step b is obtained contain alkaline solution and boil slag with the pressure of white tungsten fine ore and tungsten ore and separate, and described pressure is boiled slag and changed the two-stage autoclave batching that step a uses over to; Described tungstenic contains alkaline solution and is used for pressing and boils wolframite, obtains black tungsten and presses and boil slag and low alkali sodium tungstate solution;
D, the black tungsten that step c is obtained are pressed and are boiled slag and separate with low alkali sodium tungstate solution, and black tungsten is pressed and boiled slag and change the two-stage autoclave batching that step a uses over to, and low alkali sodium tungstate solution shifts to be smelted subsequent handling and handle.
2, the method for decomposing deeply extracting tungsten that the multiclass tungsten minerals is united according to claim 1, it is characterized in that among the described step a white tungsten pressed and boil slag, tungsten ore and press and boil slag, black tungsten and press and boil slag and add alkali lye and size mixing, the control liquid-solid ratio is 2～4: 1, alkali concn is 200～350g/l, 150～200 ℃ of temperature, carried out two-stage autoclave under pressure 0.4～0.8MPa 0.5～1.5 hour, step-down discharge separated secondary is pressed and is boiled slag and low tungsten alkaline solution again; In step b, white tungsten fine ore, tungsten ore dry grinded and cross 325 mesh sieves more than 95%, press tungsten concentrate tungstenic amount and add 3.0～5.0 times of caustic soda of theoretical amount, alkali concn is 400～550g/l, regulating liquid-solid ratio is 1.5～2.0: 1, confected materials is added pressure boil still, 190～200 ℃ of temperature, pressure 0.8～1.0MPa leached 1.0～1.5 hours down; Wolframite is dry grinded and is crossed 325 mesh sieves more than 90% in step c, add high-alkali tungstenic solution and caustic soda by wolframite tungstenic amount, the alkali consumption is 1.4～2.0 times of theoretical amount, the water glass that adds wolframite weight 2%, the microcosmic salt that adds wolframite calcium content 80～100%, the nitre of adding wolframite weight 2%, regulating liquid-solid ratio is 2～4: 1, at 190～200 ℃, 1.0～1.2MPa leached 1.0～1.5 hours down.
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| CNB2005100320119A CN100390311C (en) | 2005-08-15 | 2005-08-15 | Method of combined dissolve to multiple tungsten to deeply extracting tungsten |
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| CNB2005100320119A CN100390311C (en) | 2005-08-15 | 2005-08-15 | Method of combined dissolve to multiple tungsten to deeply extracting tungsten |
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| CN1730686A true CN1730686A (en) | 2006-02-08 |
| CN100390311C CN100390311C (en) | 2008-05-28 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102747223A (en) * | 2012-07-20 | 2012-10-24 | 郴州钻石钨制品有限责任公司 | Method for extracting tungsten from tungsten mineral by using soda and adopting high-pressure leaching process |
| CN108913884A (en) * | 2018-07-23 | 2018-11-30 | 中国有色集团（广西）平桂飞碟股份有限公司 | Low alkali high temperature and pressure decomposes the method that wolframite prepares coarse sodium tungstate |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1240859C (en) * | 2002-06-07 | 2006-02-08 | 中南大学 | Method for decomposing calcioscheelite and mixed wolframite calcioscheelite under normal pressure by sodium hydrate |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102747223A (en) * | 2012-07-20 | 2012-10-24 | 郴州钻石钨制品有限责任公司 | Method for extracting tungsten from tungsten mineral by using soda and adopting high-pressure leaching process |
| CN102747223B (en) * | 2012-07-20 | 2013-10-02 | 郴州钻石钨制品有限责任公司 | Method for extracting tungsten from tungsten mineral by using soda and adopting high-pressure leaching process |
| CN108913884A (en) * | 2018-07-23 | 2018-11-30 | 中国有色集团（广西）平桂飞碟股份有限公司 | Low alkali high temperature and pressure decomposes the method that wolframite prepares coarse sodium tungstate |
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| CN100390311C (en) | 2008-05-28 |
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Granted publication date: 20080528 Termination date: 20170815 |